Routine Analytical Chemistry Sub-Group Technical Report 2016 Collaborative Study of CORESTA Monitor 8 (CM8) for the Determination of Test Piece Weight, TPM, Water, Nicotine, NFDPM, Carbon Monoxide and Puff Count Obtained under Mainstream ‘ISO’ and ‘Intense’ Smoking Regimes February 2017 Co-ordinator: Linda A. Crumpler, Cerulean, USA Authors: Guy Jaccard and Donatien Tafin Djoko Philip Morris International, Switzerland
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2016 Collaborative Study of CORESTA Monitor 8 (CM8) · 2016 Collaborative Study of CORESTA Monitor 8 (CM8) for the Determination of Test Piece Weight, TPM, Water, Nicotine, NFDPM,
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Transcript
Routine Analytical Chemistry Sub-Group
Technical Report
2016 Collaborative Study of
CORESTA Monitor 8 (CM8)
for the Determination of Test Piece Weight TPM Water Nicotine NFDPM
Carbon Monoxide and Puff Count Obtained under Mainstream lsquoISOrsquo and lsquoIntensersquo
Smoking Regimes
February 2017
Co-ordinator
Linda A Crumpler Cerulean USA
Authors
Guy Jaccard and Donatien Tafin Djoko
Philip Morris International Switzerland
Table of Contents
Introduction 3 1
Organisation 3 2
21 Participants 3
22 Protocol 4
Raw Data 5 3
Statistical Analysis 19 4
Exclusion of outliers 19 41
411 Numerical outlier technique Cochran amp Grubbs test 19
Repeatability and reproducibility estimation 19 42
Data Representation 21 5
51 ISO smoking regime 22
52 Intense smoking regime 25
Comparison 28 6
61 Comparisons of Linear with Rotary smoking machines for test piece CM8 28
62 Comparison with previous studies 28
Conclusion 31 7
APPENDIX A - List of Participating Laboratories 32
APPENDIX B ndash Experimental Protocol 33
APPENDIX C ndash Departures from Experimental Protocol 34
APPENDIX D ndash Raw Data Set 35
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure 44
APPENDIX F ndash Linear - Rotary Comparisons 45
APPENDIX G ndash Rotary Smoking Machines 52
APPENDIX H ndash Linear Smoking Machines 59
APPENDIX I ndash Equipment Survey 66
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 377
Introduction 1
The CORESTA Routine Analytical Chemistry Sub-Group has been given the responsibility to
organize the annual testing of the CORESTA Monitor test piece
The 2016 study was designed
to measure mainstream ISO and Intense smoke yields of nicotine-free dry particulate
matter (NFDPM) nicotine and carbon monoxide (CO) to verify the current monitor test
piece CM8
to determine intra- and inter-laboratory variability for the measured ISO and Intense smoke
yields for the CM8
to verify the conditioned weight for the CM8
Organisation 2
21 Participants
In total 25 laboratories participated in the 2016 study Appendix A lists the participating
laboratories in alphabetical order Note the mix of labs between ISO and Intense differed
25 laboratories delivered data for ISO mainstream smoke for the CM8 test piece using 36
smoking machines (20 rotary smoking machines and 16 linear smoking machines)
20 laboratories delivered data for Intense mainstream smoke for the CM8 test piece using 28
smoking machines (15 rotary smoking machines and 13 linear smoking machines)
One laboratory provided an incomplete data set
Table 1 summarises the number and type of smoking machines used
Table 1 Number of smoking machines
Machine Class ISO Intense
Linear smoking machines 16 13
LX-20 type 2 2
SM450 type 14 11
Rotary smoking machines 20 15
RM20A type 1 1
RM20D type 2 2
RM20H type 5 3
RM200 type 1 1
RM200A type 11 8
Total 36 28
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 477
Table 2 summarises the number of datasets provided for the reported parameters
Table 2 Number of datasets obtained
Physical Parameter
WEIGHT 175
Smoking Parameter ISO Intense
TPM 180 140
WATER 180 140
NIC 180 140
NFDPM 180 140
CO 180 140
PUFF 180 140
Total individual data obtained 1080 840
Total individual data expected 1080 840
A laboratory code number has been assigned in confidence by the study co-ordinator to each
of the individual smoking machines used in the study
22 Protocol
Participants were requested to follow the protocol ldquoAnnual Study of the CORESTA Monitor
Test Piece CM8 - 2016 Experimental Protocolrdquo (provided in Appendix B) to analyse the CM8
test pieces and to report the seven parameters listed in Table 3
Table 3 Parameters to be reported
Parameter Number of replicates Unit Code
Conditioned Weight 5 mgtest piece (tp) WEIGHT
Total Particulate Matter 5 mgtest piece (tp) TPM
Water content (smoke) 5 mgtest piece (tp) WATER
Smoke Nicotine 5 mgtest piece (tp) NIC
Nicotine Free Dry
Particulate Matter 5 mgtest piece (tp) NFDPM
Carbon Monoxide 5 mgtest piece (tp) CO
Puff count 5 pufftest piece (tp) PUFF
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 577
CM8 test pieces should have been smoked under two different mainstream smoking regimes
with a fixed butt length of 32 mm as defined in the following table
Table 4 Mainstream ISO and Intense (Health Canada Intense or HCI) smoking regime
parameters
Smoking
Regime
Puff Volume
(mL)
Puff Frequency
(s)
Puff Duration
(s)
Vent Blocking
()
ISO 35 60 2 0
Intense (HCI) 55 30 2 100
The CM8 test piece was purchased by the participants individually via Borgwaldt KC or
Cerulean
Raw Data 3
Table 5 gives the results for conditioned weight while Tables 6 to 11 list the results for the
reported parameters for ISO smoking regime Tables 12 to 17 list the results for intense
smoking regime Basic statistics (mean and standard deviation) were applied to summarize the
raw data for each smoking machine used and parameters reported for CM8 test piece At this
stage no outlier statistics were applied Appendix D contains the raw data (single values) for
every measured parameter reported by smoking machine included in the study
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 677
Table 5 WEIGHT mean and standard deviation per laboratory code
Lab Code Machine Type Mean SD CV [] Sample size
1A R 96055 2731 0284 5
1B L 96519 3313 0343 5
2A R 94828 2622 0277 5
2B L 95000 5958 0627 5
3 R 90323 3183 0352 5
4A R 96060 2510 0261 5
4B R 96200 6481 0674 5
5A R 96494 1638 0170 5
5B R 95620 2978 0311 5
6A R 96612 4814 0498 5
6B L 96604 2688 0278 5
7A L 95598 3295 0345 5
7B R 95490 3365 0352 5
8 R 96653 2676 0277 5
9A L 95220 2564 0269 5
9B R 95900 2264 0236 5
10 L 96640 2595 0269 5
11 L 95968 8571 0893 5
12A R 95840 4930 0514 5
12B R 96226 2852 0296 5
12C L 95960 2702 0282 5
13A R 95806 2698 0282 5
13B R 95901 5717 0596 5
14 R 96102 3340 0348 5
15 R 95871 4505 0470 5
16 L 96286 4512 0469 5
17 L 95626 3166 0331 5
18 L 95285 3720 0390 5
19 L 95285 3720 0390 5
20 L 95767 5690 0594 5
22A R 96300 1414 0147 5
22B R 96240 1517 0158 5
23 R 94926 3700 0390 5
24 L 95591 5108 0534 5
25 L 96223 5979 0621 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 777
Table 6 ISO smoking regime TPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1793 024 132 5
2B L 1765 063 357 5
6B L 1574 061 387 5
7A L 1804 039 214 5
9A L 1698 033 197 5
10 L 1807 048 265 5
11 L 1828 045 248 5
12C L 1728 055 321 5
16 L 1742 010 058 5
17 L 1616 030 187 5
18 L 1772 036 205 5
19 L 1772 036 205 5
20 L 1783 040 224 5
21 L 1832 050 272 5
24 L 1791 033 185 5
25 L 1607 079 494 5
1A R 1749 024 135 5
2A R 1698 028 166 5
3 R 1760 019 107 5
4A R 1723 028 165 5
4B R 1769 038 212 5
5A R 1703 022 127 5
5B R 1724 031 178 5
6A R 1740 031 176 5
7B R 1646 017 103 5
8 R 1737 022 125 5
9B R 1711 025 147 5
12A R 1758 040 227 5
12B R 1790 014 078 5
13A R 1674 017 104 5
13B R 1700 020 115 5
14 R 1746 044 254 5
15 R 1719 041 238 5
22A R 1752 020 115 5
22B R 1731 022 129 5
23 R 1651 037 226 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 877
Table 7 ISO Smoking regime WATER mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 161 007 428 5
2B L 145 008 518 5
6B L 118 014 1213 5
7A L 175 006 364 5
9A L 142 011 802 5
10 L 177 010 581 5
11 L 142 009 632 5
12C L 122 008 645 5
16 L 142 012 872 5
17 L 145 026 1823 5
18 L 147 019 1299 5
19 L 147 019 1299 5
20 L 214 013 611 5
21 L 120 024 2024 5
24 L 156 009 551 5
25 L 127 016 1261 5
1A R 215 007 316 5
2A R 174 008 444 5
3 R 196 010 493 5
4A R 197 008 406 5
4B R 213 013 629 5
5A R 197 009 471 5
5B R 192 008 419 5
6A R 227 010 445 5
7B R 184 007 396 5
8 R 206 013 637 5
9B R 203 012 579 5
12A R 250 012 464 5
12B R 244 010 430 5
13A R 205 007 362 5
13B R 204 012 576 5
14 R 228 017 739 5
15 R 188 016 834 5
22A R 219 007 337 5
22B R 215 005 225 5
23 R 179 003 179 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 977
Table 8 ISO Smoking regime Nicotine mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1704 0029 170 5
2B L 1706 0039 227 5
6B L 1624 0048 295 5
7A L 1687 0033 194 5
9A L 1612 0200 1240 5
10 L 1748 0070 401 5
11 L 1691 0028 166 5
12C L 1669 0034 206 5
16 L 1731 0028 159 5
17 L 1674 0046 276 5
18 L 1697 0014 082 5
19 L 1697 0014 082 5
20 L 1734 0021 124 5
21 L 1812 0048 266 5
24 L 1694 0037 217 5
25 L 1743 0154 883 5
1A R 1669 0023 141 5
2A R 1638 0037 224 5
3 R 1652 0018 110 5
4A R 1630 0042 255 5
4B R 1653 0035 214 5
5A R 1612 0023 142 5
5B R 1602 0023 141 5
6A R 1661 0037 225 5
7B R 1564 0022 140 5
8 R 1535 0031 204 5
9B R 1659 0047 285 5
12A R 1719 0024 142 5
12B R 1718 0037 216 5
13A R 1497 0024 163 5
13B R 1546 0013 086 5
14 R 1590 0035 217 5
15 R 1651 0030 181 5
22A R 1612 0011 068 5
22B R 1630 0012 075 5
23 R 1639 0026 159 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1077
Table 9 ISO smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1462 016 111 5
2B L 1449 053 366 5
6B L 1294 044 344 5
7A L 1460 031 214 5
9A L 1395 011 080 5
10 L 1455 039 269 5
11 L 1518 036 236 5
12C L 1439 049 338 5
16 L 1427 013 092 5
17 L 1304 054 413 5
18 L 1456 020 135 5
19 L 1456 020 135 5
20 L 1395 036 255 5
21 L 1531 057 371 5
24 L 1466 023 154 5
25 L 1306 066 509 5
1A R 1367 020 145 5
2A R 1361 023 169 5
3 R 1398 012 083 5
4A R 1363 024 176 5
4B R 1391 028 201 5
5A R 1347 014 107 5
5B R 1372 023 166 5
6A R 1346 019 142 5
7B R 1305 020 153 5
8 R 1378 026 192 5
9B R 1342 015 114 5
12A R 1337 037 278 5
12B R 1375 018 129 5
13A R 1319 015 112 5
13B R 1341 009 069 5
14 R 1359 028 204 5
15 R 1366 029 214 5
22A R 1371 019 136 5
22B R 1353 024 175 5
23 R 1308 037 283 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1177
Table 10 ISO Smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1335 020 150 5
2B L 1297 037 288 5
6B L 1260 099 790 5
7A L 1374 034 249 5
9A L 1233 019 153 5
10 L 1219 054 445 5
11 L 1267 044 350 5
12C L 1325 033 248 5
16 L 1307 024 185 5
17 L 1196 029 242 5
18 L 1335 010 072 5
19 L 1335 010 072 5
20 L 1324 033 248 5
21 L 1363 032 238 5
24 L 1263 040 315 5
25 L 1194 069 574 5
1A R 1368 010 076 5
2A R 1308 018 135 5
3 R 1345 023 172 5
4A R 1340 011 079 5
4B R 1394 041 294 5
5A R 1292 028 216 5
5B R 1360 034 251 5
6A R 1372 023 166 5
7B R 1291 013 098 5
8 R 1369 025 183 5
9B R 1276 023 182 5
12A R 1317 034 256 5
12B R 1375 024 175 5
13A R 1334 021 155 5
13B R 1338 030 227 5
14 R 1366 023 167 5
15 R 1377 019 139 5
22A R 1344 016 118 5
22B R 1341 016 116 5
23 R 1334 029 217 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1277
Table 11 ISO Smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 796 005 059 5
2B L 806 012 144 5
6B L 814 018 219 5
7A L 789 009 112 5
9A L 781 024 306 5
10 L 802 020 245 5
11 L 784 018 225 5
12C L 794 021 263 5
16 L 850 014 168 5
17 L 774 016 203 5
18 L 787 015 187 5
19 L 787 015 187 5
20 L 769 014 188 5
21 L 808 008 097 5
24 L 792 010 128 5
25 L 751 030 400 5
1A R 767 005 068 5
2A R 727 008 109 5
3 R 779 008 099 5
4A R 748 011 146 5
4B R 758 013 172 5
5A R 782 011 144 5
5B R 766 017 216 5
6A R 773 009 117 5
7B R 716 011 160 5
8 R 754 010 127 5
9B R 755 008 107 5
12A R 755 006 078 5
12B R 771 008 102 5
13A R 740 017 225 5
13B R 769 007 091 5
14 R 761 011 140 5
15 R 750 018 246 5
22A R 757 008 110 5
22B R 759 007 088 5
23 R 732 009 117 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1377
Table 12 Intense smoking regime TPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 4551 091 200 5
2B L 4391 078 178 5
6B L 3936 067 170 5
9A L 4471 060 134 5
10 L 4667 073 157 5
11 L 5068 136 269 5
12C L 4644 031 066 5
17 L 4346 106 243 5
19 L 4566 087 190 5
20 L 4616 122 265 5
21 L 5008 077 153 5
24 L 4782 094 196 5
25 L 4434 081 182 5
1A R 4168 016 039 5
2A R 4014 024 061 5
3 R 4247 035 083 5
4A R 4097 039 095 5
4B R 4181 064 153 5
5B R 3997 040 101 5
6A R 4076 074 181 5
8 R 4044 043 107 5
9B R 4097 033 080 5
12A R 4125 046 112 5
12B R 4257 039 092 5
15 R 3957 052 131 5
22A R 4046 028 069 5
22B R 4015 045 112 5
23 R 3830 073 192 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1477
Table 13 Intense smoking regime Water mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1237 038 305 5
2B L 999 037 375 5
6B L 906 034 381 5
9A L 1147 043 373 5
10 L 1152 052 453 5
11 L 1488 053 356 5
12C L 1061 019 179 5
17 L 1027 028 274 5
19 L 1095 038 348 5
20 L 1216 083 681 5
21 L 1285 026 206 5
24 L 1235 060 484 5
25 L 1004 031 307 5
1A R 1024 014 138 5
2A R 797 016 197 5
3 R 974 031 317 5
4A R 911 034 368 5
4B R 931 027 287 5
5B R 815 041 507 5
6A R 923 038 411 5
8 R 929 033 354 5
9B R 927 028 301 5
12A R 1004 051 508 5
12B R 935 017 181 5
15 R 823 029 349 5
22A R 953 005 052 5
22B R 926 038 410 5
23 R 1598 065 404 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1577
Table 14 Intense smoking regime Nicotine mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 3484 0055 158 5
2B L 3434 0048 141 5
6B L 3342 0051 153 5
9A L 3494 0089 255 5
10 L 3578 0226 633 5
11 L 3620 0082 225 5
12C L 3402 0024 070 5
17 L 3622 0075 208 5
19 L 3520 0012 035 5
20 L 3552 0230 647 5
21 L 3712 0030 082 5
24 L 3524 0061 174 5
25 L 2986 0052 173 5
1A R 3385 0020 060 5
2A R 3317 0030 090 5
3 R 3479 0023 067 5
4A R 3369 0037 109 5
4B R 3340 0053 160 5
5B R 1677 0025 148 5
6A R 3390 0066 195 5
8 R 2967 0044 149 5
9B R 3410 0048 142 5
12A R 3452 0030 085 5
12B R 3520 0068 192 5
15 R 3333 0099 296 5
22A R 3222 0051 159 5
22B R 3210 0049 151 5
23 R 6610 0108 163 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1677
Table 15 Intense smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2965 054 183 5
2B L 3048 092 301 5
6B L 2696 035 131 5
9A L 2975 038 129 5
10 L 3157 047 148 5
11 L 3218 082 255 5
12C L 3243 015 047 5
17 L 3157 079 250 5
19 L 3119 084 268 5
20 L 3045 056 185 5
21 L 3351 066 198 5
24 L 3195 050 158 5
25 L 3132 054 174 5
1A R 2806 018 065 5
2A R 2885 012 043 5
3 R 2925 040 135 5
4A R 2849 021 074 5
4B R 2917 035 119 5
5B R 3013 023 077 5
6A R 2811 036 129 5
8 R 2819 021 074 5
9B R 2832 032 115 5
12A R 2776 048 171 5
12B R 2970 026 086 5
15 R 2800 035 124 5
22A R 2770 025 091 5
22B R 2768 049 178 5
23 R 1570 060 384 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1777
Table 16 Intense smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2478 034 137 5
2B L 2472 027 111 5
6B L 2367 039 165 5
9A L 2423 065 270 5
10 L 2373 018 077 5
11 L 2568 029 114 5
12C L 2497 028 113 5
17 L 2321 032 139 5
19 L 2488 022 086 5
20 L 2489 056 227 5
21 L 2523 045 177 5
24 L 2470 052 211 5
25 L 2399 089 369 5
1A R 2505 033 131 5
2A R 2485 037 149 5
3 R 2605 031 119 5
4A R 2513 031 125 5
4B R 2542 047 185 5
5B R 2480 022 088 5
6A R 2570 024 092 5
8 R 2532 047 185 5
9B R 2457 044 181 5
12A R 2506 023 093 5
12B R 2523 018 069 5
15 R 2547 039 154 5
22A R 2470 034 138 5
22B R 2466 032 130 5
23 R 2508 030 119 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1877
Table 17 Intense smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 1138 022 191 5
2B L 1154 019 162 5
6B L 1170 008 068 5
9A L 1095 013 114 5
10 L 1138 023 199 5
11 L 1127 016 138 5
12C L 1115 022 199 5
17 L 1110 009 079 5
19 L 1059 011 101 5
20 L 1087 019 176 5
21 L 1121 019 169 5
24 L 1106 027 248 5
25 L 1102 012 105 5
1A R 1111 018 159 5
2A R 1059 014 130 5
3 R 1152 013 110 5
4A R 1078 008 070 5
4B R 1105 016 143 5
5B R 1134 030 267 5
6A R 1136 004 034 5
8 R 1075 015 142 5
9B R 1077 006 054 5
12A R 1102 020 186 5
12B R 1097 016 148 5
15 R 1084 010 091 5
22A R 1112 016 147 5
22B R 1106 014 122 5
23 R 1066 009 088 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1977
Statistical Analysis 4
Exclusion of outliers 41
411 Numerical outlier technique Cochran amp Grubbs test
The statistical evaluation of data for this collaborative study followed the methods provided
by ISO 5725-21 For outlier testing the Grubbs and Cochran methods were used
ISO 5725-2 Tests Consistency
Cochranrsquos ndash test Within-laboratory variability Suitable for detecting whether the highest value in a set of laboratory standard deviations is an outlier or not
Grubbsrsquo ndash test Between-laboratory variability Suitable for detecting whether the highest (or lowest) laboratories averages are outliers or not
The protocol ldquoHarmonized statistical procedurerdquo defined by IUPAC (International Union of
Pure and Applied Chemistry) has been applied as well It consists of sequential applications of
the Cochran and Grubbs tests until no further outliers are detected or until a drop of more than
222 (for this study =29) in the original number of laboratories would occur (see flowchart
in Appendix F)
First apply the Cochran outlier test and if an outlying laboratory is identified then a single
value Grubbs test is performed on the individual values of this outlying laboratory (Individual
Grubbs) If no individual value is identified as outlier the outlying laboratory is removed
When an individual value is identified as an outlier only this value is removed
Afterwards single-value Grubbs test is applied and outlying laboratories are removed If no
laboratory is identified as outlier the pair-value test is applied (two values at the same end)
Remove any laboratory(ies) flagged by these tests but stop removal if more than 222 (2 of
9 laboratories) would be removed
The test was performed with both linear and rotary smoking machines together but also with
rotary respectively linear smoking machines separately The results provided in the report for
all smoking machines respectively with linear or rotary only smoking machines are obtained
after exclusion of the outliers for those respective categories
Note
The paired value Grubbsrsquo test is an extension of the single value Grubbs test for pairs of
outliers The use is advised in ISO 5725 to detect pairs of outlier undetectable sequentially by
using single value Grubbs test
The outlying laboratories are provided in the Tables 18 to 23
Repeatability and reproducibility estimation 42
Repeatability and reproducibility limits are calculated for both smoking regimes each
parameter and for both smoking machine types The results are summarized in tables 18 to 23
with all machines grouped respectively with linear or rotary machines only both with ISO
and intense smoking regimes Outlying laboratories are provided in the same tables The
corresponding graphs named ldquoindividual valuesrdquo are given in Part 5 of this report
1 ISO 5725-21994 Accuracy (trueness and precision) of measurement methods and results ndash Part 2 Basic
method for the determination of repeatability and reproducibility of a standard measurement method
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 2077
Table 18 r amp R estimations for CM8 under ISO smoking regime (all machines)
p n Global Mean Sr CVr[] r SR CVR [] R C GG2 Stragglers Parameter
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
Table of Contents
Introduction 3 1
Organisation 3 2
21 Participants 3
22 Protocol 4
Raw Data 5 3
Statistical Analysis 19 4
Exclusion of outliers 19 41
411 Numerical outlier technique Cochran amp Grubbs test 19
Repeatability and reproducibility estimation 19 42
Data Representation 21 5
51 ISO smoking regime 22
52 Intense smoking regime 25
Comparison 28 6
61 Comparisons of Linear with Rotary smoking machines for test piece CM8 28
62 Comparison with previous studies 28
Conclusion 31 7
APPENDIX A - List of Participating Laboratories 32
APPENDIX B ndash Experimental Protocol 33
APPENDIX C ndash Departures from Experimental Protocol 34
APPENDIX D ndash Raw Data Set 35
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure 44
APPENDIX F ndash Linear - Rotary Comparisons 45
APPENDIX G ndash Rotary Smoking Machines 52
APPENDIX H ndash Linear Smoking Machines 59
APPENDIX I ndash Equipment Survey 66
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 377
Introduction 1
The CORESTA Routine Analytical Chemistry Sub-Group has been given the responsibility to
organize the annual testing of the CORESTA Monitor test piece
The 2016 study was designed
to measure mainstream ISO and Intense smoke yields of nicotine-free dry particulate
matter (NFDPM) nicotine and carbon monoxide (CO) to verify the current monitor test
piece CM8
to determine intra- and inter-laboratory variability for the measured ISO and Intense smoke
yields for the CM8
to verify the conditioned weight for the CM8
Organisation 2
21 Participants
In total 25 laboratories participated in the 2016 study Appendix A lists the participating
laboratories in alphabetical order Note the mix of labs between ISO and Intense differed
25 laboratories delivered data for ISO mainstream smoke for the CM8 test piece using 36
smoking machines (20 rotary smoking machines and 16 linear smoking machines)
20 laboratories delivered data for Intense mainstream smoke for the CM8 test piece using 28
smoking machines (15 rotary smoking machines and 13 linear smoking machines)
One laboratory provided an incomplete data set
Table 1 summarises the number and type of smoking machines used
Table 1 Number of smoking machines
Machine Class ISO Intense
Linear smoking machines 16 13
LX-20 type 2 2
SM450 type 14 11
Rotary smoking machines 20 15
RM20A type 1 1
RM20D type 2 2
RM20H type 5 3
RM200 type 1 1
RM200A type 11 8
Total 36 28
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 477
Table 2 summarises the number of datasets provided for the reported parameters
Table 2 Number of datasets obtained
Physical Parameter
WEIGHT 175
Smoking Parameter ISO Intense
TPM 180 140
WATER 180 140
NIC 180 140
NFDPM 180 140
CO 180 140
PUFF 180 140
Total individual data obtained 1080 840
Total individual data expected 1080 840
A laboratory code number has been assigned in confidence by the study co-ordinator to each
of the individual smoking machines used in the study
22 Protocol
Participants were requested to follow the protocol ldquoAnnual Study of the CORESTA Monitor
Test Piece CM8 - 2016 Experimental Protocolrdquo (provided in Appendix B) to analyse the CM8
test pieces and to report the seven parameters listed in Table 3
Table 3 Parameters to be reported
Parameter Number of replicates Unit Code
Conditioned Weight 5 mgtest piece (tp) WEIGHT
Total Particulate Matter 5 mgtest piece (tp) TPM
Water content (smoke) 5 mgtest piece (tp) WATER
Smoke Nicotine 5 mgtest piece (tp) NIC
Nicotine Free Dry
Particulate Matter 5 mgtest piece (tp) NFDPM
Carbon Monoxide 5 mgtest piece (tp) CO
Puff count 5 pufftest piece (tp) PUFF
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 577
CM8 test pieces should have been smoked under two different mainstream smoking regimes
with a fixed butt length of 32 mm as defined in the following table
Table 4 Mainstream ISO and Intense (Health Canada Intense or HCI) smoking regime
parameters
Smoking
Regime
Puff Volume
(mL)
Puff Frequency
(s)
Puff Duration
(s)
Vent Blocking
()
ISO 35 60 2 0
Intense (HCI) 55 30 2 100
The CM8 test piece was purchased by the participants individually via Borgwaldt KC or
Cerulean
Raw Data 3
Table 5 gives the results for conditioned weight while Tables 6 to 11 list the results for the
reported parameters for ISO smoking regime Tables 12 to 17 list the results for intense
smoking regime Basic statistics (mean and standard deviation) were applied to summarize the
raw data for each smoking machine used and parameters reported for CM8 test piece At this
stage no outlier statistics were applied Appendix D contains the raw data (single values) for
every measured parameter reported by smoking machine included in the study
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 677
Table 5 WEIGHT mean and standard deviation per laboratory code
Lab Code Machine Type Mean SD CV [] Sample size
1A R 96055 2731 0284 5
1B L 96519 3313 0343 5
2A R 94828 2622 0277 5
2B L 95000 5958 0627 5
3 R 90323 3183 0352 5
4A R 96060 2510 0261 5
4B R 96200 6481 0674 5
5A R 96494 1638 0170 5
5B R 95620 2978 0311 5
6A R 96612 4814 0498 5
6B L 96604 2688 0278 5
7A L 95598 3295 0345 5
7B R 95490 3365 0352 5
8 R 96653 2676 0277 5
9A L 95220 2564 0269 5
9B R 95900 2264 0236 5
10 L 96640 2595 0269 5
11 L 95968 8571 0893 5
12A R 95840 4930 0514 5
12B R 96226 2852 0296 5
12C L 95960 2702 0282 5
13A R 95806 2698 0282 5
13B R 95901 5717 0596 5
14 R 96102 3340 0348 5
15 R 95871 4505 0470 5
16 L 96286 4512 0469 5
17 L 95626 3166 0331 5
18 L 95285 3720 0390 5
19 L 95285 3720 0390 5
20 L 95767 5690 0594 5
22A R 96300 1414 0147 5
22B R 96240 1517 0158 5
23 R 94926 3700 0390 5
24 L 95591 5108 0534 5
25 L 96223 5979 0621 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 777
Table 6 ISO smoking regime TPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1793 024 132 5
2B L 1765 063 357 5
6B L 1574 061 387 5
7A L 1804 039 214 5
9A L 1698 033 197 5
10 L 1807 048 265 5
11 L 1828 045 248 5
12C L 1728 055 321 5
16 L 1742 010 058 5
17 L 1616 030 187 5
18 L 1772 036 205 5
19 L 1772 036 205 5
20 L 1783 040 224 5
21 L 1832 050 272 5
24 L 1791 033 185 5
25 L 1607 079 494 5
1A R 1749 024 135 5
2A R 1698 028 166 5
3 R 1760 019 107 5
4A R 1723 028 165 5
4B R 1769 038 212 5
5A R 1703 022 127 5
5B R 1724 031 178 5
6A R 1740 031 176 5
7B R 1646 017 103 5
8 R 1737 022 125 5
9B R 1711 025 147 5
12A R 1758 040 227 5
12B R 1790 014 078 5
13A R 1674 017 104 5
13B R 1700 020 115 5
14 R 1746 044 254 5
15 R 1719 041 238 5
22A R 1752 020 115 5
22B R 1731 022 129 5
23 R 1651 037 226 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 877
Table 7 ISO Smoking regime WATER mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 161 007 428 5
2B L 145 008 518 5
6B L 118 014 1213 5
7A L 175 006 364 5
9A L 142 011 802 5
10 L 177 010 581 5
11 L 142 009 632 5
12C L 122 008 645 5
16 L 142 012 872 5
17 L 145 026 1823 5
18 L 147 019 1299 5
19 L 147 019 1299 5
20 L 214 013 611 5
21 L 120 024 2024 5
24 L 156 009 551 5
25 L 127 016 1261 5
1A R 215 007 316 5
2A R 174 008 444 5
3 R 196 010 493 5
4A R 197 008 406 5
4B R 213 013 629 5
5A R 197 009 471 5
5B R 192 008 419 5
6A R 227 010 445 5
7B R 184 007 396 5
8 R 206 013 637 5
9B R 203 012 579 5
12A R 250 012 464 5
12B R 244 010 430 5
13A R 205 007 362 5
13B R 204 012 576 5
14 R 228 017 739 5
15 R 188 016 834 5
22A R 219 007 337 5
22B R 215 005 225 5
23 R 179 003 179 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 977
Table 8 ISO Smoking regime Nicotine mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1704 0029 170 5
2B L 1706 0039 227 5
6B L 1624 0048 295 5
7A L 1687 0033 194 5
9A L 1612 0200 1240 5
10 L 1748 0070 401 5
11 L 1691 0028 166 5
12C L 1669 0034 206 5
16 L 1731 0028 159 5
17 L 1674 0046 276 5
18 L 1697 0014 082 5
19 L 1697 0014 082 5
20 L 1734 0021 124 5
21 L 1812 0048 266 5
24 L 1694 0037 217 5
25 L 1743 0154 883 5
1A R 1669 0023 141 5
2A R 1638 0037 224 5
3 R 1652 0018 110 5
4A R 1630 0042 255 5
4B R 1653 0035 214 5
5A R 1612 0023 142 5
5B R 1602 0023 141 5
6A R 1661 0037 225 5
7B R 1564 0022 140 5
8 R 1535 0031 204 5
9B R 1659 0047 285 5
12A R 1719 0024 142 5
12B R 1718 0037 216 5
13A R 1497 0024 163 5
13B R 1546 0013 086 5
14 R 1590 0035 217 5
15 R 1651 0030 181 5
22A R 1612 0011 068 5
22B R 1630 0012 075 5
23 R 1639 0026 159 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1077
Table 9 ISO smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1462 016 111 5
2B L 1449 053 366 5
6B L 1294 044 344 5
7A L 1460 031 214 5
9A L 1395 011 080 5
10 L 1455 039 269 5
11 L 1518 036 236 5
12C L 1439 049 338 5
16 L 1427 013 092 5
17 L 1304 054 413 5
18 L 1456 020 135 5
19 L 1456 020 135 5
20 L 1395 036 255 5
21 L 1531 057 371 5
24 L 1466 023 154 5
25 L 1306 066 509 5
1A R 1367 020 145 5
2A R 1361 023 169 5
3 R 1398 012 083 5
4A R 1363 024 176 5
4B R 1391 028 201 5
5A R 1347 014 107 5
5B R 1372 023 166 5
6A R 1346 019 142 5
7B R 1305 020 153 5
8 R 1378 026 192 5
9B R 1342 015 114 5
12A R 1337 037 278 5
12B R 1375 018 129 5
13A R 1319 015 112 5
13B R 1341 009 069 5
14 R 1359 028 204 5
15 R 1366 029 214 5
22A R 1371 019 136 5
22B R 1353 024 175 5
23 R 1308 037 283 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1177
Table 10 ISO Smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1335 020 150 5
2B L 1297 037 288 5
6B L 1260 099 790 5
7A L 1374 034 249 5
9A L 1233 019 153 5
10 L 1219 054 445 5
11 L 1267 044 350 5
12C L 1325 033 248 5
16 L 1307 024 185 5
17 L 1196 029 242 5
18 L 1335 010 072 5
19 L 1335 010 072 5
20 L 1324 033 248 5
21 L 1363 032 238 5
24 L 1263 040 315 5
25 L 1194 069 574 5
1A R 1368 010 076 5
2A R 1308 018 135 5
3 R 1345 023 172 5
4A R 1340 011 079 5
4B R 1394 041 294 5
5A R 1292 028 216 5
5B R 1360 034 251 5
6A R 1372 023 166 5
7B R 1291 013 098 5
8 R 1369 025 183 5
9B R 1276 023 182 5
12A R 1317 034 256 5
12B R 1375 024 175 5
13A R 1334 021 155 5
13B R 1338 030 227 5
14 R 1366 023 167 5
15 R 1377 019 139 5
22A R 1344 016 118 5
22B R 1341 016 116 5
23 R 1334 029 217 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1277
Table 11 ISO Smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 796 005 059 5
2B L 806 012 144 5
6B L 814 018 219 5
7A L 789 009 112 5
9A L 781 024 306 5
10 L 802 020 245 5
11 L 784 018 225 5
12C L 794 021 263 5
16 L 850 014 168 5
17 L 774 016 203 5
18 L 787 015 187 5
19 L 787 015 187 5
20 L 769 014 188 5
21 L 808 008 097 5
24 L 792 010 128 5
25 L 751 030 400 5
1A R 767 005 068 5
2A R 727 008 109 5
3 R 779 008 099 5
4A R 748 011 146 5
4B R 758 013 172 5
5A R 782 011 144 5
5B R 766 017 216 5
6A R 773 009 117 5
7B R 716 011 160 5
8 R 754 010 127 5
9B R 755 008 107 5
12A R 755 006 078 5
12B R 771 008 102 5
13A R 740 017 225 5
13B R 769 007 091 5
14 R 761 011 140 5
15 R 750 018 246 5
22A R 757 008 110 5
22B R 759 007 088 5
23 R 732 009 117 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1377
Table 12 Intense smoking regime TPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 4551 091 200 5
2B L 4391 078 178 5
6B L 3936 067 170 5
9A L 4471 060 134 5
10 L 4667 073 157 5
11 L 5068 136 269 5
12C L 4644 031 066 5
17 L 4346 106 243 5
19 L 4566 087 190 5
20 L 4616 122 265 5
21 L 5008 077 153 5
24 L 4782 094 196 5
25 L 4434 081 182 5
1A R 4168 016 039 5
2A R 4014 024 061 5
3 R 4247 035 083 5
4A R 4097 039 095 5
4B R 4181 064 153 5
5B R 3997 040 101 5
6A R 4076 074 181 5
8 R 4044 043 107 5
9B R 4097 033 080 5
12A R 4125 046 112 5
12B R 4257 039 092 5
15 R 3957 052 131 5
22A R 4046 028 069 5
22B R 4015 045 112 5
23 R 3830 073 192 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1477
Table 13 Intense smoking regime Water mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1237 038 305 5
2B L 999 037 375 5
6B L 906 034 381 5
9A L 1147 043 373 5
10 L 1152 052 453 5
11 L 1488 053 356 5
12C L 1061 019 179 5
17 L 1027 028 274 5
19 L 1095 038 348 5
20 L 1216 083 681 5
21 L 1285 026 206 5
24 L 1235 060 484 5
25 L 1004 031 307 5
1A R 1024 014 138 5
2A R 797 016 197 5
3 R 974 031 317 5
4A R 911 034 368 5
4B R 931 027 287 5
5B R 815 041 507 5
6A R 923 038 411 5
8 R 929 033 354 5
9B R 927 028 301 5
12A R 1004 051 508 5
12B R 935 017 181 5
15 R 823 029 349 5
22A R 953 005 052 5
22B R 926 038 410 5
23 R 1598 065 404 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1577
Table 14 Intense smoking regime Nicotine mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 3484 0055 158 5
2B L 3434 0048 141 5
6B L 3342 0051 153 5
9A L 3494 0089 255 5
10 L 3578 0226 633 5
11 L 3620 0082 225 5
12C L 3402 0024 070 5
17 L 3622 0075 208 5
19 L 3520 0012 035 5
20 L 3552 0230 647 5
21 L 3712 0030 082 5
24 L 3524 0061 174 5
25 L 2986 0052 173 5
1A R 3385 0020 060 5
2A R 3317 0030 090 5
3 R 3479 0023 067 5
4A R 3369 0037 109 5
4B R 3340 0053 160 5
5B R 1677 0025 148 5
6A R 3390 0066 195 5
8 R 2967 0044 149 5
9B R 3410 0048 142 5
12A R 3452 0030 085 5
12B R 3520 0068 192 5
15 R 3333 0099 296 5
22A R 3222 0051 159 5
22B R 3210 0049 151 5
23 R 6610 0108 163 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1677
Table 15 Intense smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2965 054 183 5
2B L 3048 092 301 5
6B L 2696 035 131 5
9A L 2975 038 129 5
10 L 3157 047 148 5
11 L 3218 082 255 5
12C L 3243 015 047 5
17 L 3157 079 250 5
19 L 3119 084 268 5
20 L 3045 056 185 5
21 L 3351 066 198 5
24 L 3195 050 158 5
25 L 3132 054 174 5
1A R 2806 018 065 5
2A R 2885 012 043 5
3 R 2925 040 135 5
4A R 2849 021 074 5
4B R 2917 035 119 5
5B R 3013 023 077 5
6A R 2811 036 129 5
8 R 2819 021 074 5
9B R 2832 032 115 5
12A R 2776 048 171 5
12B R 2970 026 086 5
15 R 2800 035 124 5
22A R 2770 025 091 5
22B R 2768 049 178 5
23 R 1570 060 384 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1777
Table 16 Intense smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2478 034 137 5
2B L 2472 027 111 5
6B L 2367 039 165 5
9A L 2423 065 270 5
10 L 2373 018 077 5
11 L 2568 029 114 5
12C L 2497 028 113 5
17 L 2321 032 139 5
19 L 2488 022 086 5
20 L 2489 056 227 5
21 L 2523 045 177 5
24 L 2470 052 211 5
25 L 2399 089 369 5
1A R 2505 033 131 5
2A R 2485 037 149 5
3 R 2605 031 119 5
4A R 2513 031 125 5
4B R 2542 047 185 5
5B R 2480 022 088 5
6A R 2570 024 092 5
8 R 2532 047 185 5
9B R 2457 044 181 5
12A R 2506 023 093 5
12B R 2523 018 069 5
15 R 2547 039 154 5
22A R 2470 034 138 5
22B R 2466 032 130 5
23 R 2508 030 119 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1877
Table 17 Intense smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 1138 022 191 5
2B L 1154 019 162 5
6B L 1170 008 068 5
9A L 1095 013 114 5
10 L 1138 023 199 5
11 L 1127 016 138 5
12C L 1115 022 199 5
17 L 1110 009 079 5
19 L 1059 011 101 5
20 L 1087 019 176 5
21 L 1121 019 169 5
24 L 1106 027 248 5
25 L 1102 012 105 5
1A R 1111 018 159 5
2A R 1059 014 130 5
3 R 1152 013 110 5
4A R 1078 008 070 5
4B R 1105 016 143 5
5B R 1134 030 267 5
6A R 1136 004 034 5
8 R 1075 015 142 5
9B R 1077 006 054 5
12A R 1102 020 186 5
12B R 1097 016 148 5
15 R 1084 010 091 5
22A R 1112 016 147 5
22B R 1106 014 122 5
23 R 1066 009 088 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1977
Statistical Analysis 4
Exclusion of outliers 41
411 Numerical outlier technique Cochran amp Grubbs test
The statistical evaluation of data for this collaborative study followed the methods provided
by ISO 5725-21 For outlier testing the Grubbs and Cochran methods were used
ISO 5725-2 Tests Consistency
Cochranrsquos ndash test Within-laboratory variability Suitable for detecting whether the highest value in a set of laboratory standard deviations is an outlier or not
Grubbsrsquo ndash test Between-laboratory variability Suitable for detecting whether the highest (or lowest) laboratories averages are outliers or not
The protocol ldquoHarmonized statistical procedurerdquo defined by IUPAC (International Union of
Pure and Applied Chemistry) has been applied as well It consists of sequential applications of
the Cochran and Grubbs tests until no further outliers are detected or until a drop of more than
222 (for this study =29) in the original number of laboratories would occur (see flowchart
in Appendix F)
First apply the Cochran outlier test and if an outlying laboratory is identified then a single
value Grubbs test is performed on the individual values of this outlying laboratory (Individual
Grubbs) If no individual value is identified as outlier the outlying laboratory is removed
When an individual value is identified as an outlier only this value is removed
Afterwards single-value Grubbs test is applied and outlying laboratories are removed If no
laboratory is identified as outlier the pair-value test is applied (two values at the same end)
Remove any laboratory(ies) flagged by these tests but stop removal if more than 222 (2 of
9 laboratories) would be removed
The test was performed with both linear and rotary smoking machines together but also with
rotary respectively linear smoking machines separately The results provided in the report for
all smoking machines respectively with linear or rotary only smoking machines are obtained
after exclusion of the outliers for those respective categories
Note
The paired value Grubbsrsquo test is an extension of the single value Grubbs test for pairs of
outliers The use is advised in ISO 5725 to detect pairs of outlier undetectable sequentially by
using single value Grubbs test
The outlying laboratories are provided in the Tables 18 to 23
Repeatability and reproducibility estimation 42
Repeatability and reproducibility limits are calculated for both smoking regimes each
parameter and for both smoking machine types The results are summarized in tables 18 to 23
with all machines grouped respectively with linear or rotary machines only both with ISO
and intense smoking regimes Outlying laboratories are provided in the same tables The
corresponding graphs named ldquoindividual valuesrdquo are given in Part 5 of this report
1 ISO 5725-21994 Accuracy (trueness and precision) of measurement methods and results ndash Part 2 Basic
method for the determination of repeatability and reproducibility of a standard measurement method
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 2077
Table 18 r amp R estimations for CM8 under ISO smoking regime (all machines)
p n Global Mean Sr CVr[] r SR CVR [] R C GG2 Stragglers Parameter
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 377
Introduction 1
The CORESTA Routine Analytical Chemistry Sub-Group has been given the responsibility to
organize the annual testing of the CORESTA Monitor test piece
The 2016 study was designed
to measure mainstream ISO and Intense smoke yields of nicotine-free dry particulate
matter (NFDPM) nicotine and carbon monoxide (CO) to verify the current monitor test
piece CM8
to determine intra- and inter-laboratory variability for the measured ISO and Intense smoke
yields for the CM8
to verify the conditioned weight for the CM8
Organisation 2
21 Participants
In total 25 laboratories participated in the 2016 study Appendix A lists the participating
laboratories in alphabetical order Note the mix of labs between ISO and Intense differed
25 laboratories delivered data for ISO mainstream smoke for the CM8 test piece using 36
smoking machines (20 rotary smoking machines and 16 linear smoking machines)
20 laboratories delivered data for Intense mainstream smoke for the CM8 test piece using 28
smoking machines (15 rotary smoking machines and 13 linear smoking machines)
One laboratory provided an incomplete data set
Table 1 summarises the number and type of smoking machines used
Table 1 Number of smoking machines
Machine Class ISO Intense
Linear smoking machines 16 13
LX-20 type 2 2
SM450 type 14 11
Rotary smoking machines 20 15
RM20A type 1 1
RM20D type 2 2
RM20H type 5 3
RM200 type 1 1
RM200A type 11 8
Total 36 28
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 477
Table 2 summarises the number of datasets provided for the reported parameters
Table 2 Number of datasets obtained
Physical Parameter
WEIGHT 175
Smoking Parameter ISO Intense
TPM 180 140
WATER 180 140
NIC 180 140
NFDPM 180 140
CO 180 140
PUFF 180 140
Total individual data obtained 1080 840
Total individual data expected 1080 840
A laboratory code number has been assigned in confidence by the study co-ordinator to each
of the individual smoking machines used in the study
22 Protocol
Participants were requested to follow the protocol ldquoAnnual Study of the CORESTA Monitor
Test Piece CM8 - 2016 Experimental Protocolrdquo (provided in Appendix B) to analyse the CM8
test pieces and to report the seven parameters listed in Table 3
Table 3 Parameters to be reported
Parameter Number of replicates Unit Code
Conditioned Weight 5 mgtest piece (tp) WEIGHT
Total Particulate Matter 5 mgtest piece (tp) TPM
Water content (smoke) 5 mgtest piece (tp) WATER
Smoke Nicotine 5 mgtest piece (tp) NIC
Nicotine Free Dry
Particulate Matter 5 mgtest piece (tp) NFDPM
Carbon Monoxide 5 mgtest piece (tp) CO
Puff count 5 pufftest piece (tp) PUFF
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 577
CM8 test pieces should have been smoked under two different mainstream smoking regimes
with a fixed butt length of 32 mm as defined in the following table
Table 4 Mainstream ISO and Intense (Health Canada Intense or HCI) smoking regime
parameters
Smoking
Regime
Puff Volume
(mL)
Puff Frequency
(s)
Puff Duration
(s)
Vent Blocking
()
ISO 35 60 2 0
Intense (HCI) 55 30 2 100
The CM8 test piece was purchased by the participants individually via Borgwaldt KC or
Cerulean
Raw Data 3
Table 5 gives the results for conditioned weight while Tables 6 to 11 list the results for the
reported parameters for ISO smoking regime Tables 12 to 17 list the results for intense
smoking regime Basic statistics (mean and standard deviation) were applied to summarize the
raw data for each smoking machine used and parameters reported for CM8 test piece At this
stage no outlier statistics were applied Appendix D contains the raw data (single values) for
every measured parameter reported by smoking machine included in the study
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 677
Table 5 WEIGHT mean and standard deviation per laboratory code
Lab Code Machine Type Mean SD CV [] Sample size
1A R 96055 2731 0284 5
1B L 96519 3313 0343 5
2A R 94828 2622 0277 5
2B L 95000 5958 0627 5
3 R 90323 3183 0352 5
4A R 96060 2510 0261 5
4B R 96200 6481 0674 5
5A R 96494 1638 0170 5
5B R 95620 2978 0311 5
6A R 96612 4814 0498 5
6B L 96604 2688 0278 5
7A L 95598 3295 0345 5
7B R 95490 3365 0352 5
8 R 96653 2676 0277 5
9A L 95220 2564 0269 5
9B R 95900 2264 0236 5
10 L 96640 2595 0269 5
11 L 95968 8571 0893 5
12A R 95840 4930 0514 5
12B R 96226 2852 0296 5
12C L 95960 2702 0282 5
13A R 95806 2698 0282 5
13B R 95901 5717 0596 5
14 R 96102 3340 0348 5
15 R 95871 4505 0470 5
16 L 96286 4512 0469 5
17 L 95626 3166 0331 5
18 L 95285 3720 0390 5
19 L 95285 3720 0390 5
20 L 95767 5690 0594 5
22A R 96300 1414 0147 5
22B R 96240 1517 0158 5
23 R 94926 3700 0390 5
24 L 95591 5108 0534 5
25 L 96223 5979 0621 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 777
Table 6 ISO smoking regime TPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1793 024 132 5
2B L 1765 063 357 5
6B L 1574 061 387 5
7A L 1804 039 214 5
9A L 1698 033 197 5
10 L 1807 048 265 5
11 L 1828 045 248 5
12C L 1728 055 321 5
16 L 1742 010 058 5
17 L 1616 030 187 5
18 L 1772 036 205 5
19 L 1772 036 205 5
20 L 1783 040 224 5
21 L 1832 050 272 5
24 L 1791 033 185 5
25 L 1607 079 494 5
1A R 1749 024 135 5
2A R 1698 028 166 5
3 R 1760 019 107 5
4A R 1723 028 165 5
4B R 1769 038 212 5
5A R 1703 022 127 5
5B R 1724 031 178 5
6A R 1740 031 176 5
7B R 1646 017 103 5
8 R 1737 022 125 5
9B R 1711 025 147 5
12A R 1758 040 227 5
12B R 1790 014 078 5
13A R 1674 017 104 5
13B R 1700 020 115 5
14 R 1746 044 254 5
15 R 1719 041 238 5
22A R 1752 020 115 5
22B R 1731 022 129 5
23 R 1651 037 226 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 877
Table 7 ISO Smoking regime WATER mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 161 007 428 5
2B L 145 008 518 5
6B L 118 014 1213 5
7A L 175 006 364 5
9A L 142 011 802 5
10 L 177 010 581 5
11 L 142 009 632 5
12C L 122 008 645 5
16 L 142 012 872 5
17 L 145 026 1823 5
18 L 147 019 1299 5
19 L 147 019 1299 5
20 L 214 013 611 5
21 L 120 024 2024 5
24 L 156 009 551 5
25 L 127 016 1261 5
1A R 215 007 316 5
2A R 174 008 444 5
3 R 196 010 493 5
4A R 197 008 406 5
4B R 213 013 629 5
5A R 197 009 471 5
5B R 192 008 419 5
6A R 227 010 445 5
7B R 184 007 396 5
8 R 206 013 637 5
9B R 203 012 579 5
12A R 250 012 464 5
12B R 244 010 430 5
13A R 205 007 362 5
13B R 204 012 576 5
14 R 228 017 739 5
15 R 188 016 834 5
22A R 219 007 337 5
22B R 215 005 225 5
23 R 179 003 179 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 977
Table 8 ISO Smoking regime Nicotine mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1704 0029 170 5
2B L 1706 0039 227 5
6B L 1624 0048 295 5
7A L 1687 0033 194 5
9A L 1612 0200 1240 5
10 L 1748 0070 401 5
11 L 1691 0028 166 5
12C L 1669 0034 206 5
16 L 1731 0028 159 5
17 L 1674 0046 276 5
18 L 1697 0014 082 5
19 L 1697 0014 082 5
20 L 1734 0021 124 5
21 L 1812 0048 266 5
24 L 1694 0037 217 5
25 L 1743 0154 883 5
1A R 1669 0023 141 5
2A R 1638 0037 224 5
3 R 1652 0018 110 5
4A R 1630 0042 255 5
4B R 1653 0035 214 5
5A R 1612 0023 142 5
5B R 1602 0023 141 5
6A R 1661 0037 225 5
7B R 1564 0022 140 5
8 R 1535 0031 204 5
9B R 1659 0047 285 5
12A R 1719 0024 142 5
12B R 1718 0037 216 5
13A R 1497 0024 163 5
13B R 1546 0013 086 5
14 R 1590 0035 217 5
15 R 1651 0030 181 5
22A R 1612 0011 068 5
22B R 1630 0012 075 5
23 R 1639 0026 159 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1077
Table 9 ISO smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1462 016 111 5
2B L 1449 053 366 5
6B L 1294 044 344 5
7A L 1460 031 214 5
9A L 1395 011 080 5
10 L 1455 039 269 5
11 L 1518 036 236 5
12C L 1439 049 338 5
16 L 1427 013 092 5
17 L 1304 054 413 5
18 L 1456 020 135 5
19 L 1456 020 135 5
20 L 1395 036 255 5
21 L 1531 057 371 5
24 L 1466 023 154 5
25 L 1306 066 509 5
1A R 1367 020 145 5
2A R 1361 023 169 5
3 R 1398 012 083 5
4A R 1363 024 176 5
4B R 1391 028 201 5
5A R 1347 014 107 5
5B R 1372 023 166 5
6A R 1346 019 142 5
7B R 1305 020 153 5
8 R 1378 026 192 5
9B R 1342 015 114 5
12A R 1337 037 278 5
12B R 1375 018 129 5
13A R 1319 015 112 5
13B R 1341 009 069 5
14 R 1359 028 204 5
15 R 1366 029 214 5
22A R 1371 019 136 5
22B R 1353 024 175 5
23 R 1308 037 283 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1177
Table 10 ISO Smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1335 020 150 5
2B L 1297 037 288 5
6B L 1260 099 790 5
7A L 1374 034 249 5
9A L 1233 019 153 5
10 L 1219 054 445 5
11 L 1267 044 350 5
12C L 1325 033 248 5
16 L 1307 024 185 5
17 L 1196 029 242 5
18 L 1335 010 072 5
19 L 1335 010 072 5
20 L 1324 033 248 5
21 L 1363 032 238 5
24 L 1263 040 315 5
25 L 1194 069 574 5
1A R 1368 010 076 5
2A R 1308 018 135 5
3 R 1345 023 172 5
4A R 1340 011 079 5
4B R 1394 041 294 5
5A R 1292 028 216 5
5B R 1360 034 251 5
6A R 1372 023 166 5
7B R 1291 013 098 5
8 R 1369 025 183 5
9B R 1276 023 182 5
12A R 1317 034 256 5
12B R 1375 024 175 5
13A R 1334 021 155 5
13B R 1338 030 227 5
14 R 1366 023 167 5
15 R 1377 019 139 5
22A R 1344 016 118 5
22B R 1341 016 116 5
23 R 1334 029 217 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1277
Table 11 ISO Smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 796 005 059 5
2B L 806 012 144 5
6B L 814 018 219 5
7A L 789 009 112 5
9A L 781 024 306 5
10 L 802 020 245 5
11 L 784 018 225 5
12C L 794 021 263 5
16 L 850 014 168 5
17 L 774 016 203 5
18 L 787 015 187 5
19 L 787 015 187 5
20 L 769 014 188 5
21 L 808 008 097 5
24 L 792 010 128 5
25 L 751 030 400 5
1A R 767 005 068 5
2A R 727 008 109 5
3 R 779 008 099 5
4A R 748 011 146 5
4B R 758 013 172 5
5A R 782 011 144 5
5B R 766 017 216 5
6A R 773 009 117 5
7B R 716 011 160 5
8 R 754 010 127 5
9B R 755 008 107 5
12A R 755 006 078 5
12B R 771 008 102 5
13A R 740 017 225 5
13B R 769 007 091 5
14 R 761 011 140 5
15 R 750 018 246 5
22A R 757 008 110 5
22B R 759 007 088 5
23 R 732 009 117 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1377
Table 12 Intense smoking regime TPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 4551 091 200 5
2B L 4391 078 178 5
6B L 3936 067 170 5
9A L 4471 060 134 5
10 L 4667 073 157 5
11 L 5068 136 269 5
12C L 4644 031 066 5
17 L 4346 106 243 5
19 L 4566 087 190 5
20 L 4616 122 265 5
21 L 5008 077 153 5
24 L 4782 094 196 5
25 L 4434 081 182 5
1A R 4168 016 039 5
2A R 4014 024 061 5
3 R 4247 035 083 5
4A R 4097 039 095 5
4B R 4181 064 153 5
5B R 3997 040 101 5
6A R 4076 074 181 5
8 R 4044 043 107 5
9B R 4097 033 080 5
12A R 4125 046 112 5
12B R 4257 039 092 5
15 R 3957 052 131 5
22A R 4046 028 069 5
22B R 4015 045 112 5
23 R 3830 073 192 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1477
Table 13 Intense smoking regime Water mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1237 038 305 5
2B L 999 037 375 5
6B L 906 034 381 5
9A L 1147 043 373 5
10 L 1152 052 453 5
11 L 1488 053 356 5
12C L 1061 019 179 5
17 L 1027 028 274 5
19 L 1095 038 348 5
20 L 1216 083 681 5
21 L 1285 026 206 5
24 L 1235 060 484 5
25 L 1004 031 307 5
1A R 1024 014 138 5
2A R 797 016 197 5
3 R 974 031 317 5
4A R 911 034 368 5
4B R 931 027 287 5
5B R 815 041 507 5
6A R 923 038 411 5
8 R 929 033 354 5
9B R 927 028 301 5
12A R 1004 051 508 5
12B R 935 017 181 5
15 R 823 029 349 5
22A R 953 005 052 5
22B R 926 038 410 5
23 R 1598 065 404 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1577
Table 14 Intense smoking regime Nicotine mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 3484 0055 158 5
2B L 3434 0048 141 5
6B L 3342 0051 153 5
9A L 3494 0089 255 5
10 L 3578 0226 633 5
11 L 3620 0082 225 5
12C L 3402 0024 070 5
17 L 3622 0075 208 5
19 L 3520 0012 035 5
20 L 3552 0230 647 5
21 L 3712 0030 082 5
24 L 3524 0061 174 5
25 L 2986 0052 173 5
1A R 3385 0020 060 5
2A R 3317 0030 090 5
3 R 3479 0023 067 5
4A R 3369 0037 109 5
4B R 3340 0053 160 5
5B R 1677 0025 148 5
6A R 3390 0066 195 5
8 R 2967 0044 149 5
9B R 3410 0048 142 5
12A R 3452 0030 085 5
12B R 3520 0068 192 5
15 R 3333 0099 296 5
22A R 3222 0051 159 5
22B R 3210 0049 151 5
23 R 6610 0108 163 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1677
Table 15 Intense smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2965 054 183 5
2B L 3048 092 301 5
6B L 2696 035 131 5
9A L 2975 038 129 5
10 L 3157 047 148 5
11 L 3218 082 255 5
12C L 3243 015 047 5
17 L 3157 079 250 5
19 L 3119 084 268 5
20 L 3045 056 185 5
21 L 3351 066 198 5
24 L 3195 050 158 5
25 L 3132 054 174 5
1A R 2806 018 065 5
2A R 2885 012 043 5
3 R 2925 040 135 5
4A R 2849 021 074 5
4B R 2917 035 119 5
5B R 3013 023 077 5
6A R 2811 036 129 5
8 R 2819 021 074 5
9B R 2832 032 115 5
12A R 2776 048 171 5
12B R 2970 026 086 5
15 R 2800 035 124 5
22A R 2770 025 091 5
22B R 2768 049 178 5
23 R 1570 060 384 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1777
Table 16 Intense smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2478 034 137 5
2B L 2472 027 111 5
6B L 2367 039 165 5
9A L 2423 065 270 5
10 L 2373 018 077 5
11 L 2568 029 114 5
12C L 2497 028 113 5
17 L 2321 032 139 5
19 L 2488 022 086 5
20 L 2489 056 227 5
21 L 2523 045 177 5
24 L 2470 052 211 5
25 L 2399 089 369 5
1A R 2505 033 131 5
2A R 2485 037 149 5
3 R 2605 031 119 5
4A R 2513 031 125 5
4B R 2542 047 185 5
5B R 2480 022 088 5
6A R 2570 024 092 5
8 R 2532 047 185 5
9B R 2457 044 181 5
12A R 2506 023 093 5
12B R 2523 018 069 5
15 R 2547 039 154 5
22A R 2470 034 138 5
22B R 2466 032 130 5
23 R 2508 030 119 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1877
Table 17 Intense smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 1138 022 191 5
2B L 1154 019 162 5
6B L 1170 008 068 5
9A L 1095 013 114 5
10 L 1138 023 199 5
11 L 1127 016 138 5
12C L 1115 022 199 5
17 L 1110 009 079 5
19 L 1059 011 101 5
20 L 1087 019 176 5
21 L 1121 019 169 5
24 L 1106 027 248 5
25 L 1102 012 105 5
1A R 1111 018 159 5
2A R 1059 014 130 5
3 R 1152 013 110 5
4A R 1078 008 070 5
4B R 1105 016 143 5
5B R 1134 030 267 5
6A R 1136 004 034 5
8 R 1075 015 142 5
9B R 1077 006 054 5
12A R 1102 020 186 5
12B R 1097 016 148 5
15 R 1084 010 091 5
22A R 1112 016 147 5
22B R 1106 014 122 5
23 R 1066 009 088 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1977
Statistical Analysis 4
Exclusion of outliers 41
411 Numerical outlier technique Cochran amp Grubbs test
The statistical evaluation of data for this collaborative study followed the methods provided
by ISO 5725-21 For outlier testing the Grubbs and Cochran methods were used
ISO 5725-2 Tests Consistency
Cochranrsquos ndash test Within-laboratory variability Suitable for detecting whether the highest value in a set of laboratory standard deviations is an outlier or not
Grubbsrsquo ndash test Between-laboratory variability Suitable for detecting whether the highest (or lowest) laboratories averages are outliers or not
The protocol ldquoHarmonized statistical procedurerdquo defined by IUPAC (International Union of
Pure and Applied Chemistry) has been applied as well It consists of sequential applications of
the Cochran and Grubbs tests until no further outliers are detected or until a drop of more than
222 (for this study =29) in the original number of laboratories would occur (see flowchart
in Appendix F)
First apply the Cochran outlier test and if an outlying laboratory is identified then a single
value Grubbs test is performed on the individual values of this outlying laboratory (Individual
Grubbs) If no individual value is identified as outlier the outlying laboratory is removed
When an individual value is identified as an outlier only this value is removed
Afterwards single-value Grubbs test is applied and outlying laboratories are removed If no
laboratory is identified as outlier the pair-value test is applied (two values at the same end)
Remove any laboratory(ies) flagged by these tests but stop removal if more than 222 (2 of
9 laboratories) would be removed
The test was performed with both linear and rotary smoking machines together but also with
rotary respectively linear smoking machines separately The results provided in the report for
all smoking machines respectively with linear or rotary only smoking machines are obtained
after exclusion of the outliers for those respective categories
Note
The paired value Grubbsrsquo test is an extension of the single value Grubbs test for pairs of
outliers The use is advised in ISO 5725 to detect pairs of outlier undetectable sequentially by
using single value Grubbs test
The outlying laboratories are provided in the Tables 18 to 23
Repeatability and reproducibility estimation 42
Repeatability and reproducibility limits are calculated for both smoking regimes each
parameter and for both smoking machine types The results are summarized in tables 18 to 23
with all machines grouped respectively with linear or rotary machines only both with ISO
and intense smoking regimes Outlying laboratories are provided in the same tables The
corresponding graphs named ldquoindividual valuesrdquo are given in Part 5 of this report
1 ISO 5725-21994 Accuracy (trueness and precision) of measurement methods and results ndash Part 2 Basic
method for the determination of repeatability and reproducibility of a standard measurement method
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 2077
Table 18 r amp R estimations for CM8 under ISO smoking regime (all machines)
p n Global Mean Sr CVr[] r SR CVR [] R C GG2 Stragglers Parameter
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 477
Table 2 summarises the number of datasets provided for the reported parameters
Table 2 Number of datasets obtained
Physical Parameter
WEIGHT 175
Smoking Parameter ISO Intense
TPM 180 140
WATER 180 140
NIC 180 140
NFDPM 180 140
CO 180 140
PUFF 180 140
Total individual data obtained 1080 840
Total individual data expected 1080 840
A laboratory code number has been assigned in confidence by the study co-ordinator to each
of the individual smoking machines used in the study
22 Protocol
Participants were requested to follow the protocol ldquoAnnual Study of the CORESTA Monitor
Test Piece CM8 - 2016 Experimental Protocolrdquo (provided in Appendix B) to analyse the CM8
test pieces and to report the seven parameters listed in Table 3
Table 3 Parameters to be reported
Parameter Number of replicates Unit Code
Conditioned Weight 5 mgtest piece (tp) WEIGHT
Total Particulate Matter 5 mgtest piece (tp) TPM
Water content (smoke) 5 mgtest piece (tp) WATER
Smoke Nicotine 5 mgtest piece (tp) NIC
Nicotine Free Dry
Particulate Matter 5 mgtest piece (tp) NFDPM
Carbon Monoxide 5 mgtest piece (tp) CO
Puff count 5 pufftest piece (tp) PUFF
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 577
CM8 test pieces should have been smoked under two different mainstream smoking regimes
with a fixed butt length of 32 mm as defined in the following table
Table 4 Mainstream ISO and Intense (Health Canada Intense or HCI) smoking regime
parameters
Smoking
Regime
Puff Volume
(mL)
Puff Frequency
(s)
Puff Duration
(s)
Vent Blocking
()
ISO 35 60 2 0
Intense (HCI) 55 30 2 100
The CM8 test piece was purchased by the participants individually via Borgwaldt KC or
Cerulean
Raw Data 3
Table 5 gives the results for conditioned weight while Tables 6 to 11 list the results for the
reported parameters for ISO smoking regime Tables 12 to 17 list the results for intense
smoking regime Basic statistics (mean and standard deviation) were applied to summarize the
raw data for each smoking machine used and parameters reported for CM8 test piece At this
stage no outlier statistics were applied Appendix D contains the raw data (single values) for
every measured parameter reported by smoking machine included in the study
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 677
Table 5 WEIGHT mean and standard deviation per laboratory code
Lab Code Machine Type Mean SD CV [] Sample size
1A R 96055 2731 0284 5
1B L 96519 3313 0343 5
2A R 94828 2622 0277 5
2B L 95000 5958 0627 5
3 R 90323 3183 0352 5
4A R 96060 2510 0261 5
4B R 96200 6481 0674 5
5A R 96494 1638 0170 5
5B R 95620 2978 0311 5
6A R 96612 4814 0498 5
6B L 96604 2688 0278 5
7A L 95598 3295 0345 5
7B R 95490 3365 0352 5
8 R 96653 2676 0277 5
9A L 95220 2564 0269 5
9B R 95900 2264 0236 5
10 L 96640 2595 0269 5
11 L 95968 8571 0893 5
12A R 95840 4930 0514 5
12B R 96226 2852 0296 5
12C L 95960 2702 0282 5
13A R 95806 2698 0282 5
13B R 95901 5717 0596 5
14 R 96102 3340 0348 5
15 R 95871 4505 0470 5
16 L 96286 4512 0469 5
17 L 95626 3166 0331 5
18 L 95285 3720 0390 5
19 L 95285 3720 0390 5
20 L 95767 5690 0594 5
22A R 96300 1414 0147 5
22B R 96240 1517 0158 5
23 R 94926 3700 0390 5
24 L 95591 5108 0534 5
25 L 96223 5979 0621 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 777
Table 6 ISO smoking regime TPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1793 024 132 5
2B L 1765 063 357 5
6B L 1574 061 387 5
7A L 1804 039 214 5
9A L 1698 033 197 5
10 L 1807 048 265 5
11 L 1828 045 248 5
12C L 1728 055 321 5
16 L 1742 010 058 5
17 L 1616 030 187 5
18 L 1772 036 205 5
19 L 1772 036 205 5
20 L 1783 040 224 5
21 L 1832 050 272 5
24 L 1791 033 185 5
25 L 1607 079 494 5
1A R 1749 024 135 5
2A R 1698 028 166 5
3 R 1760 019 107 5
4A R 1723 028 165 5
4B R 1769 038 212 5
5A R 1703 022 127 5
5B R 1724 031 178 5
6A R 1740 031 176 5
7B R 1646 017 103 5
8 R 1737 022 125 5
9B R 1711 025 147 5
12A R 1758 040 227 5
12B R 1790 014 078 5
13A R 1674 017 104 5
13B R 1700 020 115 5
14 R 1746 044 254 5
15 R 1719 041 238 5
22A R 1752 020 115 5
22B R 1731 022 129 5
23 R 1651 037 226 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 877
Table 7 ISO Smoking regime WATER mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 161 007 428 5
2B L 145 008 518 5
6B L 118 014 1213 5
7A L 175 006 364 5
9A L 142 011 802 5
10 L 177 010 581 5
11 L 142 009 632 5
12C L 122 008 645 5
16 L 142 012 872 5
17 L 145 026 1823 5
18 L 147 019 1299 5
19 L 147 019 1299 5
20 L 214 013 611 5
21 L 120 024 2024 5
24 L 156 009 551 5
25 L 127 016 1261 5
1A R 215 007 316 5
2A R 174 008 444 5
3 R 196 010 493 5
4A R 197 008 406 5
4B R 213 013 629 5
5A R 197 009 471 5
5B R 192 008 419 5
6A R 227 010 445 5
7B R 184 007 396 5
8 R 206 013 637 5
9B R 203 012 579 5
12A R 250 012 464 5
12B R 244 010 430 5
13A R 205 007 362 5
13B R 204 012 576 5
14 R 228 017 739 5
15 R 188 016 834 5
22A R 219 007 337 5
22B R 215 005 225 5
23 R 179 003 179 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 977
Table 8 ISO Smoking regime Nicotine mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1704 0029 170 5
2B L 1706 0039 227 5
6B L 1624 0048 295 5
7A L 1687 0033 194 5
9A L 1612 0200 1240 5
10 L 1748 0070 401 5
11 L 1691 0028 166 5
12C L 1669 0034 206 5
16 L 1731 0028 159 5
17 L 1674 0046 276 5
18 L 1697 0014 082 5
19 L 1697 0014 082 5
20 L 1734 0021 124 5
21 L 1812 0048 266 5
24 L 1694 0037 217 5
25 L 1743 0154 883 5
1A R 1669 0023 141 5
2A R 1638 0037 224 5
3 R 1652 0018 110 5
4A R 1630 0042 255 5
4B R 1653 0035 214 5
5A R 1612 0023 142 5
5B R 1602 0023 141 5
6A R 1661 0037 225 5
7B R 1564 0022 140 5
8 R 1535 0031 204 5
9B R 1659 0047 285 5
12A R 1719 0024 142 5
12B R 1718 0037 216 5
13A R 1497 0024 163 5
13B R 1546 0013 086 5
14 R 1590 0035 217 5
15 R 1651 0030 181 5
22A R 1612 0011 068 5
22B R 1630 0012 075 5
23 R 1639 0026 159 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1077
Table 9 ISO smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1462 016 111 5
2B L 1449 053 366 5
6B L 1294 044 344 5
7A L 1460 031 214 5
9A L 1395 011 080 5
10 L 1455 039 269 5
11 L 1518 036 236 5
12C L 1439 049 338 5
16 L 1427 013 092 5
17 L 1304 054 413 5
18 L 1456 020 135 5
19 L 1456 020 135 5
20 L 1395 036 255 5
21 L 1531 057 371 5
24 L 1466 023 154 5
25 L 1306 066 509 5
1A R 1367 020 145 5
2A R 1361 023 169 5
3 R 1398 012 083 5
4A R 1363 024 176 5
4B R 1391 028 201 5
5A R 1347 014 107 5
5B R 1372 023 166 5
6A R 1346 019 142 5
7B R 1305 020 153 5
8 R 1378 026 192 5
9B R 1342 015 114 5
12A R 1337 037 278 5
12B R 1375 018 129 5
13A R 1319 015 112 5
13B R 1341 009 069 5
14 R 1359 028 204 5
15 R 1366 029 214 5
22A R 1371 019 136 5
22B R 1353 024 175 5
23 R 1308 037 283 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1177
Table 10 ISO Smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1335 020 150 5
2B L 1297 037 288 5
6B L 1260 099 790 5
7A L 1374 034 249 5
9A L 1233 019 153 5
10 L 1219 054 445 5
11 L 1267 044 350 5
12C L 1325 033 248 5
16 L 1307 024 185 5
17 L 1196 029 242 5
18 L 1335 010 072 5
19 L 1335 010 072 5
20 L 1324 033 248 5
21 L 1363 032 238 5
24 L 1263 040 315 5
25 L 1194 069 574 5
1A R 1368 010 076 5
2A R 1308 018 135 5
3 R 1345 023 172 5
4A R 1340 011 079 5
4B R 1394 041 294 5
5A R 1292 028 216 5
5B R 1360 034 251 5
6A R 1372 023 166 5
7B R 1291 013 098 5
8 R 1369 025 183 5
9B R 1276 023 182 5
12A R 1317 034 256 5
12B R 1375 024 175 5
13A R 1334 021 155 5
13B R 1338 030 227 5
14 R 1366 023 167 5
15 R 1377 019 139 5
22A R 1344 016 118 5
22B R 1341 016 116 5
23 R 1334 029 217 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1277
Table 11 ISO Smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 796 005 059 5
2B L 806 012 144 5
6B L 814 018 219 5
7A L 789 009 112 5
9A L 781 024 306 5
10 L 802 020 245 5
11 L 784 018 225 5
12C L 794 021 263 5
16 L 850 014 168 5
17 L 774 016 203 5
18 L 787 015 187 5
19 L 787 015 187 5
20 L 769 014 188 5
21 L 808 008 097 5
24 L 792 010 128 5
25 L 751 030 400 5
1A R 767 005 068 5
2A R 727 008 109 5
3 R 779 008 099 5
4A R 748 011 146 5
4B R 758 013 172 5
5A R 782 011 144 5
5B R 766 017 216 5
6A R 773 009 117 5
7B R 716 011 160 5
8 R 754 010 127 5
9B R 755 008 107 5
12A R 755 006 078 5
12B R 771 008 102 5
13A R 740 017 225 5
13B R 769 007 091 5
14 R 761 011 140 5
15 R 750 018 246 5
22A R 757 008 110 5
22B R 759 007 088 5
23 R 732 009 117 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1377
Table 12 Intense smoking regime TPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 4551 091 200 5
2B L 4391 078 178 5
6B L 3936 067 170 5
9A L 4471 060 134 5
10 L 4667 073 157 5
11 L 5068 136 269 5
12C L 4644 031 066 5
17 L 4346 106 243 5
19 L 4566 087 190 5
20 L 4616 122 265 5
21 L 5008 077 153 5
24 L 4782 094 196 5
25 L 4434 081 182 5
1A R 4168 016 039 5
2A R 4014 024 061 5
3 R 4247 035 083 5
4A R 4097 039 095 5
4B R 4181 064 153 5
5B R 3997 040 101 5
6A R 4076 074 181 5
8 R 4044 043 107 5
9B R 4097 033 080 5
12A R 4125 046 112 5
12B R 4257 039 092 5
15 R 3957 052 131 5
22A R 4046 028 069 5
22B R 4015 045 112 5
23 R 3830 073 192 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1477
Table 13 Intense smoking regime Water mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1237 038 305 5
2B L 999 037 375 5
6B L 906 034 381 5
9A L 1147 043 373 5
10 L 1152 052 453 5
11 L 1488 053 356 5
12C L 1061 019 179 5
17 L 1027 028 274 5
19 L 1095 038 348 5
20 L 1216 083 681 5
21 L 1285 026 206 5
24 L 1235 060 484 5
25 L 1004 031 307 5
1A R 1024 014 138 5
2A R 797 016 197 5
3 R 974 031 317 5
4A R 911 034 368 5
4B R 931 027 287 5
5B R 815 041 507 5
6A R 923 038 411 5
8 R 929 033 354 5
9B R 927 028 301 5
12A R 1004 051 508 5
12B R 935 017 181 5
15 R 823 029 349 5
22A R 953 005 052 5
22B R 926 038 410 5
23 R 1598 065 404 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1577
Table 14 Intense smoking regime Nicotine mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 3484 0055 158 5
2B L 3434 0048 141 5
6B L 3342 0051 153 5
9A L 3494 0089 255 5
10 L 3578 0226 633 5
11 L 3620 0082 225 5
12C L 3402 0024 070 5
17 L 3622 0075 208 5
19 L 3520 0012 035 5
20 L 3552 0230 647 5
21 L 3712 0030 082 5
24 L 3524 0061 174 5
25 L 2986 0052 173 5
1A R 3385 0020 060 5
2A R 3317 0030 090 5
3 R 3479 0023 067 5
4A R 3369 0037 109 5
4B R 3340 0053 160 5
5B R 1677 0025 148 5
6A R 3390 0066 195 5
8 R 2967 0044 149 5
9B R 3410 0048 142 5
12A R 3452 0030 085 5
12B R 3520 0068 192 5
15 R 3333 0099 296 5
22A R 3222 0051 159 5
22B R 3210 0049 151 5
23 R 6610 0108 163 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1677
Table 15 Intense smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2965 054 183 5
2B L 3048 092 301 5
6B L 2696 035 131 5
9A L 2975 038 129 5
10 L 3157 047 148 5
11 L 3218 082 255 5
12C L 3243 015 047 5
17 L 3157 079 250 5
19 L 3119 084 268 5
20 L 3045 056 185 5
21 L 3351 066 198 5
24 L 3195 050 158 5
25 L 3132 054 174 5
1A R 2806 018 065 5
2A R 2885 012 043 5
3 R 2925 040 135 5
4A R 2849 021 074 5
4B R 2917 035 119 5
5B R 3013 023 077 5
6A R 2811 036 129 5
8 R 2819 021 074 5
9B R 2832 032 115 5
12A R 2776 048 171 5
12B R 2970 026 086 5
15 R 2800 035 124 5
22A R 2770 025 091 5
22B R 2768 049 178 5
23 R 1570 060 384 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1777
Table 16 Intense smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2478 034 137 5
2B L 2472 027 111 5
6B L 2367 039 165 5
9A L 2423 065 270 5
10 L 2373 018 077 5
11 L 2568 029 114 5
12C L 2497 028 113 5
17 L 2321 032 139 5
19 L 2488 022 086 5
20 L 2489 056 227 5
21 L 2523 045 177 5
24 L 2470 052 211 5
25 L 2399 089 369 5
1A R 2505 033 131 5
2A R 2485 037 149 5
3 R 2605 031 119 5
4A R 2513 031 125 5
4B R 2542 047 185 5
5B R 2480 022 088 5
6A R 2570 024 092 5
8 R 2532 047 185 5
9B R 2457 044 181 5
12A R 2506 023 093 5
12B R 2523 018 069 5
15 R 2547 039 154 5
22A R 2470 034 138 5
22B R 2466 032 130 5
23 R 2508 030 119 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1877
Table 17 Intense smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 1138 022 191 5
2B L 1154 019 162 5
6B L 1170 008 068 5
9A L 1095 013 114 5
10 L 1138 023 199 5
11 L 1127 016 138 5
12C L 1115 022 199 5
17 L 1110 009 079 5
19 L 1059 011 101 5
20 L 1087 019 176 5
21 L 1121 019 169 5
24 L 1106 027 248 5
25 L 1102 012 105 5
1A R 1111 018 159 5
2A R 1059 014 130 5
3 R 1152 013 110 5
4A R 1078 008 070 5
4B R 1105 016 143 5
5B R 1134 030 267 5
6A R 1136 004 034 5
8 R 1075 015 142 5
9B R 1077 006 054 5
12A R 1102 020 186 5
12B R 1097 016 148 5
15 R 1084 010 091 5
22A R 1112 016 147 5
22B R 1106 014 122 5
23 R 1066 009 088 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1977
Statistical Analysis 4
Exclusion of outliers 41
411 Numerical outlier technique Cochran amp Grubbs test
The statistical evaluation of data for this collaborative study followed the methods provided
by ISO 5725-21 For outlier testing the Grubbs and Cochran methods were used
ISO 5725-2 Tests Consistency
Cochranrsquos ndash test Within-laboratory variability Suitable for detecting whether the highest value in a set of laboratory standard deviations is an outlier or not
Grubbsrsquo ndash test Between-laboratory variability Suitable for detecting whether the highest (or lowest) laboratories averages are outliers or not
The protocol ldquoHarmonized statistical procedurerdquo defined by IUPAC (International Union of
Pure and Applied Chemistry) has been applied as well It consists of sequential applications of
the Cochran and Grubbs tests until no further outliers are detected or until a drop of more than
222 (for this study =29) in the original number of laboratories would occur (see flowchart
in Appendix F)
First apply the Cochran outlier test and if an outlying laboratory is identified then a single
value Grubbs test is performed on the individual values of this outlying laboratory (Individual
Grubbs) If no individual value is identified as outlier the outlying laboratory is removed
When an individual value is identified as an outlier only this value is removed
Afterwards single-value Grubbs test is applied and outlying laboratories are removed If no
laboratory is identified as outlier the pair-value test is applied (two values at the same end)
Remove any laboratory(ies) flagged by these tests but stop removal if more than 222 (2 of
9 laboratories) would be removed
The test was performed with both linear and rotary smoking machines together but also with
rotary respectively linear smoking machines separately The results provided in the report for
all smoking machines respectively with linear or rotary only smoking machines are obtained
after exclusion of the outliers for those respective categories
Note
The paired value Grubbsrsquo test is an extension of the single value Grubbs test for pairs of
outliers The use is advised in ISO 5725 to detect pairs of outlier undetectable sequentially by
using single value Grubbs test
The outlying laboratories are provided in the Tables 18 to 23
Repeatability and reproducibility estimation 42
Repeatability and reproducibility limits are calculated for both smoking regimes each
parameter and for both smoking machine types The results are summarized in tables 18 to 23
with all machines grouped respectively with linear or rotary machines only both with ISO
and intense smoking regimes Outlying laboratories are provided in the same tables The
corresponding graphs named ldquoindividual valuesrdquo are given in Part 5 of this report
1 ISO 5725-21994 Accuracy (trueness and precision) of measurement methods and results ndash Part 2 Basic
method for the determination of repeatability and reproducibility of a standard measurement method
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 2077
Table 18 r amp R estimations for CM8 under ISO smoking regime (all machines)
p n Global Mean Sr CVr[] r SR CVR [] R C GG2 Stragglers Parameter
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 577
CM8 test pieces should have been smoked under two different mainstream smoking regimes
with a fixed butt length of 32 mm as defined in the following table
Table 4 Mainstream ISO and Intense (Health Canada Intense or HCI) smoking regime
parameters
Smoking
Regime
Puff Volume
(mL)
Puff Frequency
(s)
Puff Duration
(s)
Vent Blocking
()
ISO 35 60 2 0
Intense (HCI) 55 30 2 100
The CM8 test piece was purchased by the participants individually via Borgwaldt KC or
Cerulean
Raw Data 3
Table 5 gives the results for conditioned weight while Tables 6 to 11 list the results for the
reported parameters for ISO smoking regime Tables 12 to 17 list the results for intense
smoking regime Basic statistics (mean and standard deviation) were applied to summarize the
raw data for each smoking machine used and parameters reported for CM8 test piece At this
stage no outlier statistics were applied Appendix D contains the raw data (single values) for
every measured parameter reported by smoking machine included in the study
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 677
Table 5 WEIGHT mean and standard deviation per laboratory code
Lab Code Machine Type Mean SD CV [] Sample size
1A R 96055 2731 0284 5
1B L 96519 3313 0343 5
2A R 94828 2622 0277 5
2B L 95000 5958 0627 5
3 R 90323 3183 0352 5
4A R 96060 2510 0261 5
4B R 96200 6481 0674 5
5A R 96494 1638 0170 5
5B R 95620 2978 0311 5
6A R 96612 4814 0498 5
6B L 96604 2688 0278 5
7A L 95598 3295 0345 5
7B R 95490 3365 0352 5
8 R 96653 2676 0277 5
9A L 95220 2564 0269 5
9B R 95900 2264 0236 5
10 L 96640 2595 0269 5
11 L 95968 8571 0893 5
12A R 95840 4930 0514 5
12B R 96226 2852 0296 5
12C L 95960 2702 0282 5
13A R 95806 2698 0282 5
13B R 95901 5717 0596 5
14 R 96102 3340 0348 5
15 R 95871 4505 0470 5
16 L 96286 4512 0469 5
17 L 95626 3166 0331 5
18 L 95285 3720 0390 5
19 L 95285 3720 0390 5
20 L 95767 5690 0594 5
22A R 96300 1414 0147 5
22B R 96240 1517 0158 5
23 R 94926 3700 0390 5
24 L 95591 5108 0534 5
25 L 96223 5979 0621 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 777
Table 6 ISO smoking regime TPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1793 024 132 5
2B L 1765 063 357 5
6B L 1574 061 387 5
7A L 1804 039 214 5
9A L 1698 033 197 5
10 L 1807 048 265 5
11 L 1828 045 248 5
12C L 1728 055 321 5
16 L 1742 010 058 5
17 L 1616 030 187 5
18 L 1772 036 205 5
19 L 1772 036 205 5
20 L 1783 040 224 5
21 L 1832 050 272 5
24 L 1791 033 185 5
25 L 1607 079 494 5
1A R 1749 024 135 5
2A R 1698 028 166 5
3 R 1760 019 107 5
4A R 1723 028 165 5
4B R 1769 038 212 5
5A R 1703 022 127 5
5B R 1724 031 178 5
6A R 1740 031 176 5
7B R 1646 017 103 5
8 R 1737 022 125 5
9B R 1711 025 147 5
12A R 1758 040 227 5
12B R 1790 014 078 5
13A R 1674 017 104 5
13B R 1700 020 115 5
14 R 1746 044 254 5
15 R 1719 041 238 5
22A R 1752 020 115 5
22B R 1731 022 129 5
23 R 1651 037 226 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 877
Table 7 ISO Smoking regime WATER mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 161 007 428 5
2B L 145 008 518 5
6B L 118 014 1213 5
7A L 175 006 364 5
9A L 142 011 802 5
10 L 177 010 581 5
11 L 142 009 632 5
12C L 122 008 645 5
16 L 142 012 872 5
17 L 145 026 1823 5
18 L 147 019 1299 5
19 L 147 019 1299 5
20 L 214 013 611 5
21 L 120 024 2024 5
24 L 156 009 551 5
25 L 127 016 1261 5
1A R 215 007 316 5
2A R 174 008 444 5
3 R 196 010 493 5
4A R 197 008 406 5
4B R 213 013 629 5
5A R 197 009 471 5
5B R 192 008 419 5
6A R 227 010 445 5
7B R 184 007 396 5
8 R 206 013 637 5
9B R 203 012 579 5
12A R 250 012 464 5
12B R 244 010 430 5
13A R 205 007 362 5
13B R 204 012 576 5
14 R 228 017 739 5
15 R 188 016 834 5
22A R 219 007 337 5
22B R 215 005 225 5
23 R 179 003 179 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 977
Table 8 ISO Smoking regime Nicotine mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1704 0029 170 5
2B L 1706 0039 227 5
6B L 1624 0048 295 5
7A L 1687 0033 194 5
9A L 1612 0200 1240 5
10 L 1748 0070 401 5
11 L 1691 0028 166 5
12C L 1669 0034 206 5
16 L 1731 0028 159 5
17 L 1674 0046 276 5
18 L 1697 0014 082 5
19 L 1697 0014 082 5
20 L 1734 0021 124 5
21 L 1812 0048 266 5
24 L 1694 0037 217 5
25 L 1743 0154 883 5
1A R 1669 0023 141 5
2A R 1638 0037 224 5
3 R 1652 0018 110 5
4A R 1630 0042 255 5
4B R 1653 0035 214 5
5A R 1612 0023 142 5
5B R 1602 0023 141 5
6A R 1661 0037 225 5
7B R 1564 0022 140 5
8 R 1535 0031 204 5
9B R 1659 0047 285 5
12A R 1719 0024 142 5
12B R 1718 0037 216 5
13A R 1497 0024 163 5
13B R 1546 0013 086 5
14 R 1590 0035 217 5
15 R 1651 0030 181 5
22A R 1612 0011 068 5
22B R 1630 0012 075 5
23 R 1639 0026 159 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1077
Table 9 ISO smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1462 016 111 5
2B L 1449 053 366 5
6B L 1294 044 344 5
7A L 1460 031 214 5
9A L 1395 011 080 5
10 L 1455 039 269 5
11 L 1518 036 236 5
12C L 1439 049 338 5
16 L 1427 013 092 5
17 L 1304 054 413 5
18 L 1456 020 135 5
19 L 1456 020 135 5
20 L 1395 036 255 5
21 L 1531 057 371 5
24 L 1466 023 154 5
25 L 1306 066 509 5
1A R 1367 020 145 5
2A R 1361 023 169 5
3 R 1398 012 083 5
4A R 1363 024 176 5
4B R 1391 028 201 5
5A R 1347 014 107 5
5B R 1372 023 166 5
6A R 1346 019 142 5
7B R 1305 020 153 5
8 R 1378 026 192 5
9B R 1342 015 114 5
12A R 1337 037 278 5
12B R 1375 018 129 5
13A R 1319 015 112 5
13B R 1341 009 069 5
14 R 1359 028 204 5
15 R 1366 029 214 5
22A R 1371 019 136 5
22B R 1353 024 175 5
23 R 1308 037 283 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1177
Table 10 ISO Smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1335 020 150 5
2B L 1297 037 288 5
6B L 1260 099 790 5
7A L 1374 034 249 5
9A L 1233 019 153 5
10 L 1219 054 445 5
11 L 1267 044 350 5
12C L 1325 033 248 5
16 L 1307 024 185 5
17 L 1196 029 242 5
18 L 1335 010 072 5
19 L 1335 010 072 5
20 L 1324 033 248 5
21 L 1363 032 238 5
24 L 1263 040 315 5
25 L 1194 069 574 5
1A R 1368 010 076 5
2A R 1308 018 135 5
3 R 1345 023 172 5
4A R 1340 011 079 5
4B R 1394 041 294 5
5A R 1292 028 216 5
5B R 1360 034 251 5
6A R 1372 023 166 5
7B R 1291 013 098 5
8 R 1369 025 183 5
9B R 1276 023 182 5
12A R 1317 034 256 5
12B R 1375 024 175 5
13A R 1334 021 155 5
13B R 1338 030 227 5
14 R 1366 023 167 5
15 R 1377 019 139 5
22A R 1344 016 118 5
22B R 1341 016 116 5
23 R 1334 029 217 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1277
Table 11 ISO Smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 796 005 059 5
2B L 806 012 144 5
6B L 814 018 219 5
7A L 789 009 112 5
9A L 781 024 306 5
10 L 802 020 245 5
11 L 784 018 225 5
12C L 794 021 263 5
16 L 850 014 168 5
17 L 774 016 203 5
18 L 787 015 187 5
19 L 787 015 187 5
20 L 769 014 188 5
21 L 808 008 097 5
24 L 792 010 128 5
25 L 751 030 400 5
1A R 767 005 068 5
2A R 727 008 109 5
3 R 779 008 099 5
4A R 748 011 146 5
4B R 758 013 172 5
5A R 782 011 144 5
5B R 766 017 216 5
6A R 773 009 117 5
7B R 716 011 160 5
8 R 754 010 127 5
9B R 755 008 107 5
12A R 755 006 078 5
12B R 771 008 102 5
13A R 740 017 225 5
13B R 769 007 091 5
14 R 761 011 140 5
15 R 750 018 246 5
22A R 757 008 110 5
22B R 759 007 088 5
23 R 732 009 117 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1377
Table 12 Intense smoking regime TPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 4551 091 200 5
2B L 4391 078 178 5
6B L 3936 067 170 5
9A L 4471 060 134 5
10 L 4667 073 157 5
11 L 5068 136 269 5
12C L 4644 031 066 5
17 L 4346 106 243 5
19 L 4566 087 190 5
20 L 4616 122 265 5
21 L 5008 077 153 5
24 L 4782 094 196 5
25 L 4434 081 182 5
1A R 4168 016 039 5
2A R 4014 024 061 5
3 R 4247 035 083 5
4A R 4097 039 095 5
4B R 4181 064 153 5
5B R 3997 040 101 5
6A R 4076 074 181 5
8 R 4044 043 107 5
9B R 4097 033 080 5
12A R 4125 046 112 5
12B R 4257 039 092 5
15 R 3957 052 131 5
22A R 4046 028 069 5
22B R 4015 045 112 5
23 R 3830 073 192 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1477
Table 13 Intense smoking regime Water mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1237 038 305 5
2B L 999 037 375 5
6B L 906 034 381 5
9A L 1147 043 373 5
10 L 1152 052 453 5
11 L 1488 053 356 5
12C L 1061 019 179 5
17 L 1027 028 274 5
19 L 1095 038 348 5
20 L 1216 083 681 5
21 L 1285 026 206 5
24 L 1235 060 484 5
25 L 1004 031 307 5
1A R 1024 014 138 5
2A R 797 016 197 5
3 R 974 031 317 5
4A R 911 034 368 5
4B R 931 027 287 5
5B R 815 041 507 5
6A R 923 038 411 5
8 R 929 033 354 5
9B R 927 028 301 5
12A R 1004 051 508 5
12B R 935 017 181 5
15 R 823 029 349 5
22A R 953 005 052 5
22B R 926 038 410 5
23 R 1598 065 404 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1577
Table 14 Intense smoking regime Nicotine mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 3484 0055 158 5
2B L 3434 0048 141 5
6B L 3342 0051 153 5
9A L 3494 0089 255 5
10 L 3578 0226 633 5
11 L 3620 0082 225 5
12C L 3402 0024 070 5
17 L 3622 0075 208 5
19 L 3520 0012 035 5
20 L 3552 0230 647 5
21 L 3712 0030 082 5
24 L 3524 0061 174 5
25 L 2986 0052 173 5
1A R 3385 0020 060 5
2A R 3317 0030 090 5
3 R 3479 0023 067 5
4A R 3369 0037 109 5
4B R 3340 0053 160 5
5B R 1677 0025 148 5
6A R 3390 0066 195 5
8 R 2967 0044 149 5
9B R 3410 0048 142 5
12A R 3452 0030 085 5
12B R 3520 0068 192 5
15 R 3333 0099 296 5
22A R 3222 0051 159 5
22B R 3210 0049 151 5
23 R 6610 0108 163 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1677
Table 15 Intense smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2965 054 183 5
2B L 3048 092 301 5
6B L 2696 035 131 5
9A L 2975 038 129 5
10 L 3157 047 148 5
11 L 3218 082 255 5
12C L 3243 015 047 5
17 L 3157 079 250 5
19 L 3119 084 268 5
20 L 3045 056 185 5
21 L 3351 066 198 5
24 L 3195 050 158 5
25 L 3132 054 174 5
1A R 2806 018 065 5
2A R 2885 012 043 5
3 R 2925 040 135 5
4A R 2849 021 074 5
4B R 2917 035 119 5
5B R 3013 023 077 5
6A R 2811 036 129 5
8 R 2819 021 074 5
9B R 2832 032 115 5
12A R 2776 048 171 5
12B R 2970 026 086 5
15 R 2800 035 124 5
22A R 2770 025 091 5
22B R 2768 049 178 5
23 R 1570 060 384 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1777
Table 16 Intense smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2478 034 137 5
2B L 2472 027 111 5
6B L 2367 039 165 5
9A L 2423 065 270 5
10 L 2373 018 077 5
11 L 2568 029 114 5
12C L 2497 028 113 5
17 L 2321 032 139 5
19 L 2488 022 086 5
20 L 2489 056 227 5
21 L 2523 045 177 5
24 L 2470 052 211 5
25 L 2399 089 369 5
1A R 2505 033 131 5
2A R 2485 037 149 5
3 R 2605 031 119 5
4A R 2513 031 125 5
4B R 2542 047 185 5
5B R 2480 022 088 5
6A R 2570 024 092 5
8 R 2532 047 185 5
9B R 2457 044 181 5
12A R 2506 023 093 5
12B R 2523 018 069 5
15 R 2547 039 154 5
22A R 2470 034 138 5
22B R 2466 032 130 5
23 R 2508 030 119 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1877
Table 17 Intense smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 1138 022 191 5
2B L 1154 019 162 5
6B L 1170 008 068 5
9A L 1095 013 114 5
10 L 1138 023 199 5
11 L 1127 016 138 5
12C L 1115 022 199 5
17 L 1110 009 079 5
19 L 1059 011 101 5
20 L 1087 019 176 5
21 L 1121 019 169 5
24 L 1106 027 248 5
25 L 1102 012 105 5
1A R 1111 018 159 5
2A R 1059 014 130 5
3 R 1152 013 110 5
4A R 1078 008 070 5
4B R 1105 016 143 5
5B R 1134 030 267 5
6A R 1136 004 034 5
8 R 1075 015 142 5
9B R 1077 006 054 5
12A R 1102 020 186 5
12B R 1097 016 148 5
15 R 1084 010 091 5
22A R 1112 016 147 5
22B R 1106 014 122 5
23 R 1066 009 088 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1977
Statistical Analysis 4
Exclusion of outliers 41
411 Numerical outlier technique Cochran amp Grubbs test
The statistical evaluation of data for this collaborative study followed the methods provided
by ISO 5725-21 For outlier testing the Grubbs and Cochran methods were used
ISO 5725-2 Tests Consistency
Cochranrsquos ndash test Within-laboratory variability Suitable for detecting whether the highest value in a set of laboratory standard deviations is an outlier or not
Grubbsrsquo ndash test Between-laboratory variability Suitable for detecting whether the highest (or lowest) laboratories averages are outliers or not
The protocol ldquoHarmonized statistical procedurerdquo defined by IUPAC (International Union of
Pure and Applied Chemistry) has been applied as well It consists of sequential applications of
the Cochran and Grubbs tests until no further outliers are detected or until a drop of more than
222 (for this study =29) in the original number of laboratories would occur (see flowchart
in Appendix F)
First apply the Cochran outlier test and if an outlying laboratory is identified then a single
value Grubbs test is performed on the individual values of this outlying laboratory (Individual
Grubbs) If no individual value is identified as outlier the outlying laboratory is removed
When an individual value is identified as an outlier only this value is removed
Afterwards single-value Grubbs test is applied and outlying laboratories are removed If no
laboratory is identified as outlier the pair-value test is applied (two values at the same end)
Remove any laboratory(ies) flagged by these tests but stop removal if more than 222 (2 of
9 laboratories) would be removed
The test was performed with both linear and rotary smoking machines together but also with
rotary respectively linear smoking machines separately The results provided in the report for
all smoking machines respectively with linear or rotary only smoking machines are obtained
after exclusion of the outliers for those respective categories
Note
The paired value Grubbsrsquo test is an extension of the single value Grubbs test for pairs of
outliers The use is advised in ISO 5725 to detect pairs of outlier undetectable sequentially by
using single value Grubbs test
The outlying laboratories are provided in the Tables 18 to 23
Repeatability and reproducibility estimation 42
Repeatability and reproducibility limits are calculated for both smoking regimes each
parameter and for both smoking machine types The results are summarized in tables 18 to 23
with all machines grouped respectively with linear or rotary machines only both with ISO
and intense smoking regimes Outlying laboratories are provided in the same tables The
corresponding graphs named ldquoindividual valuesrdquo are given in Part 5 of this report
1 ISO 5725-21994 Accuracy (trueness and precision) of measurement methods and results ndash Part 2 Basic
method for the determination of repeatability and reproducibility of a standard measurement method
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 2077
Table 18 r amp R estimations for CM8 under ISO smoking regime (all machines)
p n Global Mean Sr CVr[] r SR CVR [] R C GG2 Stragglers Parameter
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 677
Table 5 WEIGHT mean and standard deviation per laboratory code
Lab Code Machine Type Mean SD CV [] Sample size
1A R 96055 2731 0284 5
1B L 96519 3313 0343 5
2A R 94828 2622 0277 5
2B L 95000 5958 0627 5
3 R 90323 3183 0352 5
4A R 96060 2510 0261 5
4B R 96200 6481 0674 5
5A R 96494 1638 0170 5
5B R 95620 2978 0311 5
6A R 96612 4814 0498 5
6B L 96604 2688 0278 5
7A L 95598 3295 0345 5
7B R 95490 3365 0352 5
8 R 96653 2676 0277 5
9A L 95220 2564 0269 5
9B R 95900 2264 0236 5
10 L 96640 2595 0269 5
11 L 95968 8571 0893 5
12A R 95840 4930 0514 5
12B R 96226 2852 0296 5
12C L 95960 2702 0282 5
13A R 95806 2698 0282 5
13B R 95901 5717 0596 5
14 R 96102 3340 0348 5
15 R 95871 4505 0470 5
16 L 96286 4512 0469 5
17 L 95626 3166 0331 5
18 L 95285 3720 0390 5
19 L 95285 3720 0390 5
20 L 95767 5690 0594 5
22A R 96300 1414 0147 5
22B R 96240 1517 0158 5
23 R 94926 3700 0390 5
24 L 95591 5108 0534 5
25 L 96223 5979 0621 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 777
Table 6 ISO smoking regime TPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1793 024 132 5
2B L 1765 063 357 5
6B L 1574 061 387 5
7A L 1804 039 214 5
9A L 1698 033 197 5
10 L 1807 048 265 5
11 L 1828 045 248 5
12C L 1728 055 321 5
16 L 1742 010 058 5
17 L 1616 030 187 5
18 L 1772 036 205 5
19 L 1772 036 205 5
20 L 1783 040 224 5
21 L 1832 050 272 5
24 L 1791 033 185 5
25 L 1607 079 494 5
1A R 1749 024 135 5
2A R 1698 028 166 5
3 R 1760 019 107 5
4A R 1723 028 165 5
4B R 1769 038 212 5
5A R 1703 022 127 5
5B R 1724 031 178 5
6A R 1740 031 176 5
7B R 1646 017 103 5
8 R 1737 022 125 5
9B R 1711 025 147 5
12A R 1758 040 227 5
12B R 1790 014 078 5
13A R 1674 017 104 5
13B R 1700 020 115 5
14 R 1746 044 254 5
15 R 1719 041 238 5
22A R 1752 020 115 5
22B R 1731 022 129 5
23 R 1651 037 226 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 877
Table 7 ISO Smoking regime WATER mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 161 007 428 5
2B L 145 008 518 5
6B L 118 014 1213 5
7A L 175 006 364 5
9A L 142 011 802 5
10 L 177 010 581 5
11 L 142 009 632 5
12C L 122 008 645 5
16 L 142 012 872 5
17 L 145 026 1823 5
18 L 147 019 1299 5
19 L 147 019 1299 5
20 L 214 013 611 5
21 L 120 024 2024 5
24 L 156 009 551 5
25 L 127 016 1261 5
1A R 215 007 316 5
2A R 174 008 444 5
3 R 196 010 493 5
4A R 197 008 406 5
4B R 213 013 629 5
5A R 197 009 471 5
5B R 192 008 419 5
6A R 227 010 445 5
7B R 184 007 396 5
8 R 206 013 637 5
9B R 203 012 579 5
12A R 250 012 464 5
12B R 244 010 430 5
13A R 205 007 362 5
13B R 204 012 576 5
14 R 228 017 739 5
15 R 188 016 834 5
22A R 219 007 337 5
22B R 215 005 225 5
23 R 179 003 179 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 977
Table 8 ISO Smoking regime Nicotine mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1704 0029 170 5
2B L 1706 0039 227 5
6B L 1624 0048 295 5
7A L 1687 0033 194 5
9A L 1612 0200 1240 5
10 L 1748 0070 401 5
11 L 1691 0028 166 5
12C L 1669 0034 206 5
16 L 1731 0028 159 5
17 L 1674 0046 276 5
18 L 1697 0014 082 5
19 L 1697 0014 082 5
20 L 1734 0021 124 5
21 L 1812 0048 266 5
24 L 1694 0037 217 5
25 L 1743 0154 883 5
1A R 1669 0023 141 5
2A R 1638 0037 224 5
3 R 1652 0018 110 5
4A R 1630 0042 255 5
4B R 1653 0035 214 5
5A R 1612 0023 142 5
5B R 1602 0023 141 5
6A R 1661 0037 225 5
7B R 1564 0022 140 5
8 R 1535 0031 204 5
9B R 1659 0047 285 5
12A R 1719 0024 142 5
12B R 1718 0037 216 5
13A R 1497 0024 163 5
13B R 1546 0013 086 5
14 R 1590 0035 217 5
15 R 1651 0030 181 5
22A R 1612 0011 068 5
22B R 1630 0012 075 5
23 R 1639 0026 159 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1077
Table 9 ISO smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1462 016 111 5
2B L 1449 053 366 5
6B L 1294 044 344 5
7A L 1460 031 214 5
9A L 1395 011 080 5
10 L 1455 039 269 5
11 L 1518 036 236 5
12C L 1439 049 338 5
16 L 1427 013 092 5
17 L 1304 054 413 5
18 L 1456 020 135 5
19 L 1456 020 135 5
20 L 1395 036 255 5
21 L 1531 057 371 5
24 L 1466 023 154 5
25 L 1306 066 509 5
1A R 1367 020 145 5
2A R 1361 023 169 5
3 R 1398 012 083 5
4A R 1363 024 176 5
4B R 1391 028 201 5
5A R 1347 014 107 5
5B R 1372 023 166 5
6A R 1346 019 142 5
7B R 1305 020 153 5
8 R 1378 026 192 5
9B R 1342 015 114 5
12A R 1337 037 278 5
12B R 1375 018 129 5
13A R 1319 015 112 5
13B R 1341 009 069 5
14 R 1359 028 204 5
15 R 1366 029 214 5
22A R 1371 019 136 5
22B R 1353 024 175 5
23 R 1308 037 283 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1177
Table 10 ISO Smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1335 020 150 5
2B L 1297 037 288 5
6B L 1260 099 790 5
7A L 1374 034 249 5
9A L 1233 019 153 5
10 L 1219 054 445 5
11 L 1267 044 350 5
12C L 1325 033 248 5
16 L 1307 024 185 5
17 L 1196 029 242 5
18 L 1335 010 072 5
19 L 1335 010 072 5
20 L 1324 033 248 5
21 L 1363 032 238 5
24 L 1263 040 315 5
25 L 1194 069 574 5
1A R 1368 010 076 5
2A R 1308 018 135 5
3 R 1345 023 172 5
4A R 1340 011 079 5
4B R 1394 041 294 5
5A R 1292 028 216 5
5B R 1360 034 251 5
6A R 1372 023 166 5
7B R 1291 013 098 5
8 R 1369 025 183 5
9B R 1276 023 182 5
12A R 1317 034 256 5
12B R 1375 024 175 5
13A R 1334 021 155 5
13B R 1338 030 227 5
14 R 1366 023 167 5
15 R 1377 019 139 5
22A R 1344 016 118 5
22B R 1341 016 116 5
23 R 1334 029 217 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1277
Table 11 ISO Smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 796 005 059 5
2B L 806 012 144 5
6B L 814 018 219 5
7A L 789 009 112 5
9A L 781 024 306 5
10 L 802 020 245 5
11 L 784 018 225 5
12C L 794 021 263 5
16 L 850 014 168 5
17 L 774 016 203 5
18 L 787 015 187 5
19 L 787 015 187 5
20 L 769 014 188 5
21 L 808 008 097 5
24 L 792 010 128 5
25 L 751 030 400 5
1A R 767 005 068 5
2A R 727 008 109 5
3 R 779 008 099 5
4A R 748 011 146 5
4B R 758 013 172 5
5A R 782 011 144 5
5B R 766 017 216 5
6A R 773 009 117 5
7B R 716 011 160 5
8 R 754 010 127 5
9B R 755 008 107 5
12A R 755 006 078 5
12B R 771 008 102 5
13A R 740 017 225 5
13B R 769 007 091 5
14 R 761 011 140 5
15 R 750 018 246 5
22A R 757 008 110 5
22B R 759 007 088 5
23 R 732 009 117 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1377
Table 12 Intense smoking regime TPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 4551 091 200 5
2B L 4391 078 178 5
6B L 3936 067 170 5
9A L 4471 060 134 5
10 L 4667 073 157 5
11 L 5068 136 269 5
12C L 4644 031 066 5
17 L 4346 106 243 5
19 L 4566 087 190 5
20 L 4616 122 265 5
21 L 5008 077 153 5
24 L 4782 094 196 5
25 L 4434 081 182 5
1A R 4168 016 039 5
2A R 4014 024 061 5
3 R 4247 035 083 5
4A R 4097 039 095 5
4B R 4181 064 153 5
5B R 3997 040 101 5
6A R 4076 074 181 5
8 R 4044 043 107 5
9B R 4097 033 080 5
12A R 4125 046 112 5
12B R 4257 039 092 5
15 R 3957 052 131 5
22A R 4046 028 069 5
22B R 4015 045 112 5
23 R 3830 073 192 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1477
Table 13 Intense smoking regime Water mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1237 038 305 5
2B L 999 037 375 5
6B L 906 034 381 5
9A L 1147 043 373 5
10 L 1152 052 453 5
11 L 1488 053 356 5
12C L 1061 019 179 5
17 L 1027 028 274 5
19 L 1095 038 348 5
20 L 1216 083 681 5
21 L 1285 026 206 5
24 L 1235 060 484 5
25 L 1004 031 307 5
1A R 1024 014 138 5
2A R 797 016 197 5
3 R 974 031 317 5
4A R 911 034 368 5
4B R 931 027 287 5
5B R 815 041 507 5
6A R 923 038 411 5
8 R 929 033 354 5
9B R 927 028 301 5
12A R 1004 051 508 5
12B R 935 017 181 5
15 R 823 029 349 5
22A R 953 005 052 5
22B R 926 038 410 5
23 R 1598 065 404 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1577
Table 14 Intense smoking regime Nicotine mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 3484 0055 158 5
2B L 3434 0048 141 5
6B L 3342 0051 153 5
9A L 3494 0089 255 5
10 L 3578 0226 633 5
11 L 3620 0082 225 5
12C L 3402 0024 070 5
17 L 3622 0075 208 5
19 L 3520 0012 035 5
20 L 3552 0230 647 5
21 L 3712 0030 082 5
24 L 3524 0061 174 5
25 L 2986 0052 173 5
1A R 3385 0020 060 5
2A R 3317 0030 090 5
3 R 3479 0023 067 5
4A R 3369 0037 109 5
4B R 3340 0053 160 5
5B R 1677 0025 148 5
6A R 3390 0066 195 5
8 R 2967 0044 149 5
9B R 3410 0048 142 5
12A R 3452 0030 085 5
12B R 3520 0068 192 5
15 R 3333 0099 296 5
22A R 3222 0051 159 5
22B R 3210 0049 151 5
23 R 6610 0108 163 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1677
Table 15 Intense smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2965 054 183 5
2B L 3048 092 301 5
6B L 2696 035 131 5
9A L 2975 038 129 5
10 L 3157 047 148 5
11 L 3218 082 255 5
12C L 3243 015 047 5
17 L 3157 079 250 5
19 L 3119 084 268 5
20 L 3045 056 185 5
21 L 3351 066 198 5
24 L 3195 050 158 5
25 L 3132 054 174 5
1A R 2806 018 065 5
2A R 2885 012 043 5
3 R 2925 040 135 5
4A R 2849 021 074 5
4B R 2917 035 119 5
5B R 3013 023 077 5
6A R 2811 036 129 5
8 R 2819 021 074 5
9B R 2832 032 115 5
12A R 2776 048 171 5
12B R 2970 026 086 5
15 R 2800 035 124 5
22A R 2770 025 091 5
22B R 2768 049 178 5
23 R 1570 060 384 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1777
Table 16 Intense smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2478 034 137 5
2B L 2472 027 111 5
6B L 2367 039 165 5
9A L 2423 065 270 5
10 L 2373 018 077 5
11 L 2568 029 114 5
12C L 2497 028 113 5
17 L 2321 032 139 5
19 L 2488 022 086 5
20 L 2489 056 227 5
21 L 2523 045 177 5
24 L 2470 052 211 5
25 L 2399 089 369 5
1A R 2505 033 131 5
2A R 2485 037 149 5
3 R 2605 031 119 5
4A R 2513 031 125 5
4B R 2542 047 185 5
5B R 2480 022 088 5
6A R 2570 024 092 5
8 R 2532 047 185 5
9B R 2457 044 181 5
12A R 2506 023 093 5
12B R 2523 018 069 5
15 R 2547 039 154 5
22A R 2470 034 138 5
22B R 2466 032 130 5
23 R 2508 030 119 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1877
Table 17 Intense smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 1138 022 191 5
2B L 1154 019 162 5
6B L 1170 008 068 5
9A L 1095 013 114 5
10 L 1138 023 199 5
11 L 1127 016 138 5
12C L 1115 022 199 5
17 L 1110 009 079 5
19 L 1059 011 101 5
20 L 1087 019 176 5
21 L 1121 019 169 5
24 L 1106 027 248 5
25 L 1102 012 105 5
1A R 1111 018 159 5
2A R 1059 014 130 5
3 R 1152 013 110 5
4A R 1078 008 070 5
4B R 1105 016 143 5
5B R 1134 030 267 5
6A R 1136 004 034 5
8 R 1075 015 142 5
9B R 1077 006 054 5
12A R 1102 020 186 5
12B R 1097 016 148 5
15 R 1084 010 091 5
22A R 1112 016 147 5
22B R 1106 014 122 5
23 R 1066 009 088 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1977
Statistical Analysis 4
Exclusion of outliers 41
411 Numerical outlier technique Cochran amp Grubbs test
The statistical evaluation of data for this collaborative study followed the methods provided
by ISO 5725-21 For outlier testing the Grubbs and Cochran methods were used
ISO 5725-2 Tests Consistency
Cochranrsquos ndash test Within-laboratory variability Suitable for detecting whether the highest value in a set of laboratory standard deviations is an outlier or not
Grubbsrsquo ndash test Between-laboratory variability Suitable for detecting whether the highest (or lowest) laboratories averages are outliers or not
The protocol ldquoHarmonized statistical procedurerdquo defined by IUPAC (International Union of
Pure and Applied Chemistry) has been applied as well It consists of sequential applications of
the Cochran and Grubbs tests until no further outliers are detected or until a drop of more than
222 (for this study =29) in the original number of laboratories would occur (see flowchart
in Appendix F)
First apply the Cochran outlier test and if an outlying laboratory is identified then a single
value Grubbs test is performed on the individual values of this outlying laboratory (Individual
Grubbs) If no individual value is identified as outlier the outlying laboratory is removed
When an individual value is identified as an outlier only this value is removed
Afterwards single-value Grubbs test is applied and outlying laboratories are removed If no
laboratory is identified as outlier the pair-value test is applied (two values at the same end)
Remove any laboratory(ies) flagged by these tests but stop removal if more than 222 (2 of
9 laboratories) would be removed
The test was performed with both linear and rotary smoking machines together but also with
rotary respectively linear smoking machines separately The results provided in the report for
all smoking machines respectively with linear or rotary only smoking machines are obtained
after exclusion of the outliers for those respective categories
Note
The paired value Grubbsrsquo test is an extension of the single value Grubbs test for pairs of
outliers The use is advised in ISO 5725 to detect pairs of outlier undetectable sequentially by
using single value Grubbs test
The outlying laboratories are provided in the Tables 18 to 23
Repeatability and reproducibility estimation 42
Repeatability and reproducibility limits are calculated for both smoking regimes each
parameter and for both smoking machine types The results are summarized in tables 18 to 23
with all machines grouped respectively with linear or rotary machines only both with ISO
and intense smoking regimes Outlying laboratories are provided in the same tables The
corresponding graphs named ldquoindividual valuesrdquo are given in Part 5 of this report
1 ISO 5725-21994 Accuracy (trueness and precision) of measurement methods and results ndash Part 2 Basic
method for the determination of repeatability and reproducibility of a standard measurement method
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 2077
Table 18 r amp R estimations for CM8 under ISO smoking regime (all machines)
p n Global Mean Sr CVr[] r SR CVR [] R C GG2 Stragglers Parameter
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 777
Table 6 ISO smoking regime TPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1793 024 132 5
2B L 1765 063 357 5
6B L 1574 061 387 5
7A L 1804 039 214 5
9A L 1698 033 197 5
10 L 1807 048 265 5
11 L 1828 045 248 5
12C L 1728 055 321 5
16 L 1742 010 058 5
17 L 1616 030 187 5
18 L 1772 036 205 5
19 L 1772 036 205 5
20 L 1783 040 224 5
21 L 1832 050 272 5
24 L 1791 033 185 5
25 L 1607 079 494 5
1A R 1749 024 135 5
2A R 1698 028 166 5
3 R 1760 019 107 5
4A R 1723 028 165 5
4B R 1769 038 212 5
5A R 1703 022 127 5
5B R 1724 031 178 5
6A R 1740 031 176 5
7B R 1646 017 103 5
8 R 1737 022 125 5
9B R 1711 025 147 5
12A R 1758 040 227 5
12B R 1790 014 078 5
13A R 1674 017 104 5
13B R 1700 020 115 5
14 R 1746 044 254 5
15 R 1719 041 238 5
22A R 1752 020 115 5
22B R 1731 022 129 5
23 R 1651 037 226 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 877
Table 7 ISO Smoking regime WATER mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 161 007 428 5
2B L 145 008 518 5
6B L 118 014 1213 5
7A L 175 006 364 5
9A L 142 011 802 5
10 L 177 010 581 5
11 L 142 009 632 5
12C L 122 008 645 5
16 L 142 012 872 5
17 L 145 026 1823 5
18 L 147 019 1299 5
19 L 147 019 1299 5
20 L 214 013 611 5
21 L 120 024 2024 5
24 L 156 009 551 5
25 L 127 016 1261 5
1A R 215 007 316 5
2A R 174 008 444 5
3 R 196 010 493 5
4A R 197 008 406 5
4B R 213 013 629 5
5A R 197 009 471 5
5B R 192 008 419 5
6A R 227 010 445 5
7B R 184 007 396 5
8 R 206 013 637 5
9B R 203 012 579 5
12A R 250 012 464 5
12B R 244 010 430 5
13A R 205 007 362 5
13B R 204 012 576 5
14 R 228 017 739 5
15 R 188 016 834 5
22A R 219 007 337 5
22B R 215 005 225 5
23 R 179 003 179 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 977
Table 8 ISO Smoking regime Nicotine mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1704 0029 170 5
2B L 1706 0039 227 5
6B L 1624 0048 295 5
7A L 1687 0033 194 5
9A L 1612 0200 1240 5
10 L 1748 0070 401 5
11 L 1691 0028 166 5
12C L 1669 0034 206 5
16 L 1731 0028 159 5
17 L 1674 0046 276 5
18 L 1697 0014 082 5
19 L 1697 0014 082 5
20 L 1734 0021 124 5
21 L 1812 0048 266 5
24 L 1694 0037 217 5
25 L 1743 0154 883 5
1A R 1669 0023 141 5
2A R 1638 0037 224 5
3 R 1652 0018 110 5
4A R 1630 0042 255 5
4B R 1653 0035 214 5
5A R 1612 0023 142 5
5B R 1602 0023 141 5
6A R 1661 0037 225 5
7B R 1564 0022 140 5
8 R 1535 0031 204 5
9B R 1659 0047 285 5
12A R 1719 0024 142 5
12B R 1718 0037 216 5
13A R 1497 0024 163 5
13B R 1546 0013 086 5
14 R 1590 0035 217 5
15 R 1651 0030 181 5
22A R 1612 0011 068 5
22B R 1630 0012 075 5
23 R 1639 0026 159 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1077
Table 9 ISO smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1462 016 111 5
2B L 1449 053 366 5
6B L 1294 044 344 5
7A L 1460 031 214 5
9A L 1395 011 080 5
10 L 1455 039 269 5
11 L 1518 036 236 5
12C L 1439 049 338 5
16 L 1427 013 092 5
17 L 1304 054 413 5
18 L 1456 020 135 5
19 L 1456 020 135 5
20 L 1395 036 255 5
21 L 1531 057 371 5
24 L 1466 023 154 5
25 L 1306 066 509 5
1A R 1367 020 145 5
2A R 1361 023 169 5
3 R 1398 012 083 5
4A R 1363 024 176 5
4B R 1391 028 201 5
5A R 1347 014 107 5
5B R 1372 023 166 5
6A R 1346 019 142 5
7B R 1305 020 153 5
8 R 1378 026 192 5
9B R 1342 015 114 5
12A R 1337 037 278 5
12B R 1375 018 129 5
13A R 1319 015 112 5
13B R 1341 009 069 5
14 R 1359 028 204 5
15 R 1366 029 214 5
22A R 1371 019 136 5
22B R 1353 024 175 5
23 R 1308 037 283 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1177
Table 10 ISO Smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1335 020 150 5
2B L 1297 037 288 5
6B L 1260 099 790 5
7A L 1374 034 249 5
9A L 1233 019 153 5
10 L 1219 054 445 5
11 L 1267 044 350 5
12C L 1325 033 248 5
16 L 1307 024 185 5
17 L 1196 029 242 5
18 L 1335 010 072 5
19 L 1335 010 072 5
20 L 1324 033 248 5
21 L 1363 032 238 5
24 L 1263 040 315 5
25 L 1194 069 574 5
1A R 1368 010 076 5
2A R 1308 018 135 5
3 R 1345 023 172 5
4A R 1340 011 079 5
4B R 1394 041 294 5
5A R 1292 028 216 5
5B R 1360 034 251 5
6A R 1372 023 166 5
7B R 1291 013 098 5
8 R 1369 025 183 5
9B R 1276 023 182 5
12A R 1317 034 256 5
12B R 1375 024 175 5
13A R 1334 021 155 5
13B R 1338 030 227 5
14 R 1366 023 167 5
15 R 1377 019 139 5
22A R 1344 016 118 5
22B R 1341 016 116 5
23 R 1334 029 217 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1277
Table 11 ISO Smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 796 005 059 5
2B L 806 012 144 5
6B L 814 018 219 5
7A L 789 009 112 5
9A L 781 024 306 5
10 L 802 020 245 5
11 L 784 018 225 5
12C L 794 021 263 5
16 L 850 014 168 5
17 L 774 016 203 5
18 L 787 015 187 5
19 L 787 015 187 5
20 L 769 014 188 5
21 L 808 008 097 5
24 L 792 010 128 5
25 L 751 030 400 5
1A R 767 005 068 5
2A R 727 008 109 5
3 R 779 008 099 5
4A R 748 011 146 5
4B R 758 013 172 5
5A R 782 011 144 5
5B R 766 017 216 5
6A R 773 009 117 5
7B R 716 011 160 5
8 R 754 010 127 5
9B R 755 008 107 5
12A R 755 006 078 5
12B R 771 008 102 5
13A R 740 017 225 5
13B R 769 007 091 5
14 R 761 011 140 5
15 R 750 018 246 5
22A R 757 008 110 5
22B R 759 007 088 5
23 R 732 009 117 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1377
Table 12 Intense smoking regime TPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 4551 091 200 5
2B L 4391 078 178 5
6B L 3936 067 170 5
9A L 4471 060 134 5
10 L 4667 073 157 5
11 L 5068 136 269 5
12C L 4644 031 066 5
17 L 4346 106 243 5
19 L 4566 087 190 5
20 L 4616 122 265 5
21 L 5008 077 153 5
24 L 4782 094 196 5
25 L 4434 081 182 5
1A R 4168 016 039 5
2A R 4014 024 061 5
3 R 4247 035 083 5
4A R 4097 039 095 5
4B R 4181 064 153 5
5B R 3997 040 101 5
6A R 4076 074 181 5
8 R 4044 043 107 5
9B R 4097 033 080 5
12A R 4125 046 112 5
12B R 4257 039 092 5
15 R 3957 052 131 5
22A R 4046 028 069 5
22B R 4015 045 112 5
23 R 3830 073 192 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1477
Table 13 Intense smoking regime Water mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1237 038 305 5
2B L 999 037 375 5
6B L 906 034 381 5
9A L 1147 043 373 5
10 L 1152 052 453 5
11 L 1488 053 356 5
12C L 1061 019 179 5
17 L 1027 028 274 5
19 L 1095 038 348 5
20 L 1216 083 681 5
21 L 1285 026 206 5
24 L 1235 060 484 5
25 L 1004 031 307 5
1A R 1024 014 138 5
2A R 797 016 197 5
3 R 974 031 317 5
4A R 911 034 368 5
4B R 931 027 287 5
5B R 815 041 507 5
6A R 923 038 411 5
8 R 929 033 354 5
9B R 927 028 301 5
12A R 1004 051 508 5
12B R 935 017 181 5
15 R 823 029 349 5
22A R 953 005 052 5
22B R 926 038 410 5
23 R 1598 065 404 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1577
Table 14 Intense smoking regime Nicotine mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 3484 0055 158 5
2B L 3434 0048 141 5
6B L 3342 0051 153 5
9A L 3494 0089 255 5
10 L 3578 0226 633 5
11 L 3620 0082 225 5
12C L 3402 0024 070 5
17 L 3622 0075 208 5
19 L 3520 0012 035 5
20 L 3552 0230 647 5
21 L 3712 0030 082 5
24 L 3524 0061 174 5
25 L 2986 0052 173 5
1A R 3385 0020 060 5
2A R 3317 0030 090 5
3 R 3479 0023 067 5
4A R 3369 0037 109 5
4B R 3340 0053 160 5
5B R 1677 0025 148 5
6A R 3390 0066 195 5
8 R 2967 0044 149 5
9B R 3410 0048 142 5
12A R 3452 0030 085 5
12B R 3520 0068 192 5
15 R 3333 0099 296 5
22A R 3222 0051 159 5
22B R 3210 0049 151 5
23 R 6610 0108 163 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1677
Table 15 Intense smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2965 054 183 5
2B L 3048 092 301 5
6B L 2696 035 131 5
9A L 2975 038 129 5
10 L 3157 047 148 5
11 L 3218 082 255 5
12C L 3243 015 047 5
17 L 3157 079 250 5
19 L 3119 084 268 5
20 L 3045 056 185 5
21 L 3351 066 198 5
24 L 3195 050 158 5
25 L 3132 054 174 5
1A R 2806 018 065 5
2A R 2885 012 043 5
3 R 2925 040 135 5
4A R 2849 021 074 5
4B R 2917 035 119 5
5B R 3013 023 077 5
6A R 2811 036 129 5
8 R 2819 021 074 5
9B R 2832 032 115 5
12A R 2776 048 171 5
12B R 2970 026 086 5
15 R 2800 035 124 5
22A R 2770 025 091 5
22B R 2768 049 178 5
23 R 1570 060 384 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1777
Table 16 Intense smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2478 034 137 5
2B L 2472 027 111 5
6B L 2367 039 165 5
9A L 2423 065 270 5
10 L 2373 018 077 5
11 L 2568 029 114 5
12C L 2497 028 113 5
17 L 2321 032 139 5
19 L 2488 022 086 5
20 L 2489 056 227 5
21 L 2523 045 177 5
24 L 2470 052 211 5
25 L 2399 089 369 5
1A R 2505 033 131 5
2A R 2485 037 149 5
3 R 2605 031 119 5
4A R 2513 031 125 5
4B R 2542 047 185 5
5B R 2480 022 088 5
6A R 2570 024 092 5
8 R 2532 047 185 5
9B R 2457 044 181 5
12A R 2506 023 093 5
12B R 2523 018 069 5
15 R 2547 039 154 5
22A R 2470 034 138 5
22B R 2466 032 130 5
23 R 2508 030 119 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1877
Table 17 Intense smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 1138 022 191 5
2B L 1154 019 162 5
6B L 1170 008 068 5
9A L 1095 013 114 5
10 L 1138 023 199 5
11 L 1127 016 138 5
12C L 1115 022 199 5
17 L 1110 009 079 5
19 L 1059 011 101 5
20 L 1087 019 176 5
21 L 1121 019 169 5
24 L 1106 027 248 5
25 L 1102 012 105 5
1A R 1111 018 159 5
2A R 1059 014 130 5
3 R 1152 013 110 5
4A R 1078 008 070 5
4B R 1105 016 143 5
5B R 1134 030 267 5
6A R 1136 004 034 5
8 R 1075 015 142 5
9B R 1077 006 054 5
12A R 1102 020 186 5
12B R 1097 016 148 5
15 R 1084 010 091 5
22A R 1112 016 147 5
22B R 1106 014 122 5
23 R 1066 009 088 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1977
Statistical Analysis 4
Exclusion of outliers 41
411 Numerical outlier technique Cochran amp Grubbs test
The statistical evaluation of data for this collaborative study followed the methods provided
by ISO 5725-21 For outlier testing the Grubbs and Cochran methods were used
ISO 5725-2 Tests Consistency
Cochranrsquos ndash test Within-laboratory variability Suitable for detecting whether the highest value in a set of laboratory standard deviations is an outlier or not
Grubbsrsquo ndash test Between-laboratory variability Suitable for detecting whether the highest (or lowest) laboratories averages are outliers or not
The protocol ldquoHarmonized statistical procedurerdquo defined by IUPAC (International Union of
Pure and Applied Chemistry) has been applied as well It consists of sequential applications of
the Cochran and Grubbs tests until no further outliers are detected or until a drop of more than
222 (for this study =29) in the original number of laboratories would occur (see flowchart
in Appendix F)
First apply the Cochran outlier test and if an outlying laboratory is identified then a single
value Grubbs test is performed on the individual values of this outlying laboratory (Individual
Grubbs) If no individual value is identified as outlier the outlying laboratory is removed
When an individual value is identified as an outlier only this value is removed
Afterwards single-value Grubbs test is applied and outlying laboratories are removed If no
laboratory is identified as outlier the pair-value test is applied (two values at the same end)
Remove any laboratory(ies) flagged by these tests but stop removal if more than 222 (2 of
9 laboratories) would be removed
The test was performed with both linear and rotary smoking machines together but also with
rotary respectively linear smoking machines separately The results provided in the report for
all smoking machines respectively with linear or rotary only smoking machines are obtained
after exclusion of the outliers for those respective categories
Note
The paired value Grubbsrsquo test is an extension of the single value Grubbs test for pairs of
outliers The use is advised in ISO 5725 to detect pairs of outlier undetectable sequentially by
using single value Grubbs test
The outlying laboratories are provided in the Tables 18 to 23
Repeatability and reproducibility estimation 42
Repeatability and reproducibility limits are calculated for both smoking regimes each
parameter and for both smoking machine types The results are summarized in tables 18 to 23
with all machines grouped respectively with linear or rotary machines only both with ISO
and intense smoking regimes Outlying laboratories are provided in the same tables The
corresponding graphs named ldquoindividual valuesrdquo are given in Part 5 of this report
1 ISO 5725-21994 Accuracy (trueness and precision) of measurement methods and results ndash Part 2 Basic
method for the determination of repeatability and reproducibility of a standard measurement method
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 2077
Table 18 r amp R estimations for CM8 under ISO smoking regime (all machines)
p n Global Mean Sr CVr[] r SR CVR [] R C GG2 Stragglers Parameter
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 877
Table 7 ISO Smoking regime WATER mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 161 007 428 5
2B L 145 008 518 5
6B L 118 014 1213 5
7A L 175 006 364 5
9A L 142 011 802 5
10 L 177 010 581 5
11 L 142 009 632 5
12C L 122 008 645 5
16 L 142 012 872 5
17 L 145 026 1823 5
18 L 147 019 1299 5
19 L 147 019 1299 5
20 L 214 013 611 5
21 L 120 024 2024 5
24 L 156 009 551 5
25 L 127 016 1261 5
1A R 215 007 316 5
2A R 174 008 444 5
3 R 196 010 493 5
4A R 197 008 406 5
4B R 213 013 629 5
5A R 197 009 471 5
5B R 192 008 419 5
6A R 227 010 445 5
7B R 184 007 396 5
8 R 206 013 637 5
9B R 203 012 579 5
12A R 250 012 464 5
12B R 244 010 430 5
13A R 205 007 362 5
13B R 204 012 576 5
14 R 228 017 739 5
15 R 188 016 834 5
22A R 219 007 337 5
22B R 215 005 225 5
23 R 179 003 179 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 977
Table 8 ISO Smoking regime Nicotine mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1704 0029 170 5
2B L 1706 0039 227 5
6B L 1624 0048 295 5
7A L 1687 0033 194 5
9A L 1612 0200 1240 5
10 L 1748 0070 401 5
11 L 1691 0028 166 5
12C L 1669 0034 206 5
16 L 1731 0028 159 5
17 L 1674 0046 276 5
18 L 1697 0014 082 5
19 L 1697 0014 082 5
20 L 1734 0021 124 5
21 L 1812 0048 266 5
24 L 1694 0037 217 5
25 L 1743 0154 883 5
1A R 1669 0023 141 5
2A R 1638 0037 224 5
3 R 1652 0018 110 5
4A R 1630 0042 255 5
4B R 1653 0035 214 5
5A R 1612 0023 142 5
5B R 1602 0023 141 5
6A R 1661 0037 225 5
7B R 1564 0022 140 5
8 R 1535 0031 204 5
9B R 1659 0047 285 5
12A R 1719 0024 142 5
12B R 1718 0037 216 5
13A R 1497 0024 163 5
13B R 1546 0013 086 5
14 R 1590 0035 217 5
15 R 1651 0030 181 5
22A R 1612 0011 068 5
22B R 1630 0012 075 5
23 R 1639 0026 159 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1077
Table 9 ISO smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1462 016 111 5
2B L 1449 053 366 5
6B L 1294 044 344 5
7A L 1460 031 214 5
9A L 1395 011 080 5
10 L 1455 039 269 5
11 L 1518 036 236 5
12C L 1439 049 338 5
16 L 1427 013 092 5
17 L 1304 054 413 5
18 L 1456 020 135 5
19 L 1456 020 135 5
20 L 1395 036 255 5
21 L 1531 057 371 5
24 L 1466 023 154 5
25 L 1306 066 509 5
1A R 1367 020 145 5
2A R 1361 023 169 5
3 R 1398 012 083 5
4A R 1363 024 176 5
4B R 1391 028 201 5
5A R 1347 014 107 5
5B R 1372 023 166 5
6A R 1346 019 142 5
7B R 1305 020 153 5
8 R 1378 026 192 5
9B R 1342 015 114 5
12A R 1337 037 278 5
12B R 1375 018 129 5
13A R 1319 015 112 5
13B R 1341 009 069 5
14 R 1359 028 204 5
15 R 1366 029 214 5
22A R 1371 019 136 5
22B R 1353 024 175 5
23 R 1308 037 283 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1177
Table 10 ISO Smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1335 020 150 5
2B L 1297 037 288 5
6B L 1260 099 790 5
7A L 1374 034 249 5
9A L 1233 019 153 5
10 L 1219 054 445 5
11 L 1267 044 350 5
12C L 1325 033 248 5
16 L 1307 024 185 5
17 L 1196 029 242 5
18 L 1335 010 072 5
19 L 1335 010 072 5
20 L 1324 033 248 5
21 L 1363 032 238 5
24 L 1263 040 315 5
25 L 1194 069 574 5
1A R 1368 010 076 5
2A R 1308 018 135 5
3 R 1345 023 172 5
4A R 1340 011 079 5
4B R 1394 041 294 5
5A R 1292 028 216 5
5B R 1360 034 251 5
6A R 1372 023 166 5
7B R 1291 013 098 5
8 R 1369 025 183 5
9B R 1276 023 182 5
12A R 1317 034 256 5
12B R 1375 024 175 5
13A R 1334 021 155 5
13B R 1338 030 227 5
14 R 1366 023 167 5
15 R 1377 019 139 5
22A R 1344 016 118 5
22B R 1341 016 116 5
23 R 1334 029 217 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1277
Table 11 ISO Smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 796 005 059 5
2B L 806 012 144 5
6B L 814 018 219 5
7A L 789 009 112 5
9A L 781 024 306 5
10 L 802 020 245 5
11 L 784 018 225 5
12C L 794 021 263 5
16 L 850 014 168 5
17 L 774 016 203 5
18 L 787 015 187 5
19 L 787 015 187 5
20 L 769 014 188 5
21 L 808 008 097 5
24 L 792 010 128 5
25 L 751 030 400 5
1A R 767 005 068 5
2A R 727 008 109 5
3 R 779 008 099 5
4A R 748 011 146 5
4B R 758 013 172 5
5A R 782 011 144 5
5B R 766 017 216 5
6A R 773 009 117 5
7B R 716 011 160 5
8 R 754 010 127 5
9B R 755 008 107 5
12A R 755 006 078 5
12B R 771 008 102 5
13A R 740 017 225 5
13B R 769 007 091 5
14 R 761 011 140 5
15 R 750 018 246 5
22A R 757 008 110 5
22B R 759 007 088 5
23 R 732 009 117 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1377
Table 12 Intense smoking regime TPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 4551 091 200 5
2B L 4391 078 178 5
6B L 3936 067 170 5
9A L 4471 060 134 5
10 L 4667 073 157 5
11 L 5068 136 269 5
12C L 4644 031 066 5
17 L 4346 106 243 5
19 L 4566 087 190 5
20 L 4616 122 265 5
21 L 5008 077 153 5
24 L 4782 094 196 5
25 L 4434 081 182 5
1A R 4168 016 039 5
2A R 4014 024 061 5
3 R 4247 035 083 5
4A R 4097 039 095 5
4B R 4181 064 153 5
5B R 3997 040 101 5
6A R 4076 074 181 5
8 R 4044 043 107 5
9B R 4097 033 080 5
12A R 4125 046 112 5
12B R 4257 039 092 5
15 R 3957 052 131 5
22A R 4046 028 069 5
22B R 4015 045 112 5
23 R 3830 073 192 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1477
Table 13 Intense smoking regime Water mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1237 038 305 5
2B L 999 037 375 5
6B L 906 034 381 5
9A L 1147 043 373 5
10 L 1152 052 453 5
11 L 1488 053 356 5
12C L 1061 019 179 5
17 L 1027 028 274 5
19 L 1095 038 348 5
20 L 1216 083 681 5
21 L 1285 026 206 5
24 L 1235 060 484 5
25 L 1004 031 307 5
1A R 1024 014 138 5
2A R 797 016 197 5
3 R 974 031 317 5
4A R 911 034 368 5
4B R 931 027 287 5
5B R 815 041 507 5
6A R 923 038 411 5
8 R 929 033 354 5
9B R 927 028 301 5
12A R 1004 051 508 5
12B R 935 017 181 5
15 R 823 029 349 5
22A R 953 005 052 5
22B R 926 038 410 5
23 R 1598 065 404 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1577
Table 14 Intense smoking regime Nicotine mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 3484 0055 158 5
2B L 3434 0048 141 5
6B L 3342 0051 153 5
9A L 3494 0089 255 5
10 L 3578 0226 633 5
11 L 3620 0082 225 5
12C L 3402 0024 070 5
17 L 3622 0075 208 5
19 L 3520 0012 035 5
20 L 3552 0230 647 5
21 L 3712 0030 082 5
24 L 3524 0061 174 5
25 L 2986 0052 173 5
1A R 3385 0020 060 5
2A R 3317 0030 090 5
3 R 3479 0023 067 5
4A R 3369 0037 109 5
4B R 3340 0053 160 5
5B R 1677 0025 148 5
6A R 3390 0066 195 5
8 R 2967 0044 149 5
9B R 3410 0048 142 5
12A R 3452 0030 085 5
12B R 3520 0068 192 5
15 R 3333 0099 296 5
22A R 3222 0051 159 5
22B R 3210 0049 151 5
23 R 6610 0108 163 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1677
Table 15 Intense smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2965 054 183 5
2B L 3048 092 301 5
6B L 2696 035 131 5
9A L 2975 038 129 5
10 L 3157 047 148 5
11 L 3218 082 255 5
12C L 3243 015 047 5
17 L 3157 079 250 5
19 L 3119 084 268 5
20 L 3045 056 185 5
21 L 3351 066 198 5
24 L 3195 050 158 5
25 L 3132 054 174 5
1A R 2806 018 065 5
2A R 2885 012 043 5
3 R 2925 040 135 5
4A R 2849 021 074 5
4B R 2917 035 119 5
5B R 3013 023 077 5
6A R 2811 036 129 5
8 R 2819 021 074 5
9B R 2832 032 115 5
12A R 2776 048 171 5
12B R 2970 026 086 5
15 R 2800 035 124 5
22A R 2770 025 091 5
22B R 2768 049 178 5
23 R 1570 060 384 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1777
Table 16 Intense smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2478 034 137 5
2B L 2472 027 111 5
6B L 2367 039 165 5
9A L 2423 065 270 5
10 L 2373 018 077 5
11 L 2568 029 114 5
12C L 2497 028 113 5
17 L 2321 032 139 5
19 L 2488 022 086 5
20 L 2489 056 227 5
21 L 2523 045 177 5
24 L 2470 052 211 5
25 L 2399 089 369 5
1A R 2505 033 131 5
2A R 2485 037 149 5
3 R 2605 031 119 5
4A R 2513 031 125 5
4B R 2542 047 185 5
5B R 2480 022 088 5
6A R 2570 024 092 5
8 R 2532 047 185 5
9B R 2457 044 181 5
12A R 2506 023 093 5
12B R 2523 018 069 5
15 R 2547 039 154 5
22A R 2470 034 138 5
22B R 2466 032 130 5
23 R 2508 030 119 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1877
Table 17 Intense smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 1138 022 191 5
2B L 1154 019 162 5
6B L 1170 008 068 5
9A L 1095 013 114 5
10 L 1138 023 199 5
11 L 1127 016 138 5
12C L 1115 022 199 5
17 L 1110 009 079 5
19 L 1059 011 101 5
20 L 1087 019 176 5
21 L 1121 019 169 5
24 L 1106 027 248 5
25 L 1102 012 105 5
1A R 1111 018 159 5
2A R 1059 014 130 5
3 R 1152 013 110 5
4A R 1078 008 070 5
4B R 1105 016 143 5
5B R 1134 030 267 5
6A R 1136 004 034 5
8 R 1075 015 142 5
9B R 1077 006 054 5
12A R 1102 020 186 5
12B R 1097 016 148 5
15 R 1084 010 091 5
22A R 1112 016 147 5
22B R 1106 014 122 5
23 R 1066 009 088 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1977
Statistical Analysis 4
Exclusion of outliers 41
411 Numerical outlier technique Cochran amp Grubbs test
The statistical evaluation of data for this collaborative study followed the methods provided
by ISO 5725-21 For outlier testing the Grubbs and Cochran methods were used
ISO 5725-2 Tests Consistency
Cochranrsquos ndash test Within-laboratory variability Suitable for detecting whether the highest value in a set of laboratory standard deviations is an outlier or not
Grubbsrsquo ndash test Between-laboratory variability Suitable for detecting whether the highest (or lowest) laboratories averages are outliers or not
The protocol ldquoHarmonized statistical procedurerdquo defined by IUPAC (International Union of
Pure and Applied Chemistry) has been applied as well It consists of sequential applications of
the Cochran and Grubbs tests until no further outliers are detected or until a drop of more than
222 (for this study =29) in the original number of laboratories would occur (see flowchart
in Appendix F)
First apply the Cochran outlier test and if an outlying laboratory is identified then a single
value Grubbs test is performed on the individual values of this outlying laboratory (Individual
Grubbs) If no individual value is identified as outlier the outlying laboratory is removed
When an individual value is identified as an outlier only this value is removed
Afterwards single-value Grubbs test is applied and outlying laboratories are removed If no
laboratory is identified as outlier the pair-value test is applied (two values at the same end)
Remove any laboratory(ies) flagged by these tests but stop removal if more than 222 (2 of
9 laboratories) would be removed
The test was performed with both linear and rotary smoking machines together but also with
rotary respectively linear smoking machines separately The results provided in the report for
all smoking machines respectively with linear or rotary only smoking machines are obtained
after exclusion of the outliers for those respective categories
Note
The paired value Grubbsrsquo test is an extension of the single value Grubbs test for pairs of
outliers The use is advised in ISO 5725 to detect pairs of outlier undetectable sequentially by
using single value Grubbs test
The outlying laboratories are provided in the Tables 18 to 23
Repeatability and reproducibility estimation 42
Repeatability and reproducibility limits are calculated for both smoking regimes each
parameter and for both smoking machine types The results are summarized in tables 18 to 23
with all machines grouped respectively with linear or rotary machines only both with ISO
and intense smoking regimes Outlying laboratories are provided in the same tables The
corresponding graphs named ldquoindividual valuesrdquo are given in Part 5 of this report
1 ISO 5725-21994 Accuracy (trueness and precision) of measurement methods and results ndash Part 2 Basic
method for the determination of repeatability and reproducibility of a standard measurement method
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 2077
Table 18 r amp R estimations for CM8 under ISO smoking regime (all machines)
p n Global Mean Sr CVr[] r SR CVR [] R C GG2 Stragglers Parameter
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 977
Table 8 ISO Smoking regime Nicotine mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1704 0029 170 5
2B L 1706 0039 227 5
6B L 1624 0048 295 5
7A L 1687 0033 194 5
9A L 1612 0200 1240 5
10 L 1748 0070 401 5
11 L 1691 0028 166 5
12C L 1669 0034 206 5
16 L 1731 0028 159 5
17 L 1674 0046 276 5
18 L 1697 0014 082 5
19 L 1697 0014 082 5
20 L 1734 0021 124 5
21 L 1812 0048 266 5
24 L 1694 0037 217 5
25 L 1743 0154 883 5
1A R 1669 0023 141 5
2A R 1638 0037 224 5
3 R 1652 0018 110 5
4A R 1630 0042 255 5
4B R 1653 0035 214 5
5A R 1612 0023 142 5
5B R 1602 0023 141 5
6A R 1661 0037 225 5
7B R 1564 0022 140 5
8 R 1535 0031 204 5
9B R 1659 0047 285 5
12A R 1719 0024 142 5
12B R 1718 0037 216 5
13A R 1497 0024 163 5
13B R 1546 0013 086 5
14 R 1590 0035 217 5
15 R 1651 0030 181 5
22A R 1612 0011 068 5
22B R 1630 0012 075 5
23 R 1639 0026 159 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1077
Table 9 ISO smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1462 016 111 5
2B L 1449 053 366 5
6B L 1294 044 344 5
7A L 1460 031 214 5
9A L 1395 011 080 5
10 L 1455 039 269 5
11 L 1518 036 236 5
12C L 1439 049 338 5
16 L 1427 013 092 5
17 L 1304 054 413 5
18 L 1456 020 135 5
19 L 1456 020 135 5
20 L 1395 036 255 5
21 L 1531 057 371 5
24 L 1466 023 154 5
25 L 1306 066 509 5
1A R 1367 020 145 5
2A R 1361 023 169 5
3 R 1398 012 083 5
4A R 1363 024 176 5
4B R 1391 028 201 5
5A R 1347 014 107 5
5B R 1372 023 166 5
6A R 1346 019 142 5
7B R 1305 020 153 5
8 R 1378 026 192 5
9B R 1342 015 114 5
12A R 1337 037 278 5
12B R 1375 018 129 5
13A R 1319 015 112 5
13B R 1341 009 069 5
14 R 1359 028 204 5
15 R 1366 029 214 5
22A R 1371 019 136 5
22B R 1353 024 175 5
23 R 1308 037 283 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1177
Table 10 ISO Smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1335 020 150 5
2B L 1297 037 288 5
6B L 1260 099 790 5
7A L 1374 034 249 5
9A L 1233 019 153 5
10 L 1219 054 445 5
11 L 1267 044 350 5
12C L 1325 033 248 5
16 L 1307 024 185 5
17 L 1196 029 242 5
18 L 1335 010 072 5
19 L 1335 010 072 5
20 L 1324 033 248 5
21 L 1363 032 238 5
24 L 1263 040 315 5
25 L 1194 069 574 5
1A R 1368 010 076 5
2A R 1308 018 135 5
3 R 1345 023 172 5
4A R 1340 011 079 5
4B R 1394 041 294 5
5A R 1292 028 216 5
5B R 1360 034 251 5
6A R 1372 023 166 5
7B R 1291 013 098 5
8 R 1369 025 183 5
9B R 1276 023 182 5
12A R 1317 034 256 5
12B R 1375 024 175 5
13A R 1334 021 155 5
13B R 1338 030 227 5
14 R 1366 023 167 5
15 R 1377 019 139 5
22A R 1344 016 118 5
22B R 1341 016 116 5
23 R 1334 029 217 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1277
Table 11 ISO Smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 796 005 059 5
2B L 806 012 144 5
6B L 814 018 219 5
7A L 789 009 112 5
9A L 781 024 306 5
10 L 802 020 245 5
11 L 784 018 225 5
12C L 794 021 263 5
16 L 850 014 168 5
17 L 774 016 203 5
18 L 787 015 187 5
19 L 787 015 187 5
20 L 769 014 188 5
21 L 808 008 097 5
24 L 792 010 128 5
25 L 751 030 400 5
1A R 767 005 068 5
2A R 727 008 109 5
3 R 779 008 099 5
4A R 748 011 146 5
4B R 758 013 172 5
5A R 782 011 144 5
5B R 766 017 216 5
6A R 773 009 117 5
7B R 716 011 160 5
8 R 754 010 127 5
9B R 755 008 107 5
12A R 755 006 078 5
12B R 771 008 102 5
13A R 740 017 225 5
13B R 769 007 091 5
14 R 761 011 140 5
15 R 750 018 246 5
22A R 757 008 110 5
22B R 759 007 088 5
23 R 732 009 117 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1377
Table 12 Intense smoking regime TPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 4551 091 200 5
2B L 4391 078 178 5
6B L 3936 067 170 5
9A L 4471 060 134 5
10 L 4667 073 157 5
11 L 5068 136 269 5
12C L 4644 031 066 5
17 L 4346 106 243 5
19 L 4566 087 190 5
20 L 4616 122 265 5
21 L 5008 077 153 5
24 L 4782 094 196 5
25 L 4434 081 182 5
1A R 4168 016 039 5
2A R 4014 024 061 5
3 R 4247 035 083 5
4A R 4097 039 095 5
4B R 4181 064 153 5
5B R 3997 040 101 5
6A R 4076 074 181 5
8 R 4044 043 107 5
9B R 4097 033 080 5
12A R 4125 046 112 5
12B R 4257 039 092 5
15 R 3957 052 131 5
22A R 4046 028 069 5
22B R 4015 045 112 5
23 R 3830 073 192 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1477
Table 13 Intense smoking regime Water mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1237 038 305 5
2B L 999 037 375 5
6B L 906 034 381 5
9A L 1147 043 373 5
10 L 1152 052 453 5
11 L 1488 053 356 5
12C L 1061 019 179 5
17 L 1027 028 274 5
19 L 1095 038 348 5
20 L 1216 083 681 5
21 L 1285 026 206 5
24 L 1235 060 484 5
25 L 1004 031 307 5
1A R 1024 014 138 5
2A R 797 016 197 5
3 R 974 031 317 5
4A R 911 034 368 5
4B R 931 027 287 5
5B R 815 041 507 5
6A R 923 038 411 5
8 R 929 033 354 5
9B R 927 028 301 5
12A R 1004 051 508 5
12B R 935 017 181 5
15 R 823 029 349 5
22A R 953 005 052 5
22B R 926 038 410 5
23 R 1598 065 404 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1577
Table 14 Intense smoking regime Nicotine mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 3484 0055 158 5
2B L 3434 0048 141 5
6B L 3342 0051 153 5
9A L 3494 0089 255 5
10 L 3578 0226 633 5
11 L 3620 0082 225 5
12C L 3402 0024 070 5
17 L 3622 0075 208 5
19 L 3520 0012 035 5
20 L 3552 0230 647 5
21 L 3712 0030 082 5
24 L 3524 0061 174 5
25 L 2986 0052 173 5
1A R 3385 0020 060 5
2A R 3317 0030 090 5
3 R 3479 0023 067 5
4A R 3369 0037 109 5
4B R 3340 0053 160 5
5B R 1677 0025 148 5
6A R 3390 0066 195 5
8 R 2967 0044 149 5
9B R 3410 0048 142 5
12A R 3452 0030 085 5
12B R 3520 0068 192 5
15 R 3333 0099 296 5
22A R 3222 0051 159 5
22B R 3210 0049 151 5
23 R 6610 0108 163 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1677
Table 15 Intense smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2965 054 183 5
2B L 3048 092 301 5
6B L 2696 035 131 5
9A L 2975 038 129 5
10 L 3157 047 148 5
11 L 3218 082 255 5
12C L 3243 015 047 5
17 L 3157 079 250 5
19 L 3119 084 268 5
20 L 3045 056 185 5
21 L 3351 066 198 5
24 L 3195 050 158 5
25 L 3132 054 174 5
1A R 2806 018 065 5
2A R 2885 012 043 5
3 R 2925 040 135 5
4A R 2849 021 074 5
4B R 2917 035 119 5
5B R 3013 023 077 5
6A R 2811 036 129 5
8 R 2819 021 074 5
9B R 2832 032 115 5
12A R 2776 048 171 5
12B R 2970 026 086 5
15 R 2800 035 124 5
22A R 2770 025 091 5
22B R 2768 049 178 5
23 R 1570 060 384 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1777
Table 16 Intense smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2478 034 137 5
2B L 2472 027 111 5
6B L 2367 039 165 5
9A L 2423 065 270 5
10 L 2373 018 077 5
11 L 2568 029 114 5
12C L 2497 028 113 5
17 L 2321 032 139 5
19 L 2488 022 086 5
20 L 2489 056 227 5
21 L 2523 045 177 5
24 L 2470 052 211 5
25 L 2399 089 369 5
1A R 2505 033 131 5
2A R 2485 037 149 5
3 R 2605 031 119 5
4A R 2513 031 125 5
4B R 2542 047 185 5
5B R 2480 022 088 5
6A R 2570 024 092 5
8 R 2532 047 185 5
9B R 2457 044 181 5
12A R 2506 023 093 5
12B R 2523 018 069 5
15 R 2547 039 154 5
22A R 2470 034 138 5
22B R 2466 032 130 5
23 R 2508 030 119 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1877
Table 17 Intense smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 1138 022 191 5
2B L 1154 019 162 5
6B L 1170 008 068 5
9A L 1095 013 114 5
10 L 1138 023 199 5
11 L 1127 016 138 5
12C L 1115 022 199 5
17 L 1110 009 079 5
19 L 1059 011 101 5
20 L 1087 019 176 5
21 L 1121 019 169 5
24 L 1106 027 248 5
25 L 1102 012 105 5
1A R 1111 018 159 5
2A R 1059 014 130 5
3 R 1152 013 110 5
4A R 1078 008 070 5
4B R 1105 016 143 5
5B R 1134 030 267 5
6A R 1136 004 034 5
8 R 1075 015 142 5
9B R 1077 006 054 5
12A R 1102 020 186 5
12B R 1097 016 148 5
15 R 1084 010 091 5
22A R 1112 016 147 5
22B R 1106 014 122 5
23 R 1066 009 088 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1977
Statistical Analysis 4
Exclusion of outliers 41
411 Numerical outlier technique Cochran amp Grubbs test
The statistical evaluation of data for this collaborative study followed the methods provided
by ISO 5725-21 For outlier testing the Grubbs and Cochran methods were used
ISO 5725-2 Tests Consistency
Cochranrsquos ndash test Within-laboratory variability Suitable for detecting whether the highest value in a set of laboratory standard deviations is an outlier or not
Grubbsrsquo ndash test Between-laboratory variability Suitable for detecting whether the highest (or lowest) laboratories averages are outliers or not
The protocol ldquoHarmonized statistical procedurerdquo defined by IUPAC (International Union of
Pure and Applied Chemistry) has been applied as well It consists of sequential applications of
the Cochran and Grubbs tests until no further outliers are detected or until a drop of more than
222 (for this study =29) in the original number of laboratories would occur (see flowchart
in Appendix F)
First apply the Cochran outlier test and if an outlying laboratory is identified then a single
value Grubbs test is performed on the individual values of this outlying laboratory (Individual
Grubbs) If no individual value is identified as outlier the outlying laboratory is removed
When an individual value is identified as an outlier only this value is removed
Afterwards single-value Grubbs test is applied and outlying laboratories are removed If no
laboratory is identified as outlier the pair-value test is applied (two values at the same end)
Remove any laboratory(ies) flagged by these tests but stop removal if more than 222 (2 of
9 laboratories) would be removed
The test was performed with both linear and rotary smoking machines together but also with
rotary respectively linear smoking machines separately The results provided in the report for
all smoking machines respectively with linear or rotary only smoking machines are obtained
after exclusion of the outliers for those respective categories
Note
The paired value Grubbsrsquo test is an extension of the single value Grubbs test for pairs of
outliers The use is advised in ISO 5725 to detect pairs of outlier undetectable sequentially by
using single value Grubbs test
The outlying laboratories are provided in the Tables 18 to 23
Repeatability and reproducibility estimation 42
Repeatability and reproducibility limits are calculated for both smoking regimes each
parameter and for both smoking machine types The results are summarized in tables 18 to 23
with all machines grouped respectively with linear or rotary machines only both with ISO
and intense smoking regimes Outlying laboratories are provided in the same tables The
corresponding graphs named ldquoindividual valuesrdquo are given in Part 5 of this report
1 ISO 5725-21994 Accuracy (trueness and precision) of measurement methods and results ndash Part 2 Basic
method for the determination of repeatability and reproducibility of a standard measurement method
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 2077
Table 18 r amp R estimations for CM8 under ISO smoking regime (all machines)
p n Global Mean Sr CVr[] r SR CVR [] R C GG2 Stragglers Parameter
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1077
Table 9 ISO smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1462 016 111 5
2B L 1449 053 366 5
6B L 1294 044 344 5
7A L 1460 031 214 5
9A L 1395 011 080 5
10 L 1455 039 269 5
11 L 1518 036 236 5
12C L 1439 049 338 5
16 L 1427 013 092 5
17 L 1304 054 413 5
18 L 1456 020 135 5
19 L 1456 020 135 5
20 L 1395 036 255 5
21 L 1531 057 371 5
24 L 1466 023 154 5
25 L 1306 066 509 5
1A R 1367 020 145 5
2A R 1361 023 169 5
3 R 1398 012 083 5
4A R 1363 024 176 5
4B R 1391 028 201 5
5A R 1347 014 107 5
5B R 1372 023 166 5
6A R 1346 019 142 5
7B R 1305 020 153 5
8 R 1378 026 192 5
9B R 1342 015 114 5
12A R 1337 037 278 5
12B R 1375 018 129 5
13A R 1319 015 112 5
13B R 1341 009 069 5
14 R 1359 028 204 5
15 R 1366 029 214 5
22A R 1371 019 136 5
22B R 1353 024 175 5
23 R 1308 037 283 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1177
Table 10 ISO Smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1335 020 150 5
2B L 1297 037 288 5
6B L 1260 099 790 5
7A L 1374 034 249 5
9A L 1233 019 153 5
10 L 1219 054 445 5
11 L 1267 044 350 5
12C L 1325 033 248 5
16 L 1307 024 185 5
17 L 1196 029 242 5
18 L 1335 010 072 5
19 L 1335 010 072 5
20 L 1324 033 248 5
21 L 1363 032 238 5
24 L 1263 040 315 5
25 L 1194 069 574 5
1A R 1368 010 076 5
2A R 1308 018 135 5
3 R 1345 023 172 5
4A R 1340 011 079 5
4B R 1394 041 294 5
5A R 1292 028 216 5
5B R 1360 034 251 5
6A R 1372 023 166 5
7B R 1291 013 098 5
8 R 1369 025 183 5
9B R 1276 023 182 5
12A R 1317 034 256 5
12B R 1375 024 175 5
13A R 1334 021 155 5
13B R 1338 030 227 5
14 R 1366 023 167 5
15 R 1377 019 139 5
22A R 1344 016 118 5
22B R 1341 016 116 5
23 R 1334 029 217 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1277
Table 11 ISO Smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 796 005 059 5
2B L 806 012 144 5
6B L 814 018 219 5
7A L 789 009 112 5
9A L 781 024 306 5
10 L 802 020 245 5
11 L 784 018 225 5
12C L 794 021 263 5
16 L 850 014 168 5
17 L 774 016 203 5
18 L 787 015 187 5
19 L 787 015 187 5
20 L 769 014 188 5
21 L 808 008 097 5
24 L 792 010 128 5
25 L 751 030 400 5
1A R 767 005 068 5
2A R 727 008 109 5
3 R 779 008 099 5
4A R 748 011 146 5
4B R 758 013 172 5
5A R 782 011 144 5
5B R 766 017 216 5
6A R 773 009 117 5
7B R 716 011 160 5
8 R 754 010 127 5
9B R 755 008 107 5
12A R 755 006 078 5
12B R 771 008 102 5
13A R 740 017 225 5
13B R 769 007 091 5
14 R 761 011 140 5
15 R 750 018 246 5
22A R 757 008 110 5
22B R 759 007 088 5
23 R 732 009 117 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1377
Table 12 Intense smoking regime TPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 4551 091 200 5
2B L 4391 078 178 5
6B L 3936 067 170 5
9A L 4471 060 134 5
10 L 4667 073 157 5
11 L 5068 136 269 5
12C L 4644 031 066 5
17 L 4346 106 243 5
19 L 4566 087 190 5
20 L 4616 122 265 5
21 L 5008 077 153 5
24 L 4782 094 196 5
25 L 4434 081 182 5
1A R 4168 016 039 5
2A R 4014 024 061 5
3 R 4247 035 083 5
4A R 4097 039 095 5
4B R 4181 064 153 5
5B R 3997 040 101 5
6A R 4076 074 181 5
8 R 4044 043 107 5
9B R 4097 033 080 5
12A R 4125 046 112 5
12B R 4257 039 092 5
15 R 3957 052 131 5
22A R 4046 028 069 5
22B R 4015 045 112 5
23 R 3830 073 192 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1477
Table 13 Intense smoking regime Water mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1237 038 305 5
2B L 999 037 375 5
6B L 906 034 381 5
9A L 1147 043 373 5
10 L 1152 052 453 5
11 L 1488 053 356 5
12C L 1061 019 179 5
17 L 1027 028 274 5
19 L 1095 038 348 5
20 L 1216 083 681 5
21 L 1285 026 206 5
24 L 1235 060 484 5
25 L 1004 031 307 5
1A R 1024 014 138 5
2A R 797 016 197 5
3 R 974 031 317 5
4A R 911 034 368 5
4B R 931 027 287 5
5B R 815 041 507 5
6A R 923 038 411 5
8 R 929 033 354 5
9B R 927 028 301 5
12A R 1004 051 508 5
12B R 935 017 181 5
15 R 823 029 349 5
22A R 953 005 052 5
22B R 926 038 410 5
23 R 1598 065 404 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1577
Table 14 Intense smoking regime Nicotine mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 3484 0055 158 5
2B L 3434 0048 141 5
6B L 3342 0051 153 5
9A L 3494 0089 255 5
10 L 3578 0226 633 5
11 L 3620 0082 225 5
12C L 3402 0024 070 5
17 L 3622 0075 208 5
19 L 3520 0012 035 5
20 L 3552 0230 647 5
21 L 3712 0030 082 5
24 L 3524 0061 174 5
25 L 2986 0052 173 5
1A R 3385 0020 060 5
2A R 3317 0030 090 5
3 R 3479 0023 067 5
4A R 3369 0037 109 5
4B R 3340 0053 160 5
5B R 1677 0025 148 5
6A R 3390 0066 195 5
8 R 2967 0044 149 5
9B R 3410 0048 142 5
12A R 3452 0030 085 5
12B R 3520 0068 192 5
15 R 3333 0099 296 5
22A R 3222 0051 159 5
22B R 3210 0049 151 5
23 R 6610 0108 163 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1677
Table 15 Intense smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2965 054 183 5
2B L 3048 092 301 5
6B L 2696 035 131 5
9A L 2975 038 129 5
10 L 3157 047 148 5
11 L 3218 082 255 5
12C L 3243 015 047 5
17 L 3157 079 250 5
19 L 3119 084 268 5
20 L 3045 056 185 5
21 L 3351 066 198 5
24 L 3195 050 158 5
25 L 3132 054 174 5
1A R 2806 018 065 5
2A R 2885 012 043 5
3 R 2925 040 135 5
4A R 2849 021 074 5
4B R 2917 035 119 5
5B R 3013 023 077 5
6A R 2811 036 129 5
8 R 2819 021 074 5
9B R 2832 032 115 5
12A R 2776 048 171 5
12B R 2970 026 086 5
15 R 2800 035 124 5
22A R 2770 025 091 5
22B R 2768 049 178 5
23 R 1570 060 384 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1777
Table 16 Intense smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2478 034 137 5
2B L 2472 027 111 5
6B L 2367 039 165 5
9A L 2423 065 270 5
10 L 2373 018 077 5
11 L 2568 029 114 5
12C L 2497 028 113 5
17 L 2321 032 139 5
19 L 2488 022 086 5
20 L 2489 056 227 5
21 L 2523 045 177 5
24 L 2470 052 211 5
25 L 2399 089 369 5
1A R 2505 033 131 5
2A R 2485 037 149 5
3 R 2605 031 119 5
4A R 2513 031 125 5
4B R 2542 047 185 5
5B R 2480 022 088 5
6A R 2570 024 092 5
8 R 2532 047 185 5
9B R 2457 044 181 5
12A R 2506 023 093 5
12B R 2523 018 069 5
15 R 2547 039 154 5
22A R 2470 034 138 5
22B R 2466 032 130 5
23 R 2508 030 119 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1877
Table 17 Intense smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 1138 022 191 5
2B L 1154 019 162 5
6B L 1170 008 068 5
9A L 1095 013 114 5
10 L 1138 023 199 5
11 L 1127 016 138 5
12C L 1115 022 199 5
17 L 1110 009 079 5
19 L 1059 011 101 5
20 L 1087 019 176 5
21 L 1121 019 169 5
24 L 1106 027 248 5
25 L 1102 012 105 5
1A R 1111 018 159 5
2A R 1059 014 130 5
3 R 1152 013 110 5
4A R 1078 008 070 5
4B R 1105 016 143 5
5B R 1134 030 267 5
6A R 1136 004 034 5
8 R 1075 015 142 5
9B R 1077 006 054 5
12A R 1102 020 186 5
12B R 1097 016 148 5
15 R 1084 010 091 5
22A R 1112 016 147 5
22B R 1106 014 122 5
23 R 1066 009 088 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1977
Statistical Analysis 4
Exclusion of outliers 41
411 Numerical outlier technique Cochran amp Grubbs test
The statistical evaluation of data for this collaborative study followed the methods provided
by ISO 5725-21 For outlier testing the Grubbs and Cochran methods were used
ISO 5725-2 Tests Consistency
Cochranrsquos ndash test Within-laboratory variability Suitable for detecting whether the highest value in a set of laboratory standard deviations is an outlier or not
Grubbsrsquo ndash test Between-laboratory variability Suitable for detecting whether the highest (or lowest) laboratories averages are outliers or not
The protocol ldquoHarmonized statistical procedurerdquo defined by IUPAC (International Union of
Pure and Applied Chemistry) has been applied as well It consists of sequential applications of
the Cochran and Grubbs tests until no further outliers are detected or until a drop of more than
222 (for this study =29) in the original number of laboratories would occur (see flowchart
in Appendix F)
First apply the Cochran outlier test and if an outlying laboratory is identified then a single
value Grubbs test is performed on the individual values of this outlying laboratory (Individual
Grubbs) If no individual value is identified as outlier the outlying laboratory is removed
When an individual value is identified as an outlier only this value is removed
Afterwards single-value Grubbs test is applied and outlying laboratories are removed If no
laboratory is identified as outlier the pair-value test is applied (two values at the same end)
Remove any laboratory(ies) flagged by these tests but stop removal if more than 222 (2 of
9 laboratories) would be removed
The test was performed with both linear and rotary smoking machines together but also with
rotary respectively linear smoking machines separately The results provided in the report for
all smoking machines respectively with linear or rotary only smoking machines are obtained
after exclusion of the outliers for those respective categories
Note
The paired value Grubbsrsquo test is an extension of the single value Grubbs test for pairs of
outliers The use is advised in ISO 5725 to detect pairs of outlier undetectable sequentially by
using single value Grubbs test
The outlying laboratories are provided in the Tables 18 to 23
Repeatability and reproducibility estimation 42
Repeatability and reproducibility limits are calculated for both smoking regimes each
parameter and for both smoking machine types The results are summarized in tables 18 to 23
with all machines grouped respectively with linear or rotary machines only both with ISO
and intense smoking regimes Outlying laboratories are provided in the same tables The
corresponding graphs named ldquoindividual valuesrdquo are given in Part 5 of this report
1 ISO 5725-21994 Accuracy (trueness and precision) of measurement methods and results ndash Part 2 Basic
method for the determination of repeatability and reproducibility of a standard measurement method
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 2077
Table 18 r amp R estimations for CM8 under ISO smoking regime (all machines)
p n Global Mean Sr CVr[] r SR CVR [] R C GG2 Stragglers Parameter
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1177
Table 10 ISO Smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1335 020 150 5
2B L 1297 037 288 5
6B L 1260 099 790 5
7A L 1374 034 249 5
9A L 1233 019 153 5
10 L 1219 054 445 5
11 L 1267 044 350 5
12C L 1325 033 248 5
16 L 1307 024 185 5
17 L 1196 029 242 5
18 L 1335 010 072 5
19 L 1335 010 072 5
20 L 1324 033 248 5
21 L 1363 032 238 5
24 L 1263 040 315 5
25 L 1194 069 574 5
1A R 1368 010 076 5
2A R 1308 018 135 5
3 R 1345 023 172 5
4A R 1340 011 079 5
4B R 1394 041 294 5
5A R 1292 028 216 5
5B R 1360 034 251 5
6A R 1372 023 166 5
7B R 1291 013 098 5
8 R 1369 025 183 5
9B R 1276 023 182 5
12A R 1317 034 256 5
12B R 1375 024 175 5
13A R 1334 021 155 5
13B R 1338 030 227 5
14 R 1366 023 167 5
15 R 1377 019 139 5
22A R 1344 016 118 5
22B R 1341 016 116 5
23 R 1334 029 217 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1277
Table 11 ISO Smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 796 005 059 5
2B L 806 012 144 5
6B L 814 018 219 5
7A L 789 009 112 5
9A L 781 024 306 5
10 L 802 020 245 5
11 L 784 018 225 5
12C L 794 021 263 5
16 L 850 014 168 5
17 L 774 016 203 5
18 L 787 015 187 5
19 L 787 015 187 5
20 L 769 014 188 5
21 L 808 008 097 5
24 L 792 010 128 5
25 L 751 030 400 5
1A R 767 005 068 5
2A R 727 008 109 5
3 R 779 008 099 5
4A R 748 011 146 5
4B R 758 013 172 5
5A R 782 011 144 5
5B R 766 017 216 5
6A R 773 009 117 5
7B R 716 011 160 5
8 R 754 010 127 5
9B R 755 008 107 5
12A R 755 006 078 5
12B R 771 008 102 5
13A R 740 017 225 5
13B R 769 007 091 5
14 R 761 011 140 5
15 R 750 018 246 5
22A R 757 008 110 5
22B R 759 007 088 5
23 R 732 009 117 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1377
Table 12 Intense smoking regime TPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 4551 091 200 5
2B L 4391 078 178 5
6B L 3936 067 170 5
9A L 4471 060 134 5
10 L 4667 073 157 5
11 L 5068 136 269 5
12C L 4644 031 066 5
17 L 4346 106 243 5
19 L 4566 087 190 5
20 L 4616 122 265 5
21 L 5008 077 153 5
24 L 4782 094 196 5
25 L 4434 081 182 5
1A R 4168 016 039 5
2A R 4014 024 061 5
3 R 4247 035 083 5
4A R 4097 039 095 5
4B R 4181 064 153 5
5B R 3997 040 101 5
6A R 4076 074 181 5
8 R 4044 043 107 5
9B R 4097 033 080 5
12A R 4125 046 112 5
12B R 4257 039 092 5
15 R 3957 052 131 5
22A R 4046 028 069 5
22B R 4015 045 112 5
23 R 3830 073 192 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1477
Table 13 Intense smoking regime Water mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1237 038 305 5
2B L 999 037 375 5
6B L 906 034 381 5
9A L 1147 043 373 5
10 L 1152 052 453 5
11 L 1488 053 356 5
12C L 1061 019 179 5
17 L 1027 028 274 5
19 L 1095 038 348 5
20 L 1216 083 681 5
21 L 1285 026 206 5
24 L 1235 060 484 5
25 L 1004 031 307 5
1A R 1024 014 138 5
2A R 797 016 197 5
3 R 974 031 317 5
4A R 911 034 368 5
4B R 931 027 287 5
5B R 815 041 507 5
6A R 923 038 411 5
8 R 929 033 354 5
9B R 927 028 301 5
12A R 1004 051 508 5
12B R 935 017 181 5
15 R 823 029 349 5
22A R 953 005 052 5
22B R 926 038 410 5
23 R 1598 065 404 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1577
Table 14 Intense smoking regime Nicotine mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 3484 0055 158 5
2B L 3434 0048 141 5
6B L 3342 0051 153 5
9A L 3494 0089 255 5
10 L 3578 0226 633 5
11 L 3620 0082 225 5
12C L 3402 0024 070 5
17 L 3622 0075 208 5
19 L 3520 0012 035 5
20 L 3552 0230 647 5
21 L 3712 0030 082 5
24 L 3524 0061 174 5
25 L 2986 0052 173 5
1A R 3385 0020 060 5
2A R 3317 0030 090 5
3 R 3479 0023 067 5
4A R 3369 0037 109 5
4B R 3340 0053 160 5
5B R 1677 0025 148 5
6A R 3390 0066 195 5
8 R 2967 0044 149 5
9B R 3410 0048 142 5
12A R 3452 0030 085 5
12B R 3520 0068 192 5
15 R 3333 0099 296 5
22A R 3222 0051 159 5
22B R 3210 0049 151 5
23 R 6610 0108 163 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1677
Table 15 Intense smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2965 054 183 5
2B L 3048 092 301 5
6B L 2696 035 131 5
9A L 2975 038 129 5
10 L 3157 047 148 5
11 L 3218 082 255 5
12C L 3243 015 047 5
17 L 3157 079 250 5
19 L 3119 084 268 5
20 L 3045 056 185 5
21 L 3351 066 198 5
24 L 3195 050 158 5
25 L 3132 054 174 5
1A R 2806 018 065 5
2A R 2885 012 043 5
3 R 2925 040 135 5
4A R 2849 021 074 5
4B R 2917 035 119 5
5B R 3013 023 077 5
6A R 2811 036 129 5
8 R 2819 021 074 5
9B R 2832 032 115 5
12A R 2776 048 171 5
12B R 2970 026 086 5
15 R 2800 035 124 5
22A R 2770 025 091 5
22B R 2768 049 178 5
23 R 1570 060 384 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1777
Table 16 Intense smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2478 034 137 5
2B L 2472 027 111 5
6B L 2367 039 165 5
9A L 2423 065 270 5
10 L 2373 018 077 5
11 L 2568 029 114 5
12C L 2497 028 113 5
17 L 2321 032 139 5
19 L 2488 022 086 5
20 L 2489 056 227 5
21 L 2523 045 177 5
24 L 2470 052 211 5
25 L 2399 089 369 5
1A R 2505 033 131 5
2A R 2485 037 149 5
3 R 2605 031 119 5
4A R 2513 031 125 5
4B R 2542 047 185 5
5B R 2480 022 088 5
6A R 2570 024 092 5
8 R 2532 047 185 5
9B R 2457 044 181 5
12A R 2506 023 093 5
12B R 2523 018 069 5
15 R 2547 039 154 5
22A R 2470 034 138 5
22B R 2466 032 130 5
23 R 2508 030 119 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1877
Table 17 Intense smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 1138 022 191 5
2B L 1154 019 162 5
6B L 1170 008 068 5
9A L 1095 013 114 5
10 L 1138 023 199 5
11 L 1127 016 138 5
12C L 1115 022 199 5
17 L 1110 009 079 5
19 L 1059 011 101 5
20 L 1087 019 176 5
21 L 1121 019 169 5
24 L 1106 027 248 5
25 L 1102 012 105 5
1A R 1111 018 159 5
2A R 1059 014 130 5
3 R 1152 013 110 5
4A R 1078 008 070 5
4B R 1105 016 143 5
5B R 1134 030 267 5
6A R 1136 004 034 5
8 R 1075 015 142 5
9B R 1077 006 054 5
12A R 1102 020 186 5
12B R 1097 016 148 5
15 R 1084 010 091 5
22A R 1112 016 147 5
22B R 1106 014 122 5
23 R 1066 009 088 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1977
Statistical Analysis 4
Exclusion of outliers 41
411 Numerical outlier technique Cochran amp Grubbs test
The statistical evaluation of data for this collaborative study followed the methods provided
by ISO 5725-21 For outlier testing the Grubbs and Cochran methods were used
ISO 5725-2 Tests Consistency
Cochranrsquos ndash test Within-laboratory variability Suitable for detecting whether the highest value in a set of laboratory standard deviations is an outlier or not
Grubbsrsquo ndash test Between-laboratory variability Suitable for detecting whether the highest (or lowest) laboratories averages are outliers or not
The protocol ldquoHarmonized statistical procedurerdquo defined by IUPAC (International Union of
Pure and Applied Chemistry) has been applied as well It consists of sequential applications of
the Cochran and Grubbs tests until no further outliers are detected or until a drop of more than
222 (for this study =29) in the original number of laboratories would occur (see flowchart
in Appendix F)
First apply the Cochran outlier test and if an outlying laboratory is identified then a single
value Grubbs test is performed on the individual values of this outlying laboratory (Individual
Grubbs) If no individual value is identified as outlier the outlying laboratory is removed
When an individual value is identified as an outlier only this value is removed
Afterwards single-value Grubbs test is applied and outlying laboratories are removed If no
laboratory is identified as outlier the pair-value test is applied (two values at the same end)
Remove any laboratory(ies) flagged by these tests but stop removal if more than 222 (2 of
9 laboratories) would be removed
The test was performed with both linear and rotary smoking machines together but also with
rotary respectively linear smoking machines separately The results provided in the report for
all smoking machines respectively with linear or rotary only smoking machines are obtained
after exclusion of the outliers for those respective categories
Note
The paired value Grubbsrsquo test is an extension of the single value Grubbs test for pairs of
outliers The use is advised in ISO 5725 to detect pairs of outlier undetectable sequentially by
using single value Grubbs test
The outlying laboratories are provided in the Tables 18 to 23
Repeatability and reproducibility estimation 42
Repeatability and reproducibility limits are calculated for both smoking regimes each
parameter and for both smoking machine types The results are summarized in tables 18 to 23
with all machines grouped respectively with linear or rotary machines only both with ISO
and intense smoking regimes Outlying laboratories are provided in the same tables The
corresponding graphs named ldquoindividual valuesrdquo are given in Part 5 of this report
1 ISO 5725-21994 Accuracy (trueness and precision) of measurement methods and results ndash Part 2 Basic
method for the determination of repeatability and reproducibility of a standard measurement method
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 2077
Table 18 r amp R estimations for CM8 under ISO smoking regime (all machines)
p n Global Mean Sr CVr[] r SR CVR [] R C GG2 Stragglers Parameter
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1277
Table 11 ISO Smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 796 005 059 5
2B L 806 012 144 5
6B L 814 018 219 5
7A L 789 009 112 5
9A L 781 024 306 5
10 L 802 020 245 5
11 L 784 018 225 5
12C L 794 021 263 5
16 L 850 014 168 5
17 L 774 016 203 5
18 L 787 015 187 5
19 L 787 015 187 5
20 L 769 014 188 5
21 L 808 008 097 5
24 L 792 010 128 5
25 L 751 030 400 5
1A R 767 005 068 5
2A R 727 008 109 5
3 R 779 008 099 5
4A R 748 011 146 5
4B R 758 013 172 5
5A R 782 011 144 5
5B R 766 017 216 5
6A R 773 009 117 5
7B R 716 011 160 5
8 R 754 010 127 5
9B R 755 008 107 5
12A R 755 006 078 5
12B R 771 008 102 5
13A R 740 017 225 5
13B R 769 007 091 5
14 R 761 011 140 5
15 R 750 018 246 5
22A R 757 008 110 5
22B R 759 007 088 5
23 R 732 009 117 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1377
Table 12 Intense smoking regime TPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 4551 091 200 5
2B L 4391 078 178 5
6B L 3936 067 170 5
9A L 4471 060 134 5
10 L 4667 073 157 5
11 L 5068 136 269 5
12C L 4644 031 066 5
17 L 4346 106 243 5
19 L 4566 087 190 5
20 L 4616 122 265 5
21 L 5008 077 153 5
24 L 4782 094 196 5
25 L 4434 081 182 5
1A R 4168 016 039 5
2A R 4014 024 061 5
3 R 4247 035 083 5
4A R 4097 039 095 5
4B R 4181 064 153 5
5B R 3997 040 101 5
6A R 4076 074 181 5
8 R 4044 043 107 5
9B R 4097 033 080 5
12A R 4125 046 112 5
12B R 4257 039 092 5
15 R 3957 052 131 5
22A R 4046 028 069 5
22B R 4015 045 112 5
23 R 3830 073 192 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1477
Table 13 Intense smoking regime Water mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1237 038 305 5
2B L 999 037 375 5
6B L 906 034 381 5
9A L 1147 043 373 5
10 L 1152 052 453 5
11 L 1488 053 356 5
12C L 1061 019 179 5
17 L 1027 028 274 5
19 L 1095 038 348 5
20 L 1216 083 681 5
21 L 1285 026 206 5
24 L 1235 060 484 5
25 L 1004 031 307 5
1A R 1024 014 138 5
2A R 797 016 197 5
3 R 974 031 317 5
4A R 911 034 368 5
4B R 931 027 287 5
5B R 815 041 507 5
6A R 923 038 411 5
8 R 929 033 354 5
9B R 927 028 301 5
12A R 1004 051 508 5
12B R 935 017 181 5
15 R 823 029 349 5
22A R 953 005 052 5
22B R 926 038 410 5
23 R 1598 065 404 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1577
Table 14 Intense smoking regime Nicotine mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 3484 0055 158 5
2B L 3434 0048 141 5
6B L 3342 0051 153 5
9A L 3494 0089 255 5
10 L 3578 0226 633 5
11 L 3620 0082 225 5
12C L 3402 0024 070 5
17 L 3622 0075 208 5
19 L 3520 0012 035 5
20 L 3552 0230 647 5
21 L 3712 0030 082 5
24 L 3524 0061 174 5
25 L 2986 0052 173 5
1A R 3385 0020 060 5
2A R 3317 0030 090 5
3 R 3479 0023 067 5
4A R 3369 0037 109 5
4B R 3340 0053 160 5
5B R 1677 0025 148 5
6A R 3390 0066 195 5
8 R 2967 0044 149 5
9B R 3410 0048 142 5
12A R 3452 0030 085 5
12B R 3520 0068 192 5
15 R 3333 0099 296 5
22A R 3222 0051 159 5
22B R 3210 0049 151 5
23 R 6610 0108 163 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1677
Table 15 Intense smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2965 054 183 5
2B L 3048 092 301 5
6B L 2696 035 131 5
9A L 2975 038 129 5
10 L 3157 047 148 5
11 L 3218 082 255 5
12C L 3243 015 047 5
17 L 3157 079 250 5
19 L 3119 084 268 5
20 L 3045 056 185 5
21 L 3351 066 198 5
24 L 3195 050 158 5
25 L 3132 054 174 5
1A R 2806 018 065 5
2A R 2885 012 043 5
3 R 2925 040 135 5
4A R 2849 021 074 5
4B R 2917 035 119 5
5B R 3013 023 077 5
6A R 2811 036 129 5
8 R 2819 021 074 5
9B R 2832 032 115 5
12A R 2776 048 171 5
12B R 2970 026 086 5
15 R 2800 035 124 5
22A R 2770 025 091 5
22B R 2768 049 178 5
23 R 1570 060 384 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1777
Table 16 Intense smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2478 034 137 5
2B L 2472 027 111 5
6B L 2367 039 165 5
9A L 2423 065 270 5
10 L 2373 018 077 5
11 L 2568 029 114 5
12C L 2497 028 113 5
17 L 2321 032 139 5
19 L 2488 022 086 5
20 L 2489 056 227 5
21 L 2523 045 177 5
24 L 2470 052 211 5
25 L 2399 089 369 5
1A R 2505 033 131 5
2A R 2485 037 149 5
3 R 2605 031 119 5
4A R 2513 031 125 5
4B R 2542 047 185 5
5B R 2480 022 088 5
6A R 2570 024 092 5
8 R 2532 047 185 5
9B R 2457 044 181 5
12A R 2506 023 093 5
12B R 2523 018 069 5
15 R 2547 039 154 5
22A R 2470 034 138 5
22B R 2466 032 130 5
23 R 2508 030 119 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1877
Table 17 Intense smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 1138 022 191 5
2B L 1154 019 162 5
6B L 1170 008 068 5
9A L 1095 013 114 5
10 L 1138 023 199 5
11 L 1127 016 138 5
12C L 1115 022 199 5
17 L 1110 009 079 5
19 L 1059 011 101 5
20 L 1087 019 176 5
21 L 1121 019 169 5
24 L 1106 027 248 5
25 L 1102 012 105 5
1A R 1111 018 159 5
2A R 1059 014 130 5
3 R 1152 013 110 5
4A R 1078 008 070 5
4B R 1105 016 143 5
5B R 1134 030 267 5
6A R 1136 004 034 5
8 R 1075 015 142 5
9B R 1077 006 054 5
12A R 1102 020 186 5
12B R 1097 016 148 5
15 R 1084 010 091 5
22A R 1112 016 147 5
22B R 1106 014 122 5
23 R 1066 009 088 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1977
Statistical Analysis 4
Exclusion of outliers 41
411 Numerical outlier technique Cochran amp Grubbs test
The statistical evaluation of data for this collaborative study followed the methods provided
by ISO 5725-21 For outlier testing the Grubbs and Cochran methods were used
ISO 5725-2 Tests Consistency
Cochranrsquos ndash test Within-laboratory variability Suitable for detecting whether the highest value in a set of laboratory standard deviations is an outlier or not
Grubbsrsquo ndash test Between-laboratory variability Suitable for detecting whether the highest (or lowest) laboratories averages are outliers or not
The protocol ldquoHarmonized statistical procedurerdquo defined by IUPAC (International Union of
Pure and Applied Chemistry) has been applied as well It consists of sequential applications of
the Cochran and Grubbs tests until no further outliers are detected or until a drop of more than
222 (for this study =29) in the original number of laboratories would occur (see flowchart
in Appendix F)
First apply the Cochran outlier test and if an outlying laboratory is identified then a single
value Grubbs test is performed on the individual values of this outlying laboratory (Individual
Grubbs) If no individual value is identified as outlier the outlying laboratory is removed
When an individual value is identified as an outlier only this value is removed
Afterwards single-value Grubbs test is applied and outlying laboratories are removed If no
laboratory is identified as outlier the pair-value test is applied (two values at the same end)
Remove any laboratory(ies) flagged by these tests but stop removal if more than 222 (2 of
9 laboratories) would be removed
The test was performed with both linear and rotary smoking machines together but also with
rotary respectively linear smoking machines separately The results provided in the report for
all smoking machines respectively with linear or rotary only smoking machines are obtained
after exclusion of the outliers for those respective categories
Note
The paired value Grubbsrsquo test is an extension of the single value Grubbs test for pairs of
outliers The use is advised in ISO 5725 to detect pairs of outlier undetectable sequentially by
using single value Grubbs test
The outlying laboratories are provided in the Tables 18 to 23
Repeatability and reproducibility estimation 42
Repeatability and reproducibility limits are calculated for both smoking regimes each
parameter and for both smoking machine types The results are summarized in tables 18 to 23
with all machines grouped respectively with linear or rotary machines only both with ISO
and intense smoking regimes Outlying laboratories are provided in the same tables The
corresponding graphs named ldquoindividual valuesrdquo are given in Part 5 of this report
1 ISO 5725-21994 Accuracy (trueness and precision) of measurement methods and results ndash Part 2 Basic
method for the determination of repeatability and reproducibility of a standard measurement method
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 2077
Table 18 r amp R estimations for CM8 under ISO smoking regime (all machines)
p n Global Mean Sr CVr[] r SR CVR [] R C GG2 Stragglers Parameter
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1377
Table 12 Intense smoking regime TPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 4551 091 200 5
2B L 4391 078 178 5
6B L 3936 067 170 5
9A L 4471 060 134 5
10 L 4667 073 157 5
11 L 5068 136 269 5
12C L 4644 031 066 5
17 L 4346 106 243 5
19 L 4566 087 190 5
20 L 4616 122 265 5
21 L 5008 077 153 5
24 L 4782 094 196 5
25 L 4434 081 182 5
1A R 4168 016 039 5
2A R 4014 024 061 5
3 R 4247 035 083 5
4A R 4097 039 095 5
4B R 4181 064 153 5
5B R 3997 040 101 5
6A R 4076 074 181 5
8 R 4044 043 107 5
9B R 4097 033 080 5
12A R 4125 046 112 5
12B R 4257 039 092 5
15 R 3957 052 131 5
22A R 4046 028 069 5
22B R 4015 045 112 5
23 R 3830 073 192 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1477
Table 13 Intense smoking regime Water mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1237 038 305 5
2B L 999 037 375 5
6B L 906 034 381 5
9A L 1147 043 373 5
10 L 1152 052 453 5
11 L 1488 053 356 5
12C L 1061 019 179 5
17 L 1027 028 274 5
19 L 1095 038 348 5
20 L 1216 083 681 5
21 L 1285 026 206 5
24 L 1235 060 484 5
25 L 1004 031 307 5
1A R 1024 014 138 5
2A R 797 016 197 5
3 R 974 031 317 5
4A R 911 034 368 5
4B R 931 027 287 5
5B R 815 041 507 5
6A R 923 038 411 5
8 R 929 033 354 5
9B R 927 028 301 5
12A R 1004 051 508 5
12B R 935 017 181 5
15 R 823 029 349 5
22A R 953 005 052 5
22B R 926 038 410 5
23 R 1598 065 404 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1577
Table 14 Intense smoking regime Nicotine mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 3484 0055 158 5
2B L 3434 0048 141 5
6B L 3342 0051 153 5
9A L 3494 0089 255 5
10 L 3578 0226 633 5
11 L 3620 0082 225 5
12C L 3402 0024 070 5
17 L 3622 0075 208 5
19 L 3520 0012 035 5
20 L 3552 0230 647 5
21 L 3712 0030 082 5
24 L 3524 0061 174 5
25 L 2986 0052 173 5
1A R 3385 0020 060 5
2A R 3317 0030 090 5
3 R 3479 0023 067 5
4A R 3369 0037 109 5
4B R 3340 0053 160 5
5B R 1677 0025 148 5
6A R 3390 0066 195 5
8 R 2967 0044 149 5
9B R 3410 0048 142 5
12A R 3452 0030 085 5
12B R 3520 0068 192 5
15 R 3333 0099 296 5
22A R 3222 0051 159 5
22B R 3210 0049 151 5
23 R 6610 0108 163 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1677
Table 15 Intense smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2965 054 183 5
2B L 3048 092 301 5
6B L 2696 035 131 5
9A L 2975 038 129 5
10 L 3157 047 148 5
11 L 3218 082 255 5
12C L 3243 015 047 5
17 L 3157 079 250 5
19 L 3119 084 268 5
20 L 3045 056 185 5
21 L 3351 066 198 5
24 L 3195 050 158 5
25 L 3132 054 174 5
1A R 2806 018 065 5
2A R 2885 012 043 5
3 R 2925 040 135 5
4A R 2849 021 074 5
4B R 2917 035 119 5
5B R 3013 023 077 5
6A R 2811 036 129 5
8 R 2819 021 074 5
9B R 2832 032 115 5
12A R 2776 048 171 5
12B R 2970 026 086 5
15 R 2800 035 124 5
22A R 2770 025 091 5
22B R 2768 049 178 5
23 R 1570 060 384 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1777
Table 16 Intense smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2478 034 137 5
2B L 2472 027 111 5
6B L 2367 039 165 5
9A L 2423 065 270 5
10 L 2373 018 077 5
11 L 2568 029 114 5
12C L 2497 028 113 5
17 L 2321 032 139 5
19 L 2488 022 086 5
20 L 2489 056 227 5
21 L 2523 045 177 5
24 L 2470 052 211 5
25 L 2399 089 369 5
1A R 2505 033 131 5
2A R 2485 037 149 5
3 R 2605 031 119 5
4A R 2513 031 125 5
4B R 2542 047 185 5
5B R 2480 022 088 5
6A R 2570 024 092 5
8 R 2532 047 185 5
9B R 2457 044 181 5
12A R 2506 023 093 5
12B R 2523 018 069 5
15 R 2547 039 154 5
22A R 2470 034 138 5
22B R 2466 032 130 5
23 R 2508 030 119 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1877
Table 17 Intense smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 1138 022 191 5
2B L 1154 019 162 5
6B L 1170 008 068 5
9A L 1095 013 114 5
10 L 1138 023 199 5
11 L 1127 016 138 5
12C L 1115 022 199 5
17 L 1110 009 079 5
19 L 1059 011 101 5
20 L 1087 019 176 5
21 L 1121 019 169 5
24 L 1106 027 248 5
25 L 1102 012 105 5
1A R 1111 018 159 5
2A R 1059 014 130 5
3 R 1152 013 110 5
4A R 1078 008 070 5
4B R 1105 016 143 5
5B R 1134 030 267 5
6A R 1136 004 034 5
8 R 1075 015 142 5
9B R 1077 006 054 5
12A R 1102 020 186 5
12B R 1097 016 148 5
15 R 1084 010 091 5
22A R 1112 016 147 5
22B R 1106 014 122 5
23 R 1066 009 088 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1977
Statistical Analysis 4
Exclusion of outliers 41
411 Numerical outlier technique Cochran amp Grubbs test
The statistical evaluation of data for this collaborative study followed the methods provided
by ISO 5725-21 For outlier testing the Grubbs and Cochran methods were used
ISO 5725-2 Tests Consistency
Cochranrsquos ndash test Within-laboratory variability Suitable for detecting whether the highest value in a set of laboratory standard deviations is an outlier or not
Grubbsrsquo ndash test Between-laboratory variability Suitable for detecting whether the highest (or lowest) laboratories averages are outliers or not
The protocol ldquoHarmonized statistical procedurerdquo defined by IUPAC (International Union of
Pure and Applied Chemistry) has been applied as well It consists of sequential applications of
the Cochran and Grubbs tests until no further outliers are detected or until a drop of more than
222 (for this study =29) in the original number of laboratories would occur (see flowchart
in Appendix F)
First apply the Cochran outlier test and if an outlying laboratory is identified then a single
value Grubbs test is performed on the individual values of this outlying laboratory (Individual
Grubbs) If no individual value is identified as outlier the outlying laboratory is removed
When an individual value is identified as an outlier only this value is removed
Afterwards single-value Grubbs test is applied and outlying laboratories are removed If no
laboratory is identified as outlier the pair-value test is applied (two values at the same end)
Remove any laboratory(ies) flagged by these tests but stop removal if more than 222 (2 of
9 laboratories) would be removed
The test was performed with both linear and rotary smoking machines together but also with
rotary respectively linear smoking machines separately The results provided in the report for
all smoking machines respectively with linear or rotary only smoking machines are obtained
after exclusion of the outliers for those respective categories
Note
The paired value Grubbsrsquo test is an extension of the single value Grubbs test for pairs of
outliers The use is advised in ISO 5725 to detect pairs of outlier undetectable sequentially by
using single value Grubbs test
The outlying laboratories are provided in the Tables 18 to 23
Repeatability and reproducibility estimation 42
Repeatability and reproducibility limits are calculated for both smoking regimes each
parameter and for both smoking machine types The results are summarized in tables 18 to 23
with all machines grouped respectively with linear or rotary machines only both with ISO
and intense smoking regimes Outlying laboratories are provided in the same tables The
corresponding graphs named ldquoindividual valuesrdquo are given in Part 5 of this report
1 ISO 5725-21994 Accuracy (trueness and precision) of measurement methods and results ndash Part 2 Basic
method for the determination of repeatability and reproducibility of a standard measurement method
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 2077
Table 18 r amp R estimations for CM8 under ISO smoking regime (all machines)
p n Global Mean Sr CVr[] r SR CVR [] R C GG2 Stragglers Parameter
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1477
Table 13 Intense smoking regime Water mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 1237 038 305 5
2B L 999 037 375 5
6B L 906 034 381 5
9A L 1147 043 373 5
10 L 1152 052 453 5
11 L 1488 053 356 5
12C L 1061 019 179 5
17 L 1027 028 274 5
19 L 1095 038 348 5
20 L 1216 083 681 5
21 L 1285 026 206 5
24 L 1235 060 484 5
25 L 1004 031 307 5
1A R 1024 014 138 5
2A R 797 016 197 5
3 R 974 031 317 5
4A R 911 034 368 5
4B R 931 027 287 5
5B R 815 041 507 5
6A R 923 038 411 5
8 R 929 033 354 5
9B R 927 028 301 5
12A R 1004 051 508 5
12B R 935 017 181 5
15 R 823 029 349 5
22A R 953 005 052 5
22B R 926 038 410 5
23 R 1598 065 404 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1577
Table 14 Intense smoking regime Nicotine mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 3484 0055 158 5
2B L 3434 0048 141 5
6B L 3342 0051 153 5
9A L 3494 0089 255 5
10 L 3578 0226 633 5
11 L 3620 0082 225 5
12C L 3402 0024 070 5
17 L 3622 0075 208 5
19 L 3520 0012 035 5
20 L 3552 0230 647 5
21 L 3712 0030 082 5
24 L 3524 0061 174 5
25 L 2986 0052 173 5
1A R 3385 0020 060 5
2A R 3317 0030 090 5
3 R 3479 0023 067 5
4A R 3369 0037 109 5
4B R 3340 0053 160 5
5B R 1677 0025 148 5
6A R 3390 0066 195 5
8 R 2967 0044 149 5
9B R 3410 0048 142 5
12A R 3452 0030 085 5
12B R 3520 0068 192 5
15 R 3333 0099 296 5
22A R 3222 0051 159 5
22B R 3210 0049 151 5
23 R 6610 0108 163 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1677
Table 15 Intense smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2965 054 183 5
2B L 3048 092 301 5
6B L 2696 035 131 5
9A L 2975 038 129 5
10 L 3157 047 148 5
11 L 3218 082 255 5
12C L 3243 015 047 5
17 L 3157 079 250 5
19 L 3119 084 268 5
20 L 3045 056 185 5
21 L 3351 066 198 5
24 L 3195 050 158 5
25 L 3132 054 174 5
1A R 2806 018 065 5
2A R 2885 012 043 5
3 R 2925 040 135 5
4A R 2849 021 074 5
4B R 2917 035 119 5
5B R 3013 023 077 5
6A R 2811 036 129 5
8 R 2819 021 074 5
9B R 2832 032 115 5
12A R 2776 048 171 5
12B R 2970 026 086 5
15 R 2800 035 124 5
22A R 2770 025 091 5
22B R 2768 049 178 5
23 R 1570 060 384 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1777
Table 16 Intense smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2478 034 137 5
2B L 2472 027 111 5
6B L 2367 039 165 5
9A L 2423 065 270 5
10 L 2373 018 077 5
11 L 2568 029 114 5
12C L 2497 028 113 5
17 L 2321 032 139 5
19 L 2488 022 086 5
20 L 2489 056 227 5
21 L 2523 045 177 5
24 L 2470 052 211 5
25 L 2399 089 369 5
1A R 2505 033 131 5
2A R 2485 037 149 5
3 R 2605 031 119 5
4A R 2513 031 125 5
4B R 2542 047 185 5
5B R 2480 022 088 5
6A R 2570 024 092 5
8 R 2532 047 185 5
9B R 2457 044 181 5
12A R 2506 023 093 5
12B R 2523 018 069 5
15 R 2547 039 154 5
22A R 2470 034 138 5
22B R 2466 032 130 5
23 R 2508 030 119 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1877
Table 17 Intense smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 1138 022 191 5
2B L 1154 019 162 5
6B L 1170 008 068 5
9A L 1095 013 114 5
10 L 1138 023 199 5
11 L 1127 016 138 5
12C L 1115 022 199 5
17 L 1110 009 079 5
19 L 1059 011 101 5
20 L 1087 019 176 5
21 L 1121 019 169 5
24 L 1106 027 248 5
25 L 1102 012 105 5
1A R 1111 018 159 5
2A R 1059 014 130 5
3 R 1152 013 110 5
4A R 1078 008 070 5
4B R 1105 016 143 5
5B R 1134 030 267 5
6A R 1136 004 034 5
8 R 1075 015 142 5
9B R 1077 006 054 5
12A R 1102 020 186 5
12B R 1097 016 148 5
15 R 1084 010 091 5
22A R 1112 016 147 5
22B R 1106 014 122 5
23 R 1066 009 088 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1977
Statistical Analysis 4
Exclusion of outliers 41
411 Numerical outlier technique Cochran amp Grubbs test
The statistical evaluation of data for this collaborative study followed the methods provided
by ISO 5725-21 For outlier testing the Grubbs and Cochran methods were used
ISO 5725-2 Tests Consistency
Cochranrsquos ndash test Within-laboratory variability Suitable for detecting whether the highest value in a set of laboratory standard deviations is an outlier or not
Grubbsrsquo ndash test Between-laboratory variability Suitable for detecting whether the highest (or lowest) laboratories averages are outliers or not
The protocol ldquoHarmonized statistical procedurerdquo defined by IUPAC (International Union of
Pure and Applied Chemistry) has been applied as well It consists of sequential applications of
the Cochran and Grubbs tests until no further outliers are detected or until a drop of more than
222 (for this study =29) in the original number of laboratories would occur (see flowchart
in Appendix F)
First apply the Cochran outlier test and if an outlying laboratory is identified then a single
value Grubbs test is performed on the individual values of this outlying laboratory (Individual
Grubbs) If no individual value is identified as outlier the outlying laboratory is removed
When an individual value is identified as an outlier only this value is removed
Afterwards single-value Grubbs test is applied and outlying laboratories are removed If no
laboratory is identified as outlier the pair-value test is applied (two values at the same end)
Remove any laboratory(ies) flagged by these tests but stop removal if more than 222 (2 of
9 laboratories) would be removed
The test was performed with both linear and rotary smoking machines together but also with
rotary respectively linear smoking machines separately The results provided in the report for
all smoking machines respectively with linear or rotary only smoking machines are obtained
after exclusion of the outliers for those respective categories
Note
The paired value Grubbsrsquo test is an extension of the single value Grubbs test for pairs of
outliers The use is advised in ISO 5725 to detect pairs of outlier undetectable sequentially by
using single value Grubbs test
The outlying laboratories are provided in the Tables 18 to 23
Repeatability and reproducibility estimation 42
Repeatability and reproducibility limits are calculated for both smoking regimes each
parameter and for both smoking machine types The results are summarized in tables 18 to 23
with all machines grouped respectively with linear or rotary machines only both with ISO
and intense smoking regimes Outlying laboratories are provided in the same tables The
corresponding graphs named ldquoindividual valuesrdquo are given in Part 5 of this report
1 ISO 5725-21994 Accuracy (trueness and precision) of measurement methods and results ndash Part 2 Basic
method for the determination of repeatability and reproducibility of a standard measurement method
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 2077
Table 18 r amp R estimations for CM8 under ISO smoking regime (all machines)
p n Global Mean Sr CVr[] r SR CVR [] R C GG2 Stragglers Parameter
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1577
Table 14 Intense smoking regime Nicotine mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 3484 0055 158 5
2B L 3434 0048 141 5
6B L 3342 0051 153 5
9A L 3494 0089 255 5
10 L 3578 0226 633 5
11 L 3620 0082 225 5
12C L 3402 0024 070 5
17 L 3622 0075 208 5
19 L 3520 0012 035 5
20 L 3552 0230 647 5
21 L 3712 0030 082 5
24 L 3524 0061 174 5
25 L 2986 0052 173 5
1A R 3385 0020 060 5
2A R 3317 0030 090 5
3 R 3479 0023 067 5
4A R 3369 0037 109 5
4B R 3340 0053 160 5
5B R 1677 0025 148 5
6A R 3390 0066 195 5
8 R 2967 0044 149 5
9B R 3410 0048 142 5
12A R 3452 0030 085 5
12B R 3520 0068 192 5
15 R 3333 0099 296 5
22A R 3222 0051 159 5
22B R 3210 0049 151 5
23 R 6610 0108 163 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1677
Table 15 Intense smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2965 054 183 5
2B L 3048 092 301 5
6B L 2696 035 131 5
9A L 2975 038 129 5
10 L 3157 047 148 5
11 L 3218 082 255 5
12C L 3243 015 047 5
17 L 3157 079 250 5
19 L 3119 084 268 5
20 L 3045 056 185 5
21 L 3351 066 198 5
24 L 3195 050 158 5
25 L 3132 054 174 5
1A R 2806 018 065 5
2A R 2885 012 043 5
3 R 2925 040 135 5
4A R 2849 021 074 5
4B R 2917 035 119 5
5B R 3013 023 077 5
6A R 2811 036 129 5
8 R 2819 021 074 5
9B R 2832 032 115 5
12A R 2776 048 171 5
12B R 2970 026 086 5
15 R 2800 035 124 5
22A R 2770 025 091 5
22B R 2768 049 178 5
23 R 1570 060 384 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1777
Table 16 Intense smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2478 034 137 5
2B L 2472 027 111 5
6B L 2367 039 165 5
9A L 2423 065 270 5
10 L 2373 018 077 5
11 L 2568 029 114 5
12C L 2497 028 113 5
17 L 2321 032 139 5
19 L 2488 022 086 5
20 L 2489 056 227 5
21 L 2523 045 177 5
24 L 2470 052 211 5
25 L 2399 089 369 5
1A R 2505 033 131 5
2A R 2485 037 149 5
3 R 2605 031 119 5
4A R 2513 031 125 5
4B R 2542 047 185 5
5B R 2480 022 088 5
6A R 2570 024 092 5
8 R 2532 047 185 5
9B R 2457 044 181 5
12A R 2506 023 093 5
12B R 2523 018 069 5
15 R 2547 039 154 5
22A R 2470 034 138 5
22B R 2466 032 130 5
23 R 2508 030 119 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1877
Table 17 Intense smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 1138 022 191 5
2B L 1154 019 162 5
6B L 1170 008 068 5
9A L 1095 013 114 5
10 L 1138 023 199 5
11 L 1127 016 138 5
12C L 1115 022 199 5
17 L 1110 009 079 5
19 L 1059 011 101 5
20 L 1087 019 176 5
21 L 1121 019 169 5
24 L 1106 027 248 5
25 L 1102 012 105 5
1A R 1111 018 159 5
2A R 1059 014 130 5
3 R 1152 013 110 5
4A R 1078 008 070 5
4B R 1105 016 143 5
5B R 1134 030 267 5
6A R 1136 004 034 5
8 R 1075 015 142 5
9B R 1077 006 054 5
12A R 1102 020 186 5
12B R 1097 016 148 5
15 R 1084 010 091 5
22A R 1112 016 147 5
22B R 1106 014 122 5
23 R 1066 009 088 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1977
Statistical Analysis 4
Exclusion of outliers 41
411 Numerical outlier technique Cochran amp Grubbs test
The statistical evaluation of data for this collaborative study followed the methods provided
by ISO 5725-21 For outlier testing the Grubbs and Cochran methods were used
ISO 5725-2 Tests Consistency
Cochranrsquos ndash test Within-laboratory variability Suitable for detecting whether the highest value in a set of laboratory standard deviations is an outlier or not
Grubbsrsquo ndash test Between-laboratory variability Suitable for detecting whether the highest (or lowest) laboratories averages are outliers or not
The protocol ldquoHarmonized statistical procedurerdquo defined by IUPAC (International Union of
Pure and Applied Chemistry) has been applied as well It consists of sequential applications of
the Cochran and Grubbs tests until no further outliers are detected or until a drop of more than
222 (for this study =29) in the original number of laboratories would occur (see flowchart
in Appendix F)
First apply the Cochran outlier test and if an outlying laboratory is identified then a single
value Grubbs test is performed on the individual values of this outlying laboratory (Individual
Grubbs) If no individual value is identified as outlier the outlying laboratory is removed
When an individual value is identified as an outlier only this value is removed
Afterwards single-value Grubbs test is applied and outlying laboratories are removed If no
laboratory is identified as outlier the pair-value test is applied (two values at the same end)
Remove any laboratory(ies) flagged by these tests but stop removal if more than 222 (2 of
9 laboratories) would be removed
The test was performed with both linear and rotary smoking machines together but also with
rotary respectively linear smoking machines separately The results provided in the report for
all smoking machines respectively with linear or rotary only smoking machines are obtained
after exclusion of the outliers for those respective categories
Note
The paired value Grubbsrsquo test is an extension of the single value Grubbs test for pairs of
outliers The use is advised in ISO 5725 to detect pairs of outlier undetectable sequentially by
using single value Grubbs test
The outlying laboratories are provided in the Tables 18 to 23
Repeatability and reproducibility estimation 42
Repeatability and reproducibility limits are calculated for both smoking regimes each
parameter and for both smoking machine types The results are summarized in tables 18 to 23
with all machines grouped respectively with linear or rotary machines only both with ISO
and intense smoking regimes Outlying laboratories are provided in the same tables The
corresponding graphs named ldquoindividual valuesrdquo are given in Part 5 of this report
1 ISO 5725-21994 Accuracy (trueness and precision) of measurement methods and results ndash Part 2 Basic
method for the determination of repeatability and reproducibility of a standard measurement method
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 2077
Table 18 r amp R estimations for CM8 under ISO smoking regime (all machines)
p n Global Mean Sr CVr[] r SR CVR [] R C GG2 Stragglers Parameter
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1677
Table 15 Intense smoking regime NFDPM mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2965 054 183 5
2B L 3048 092 301 5
6B L 2696 035 131 5
9A L 2975 038 129 5
10 L 3157 047 148 5
11 L 3218 082 255 5
12C L 3243 015 047 5
17 L 3157 079 250 5
19 L 3119 084 268 5
20 L 3045 056 185 5
21 L 3351 066 198 5
24 L 3195 050 158 5
25 L 3132 054 174 5
1A R 2806 018 065 5
2A R 2885 012 043 5
3 R 2925 040 135 5
4A R 2849 021 074 5
4B R 2917 035 119 5
5B R 3013 023 077 5
6A R 2811 036 129 5
8 R 2819 021 074 5
9B R 2832 032 115 5
12A R 2776 048 171 5
12B R 2970 026 086 5
15 R 2800 035 124 5
22A R 2770 025 091 5
22B R 2768 049 178 5
23 R 1570 060 384 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1777
Table 16 Intense smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2478 034 137 5
2B L 2472 027 111 5
6B L 2367 039 165 5
9A L 2423 065 270 5
10 L 2373 018 077 5
11 L 2568 029 114 5
12C L 2497 028 113 5
17 L 2321 032 139 5
19 L 2488 022 086 5
20 L 2489 056 227 5
21 L 2523 045 177 5
24 L 2470 052 211 5
25 L 2399 089 369 5
1A R 2505 033 131 5
2A R 2485 037 149 5
3 R 2605 031 119 5
4A R 2513 031 125 5
4B R 2542 047 185 5
5B R 2480 022 088 5
6A R 2570 024 092 5
8 R 2532 047 185 5
9B R 2457 044 181 5
12A R 2506 023 093 5
12B R 2523 018 069 5
15 R 2547 039 154 5
22A R 2470 034 138 5
22B R 2466 032 130 5
23 R 2508 030 119 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1877
Table 17 Intense smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 1138 022 191 5
2B L 1154 019 162 5
6B L 1170 008 068 5
9A L 1095 013 114 5
10 L 1138 023 199 5
11 L 1127 016 138 5
12C L 1115 022 199 5
17 L 1110 009 079 5
19 L 1059 011 101 5
20 L 1087 019 176 5
21 L 1121 019 169 5
24 L 1106 027 248 5
25 L 1102 012 105 5
1A R 1111 018 159 5
2A R 1059 014 130 5
3 R 1152 013 110 5
4A R 1078 008 070 5
4B R 1105 016 143 5
5B R 1134 030 267 5
6A R 1136 004 034 5
8 R 1075 015 142 5
9B R 1077 006 054 5
12A R 1102 020 186 5
12B R 1097 016 148 5
15 R 1084 010 091 5
22A R 1112 016 147 5
22B R 1106 014 122 5
23 R 1066 009 088 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1977
Statistical Analysis 4
Exclusion of outliers 41
411 Numerical outlier technique Cochran amp Grubbs test
The statistical evaluation of data for this collaborative study followed the methods provided
by ISO 5725-21 For outlier testing the Grubbs and Cochran methods were used
ISO 5725-2 Tests Consistency
Cochranrsquos ndash test Within-laboratory variability Suitable for detecting whether the highest value in a set of laboratory standard deviations is an outlier or not
Grubbsrsquo ndash test Between-laboratory variability Suitable for detecting whether the highest (or lowest) laboratories averages are outliers or not
The protocol ldquoHarmonized statistical procedurerdquo defined by IUPAC (International Union of
Pure and Applied Chemistry) has been applied as well It consists of sequential applications of
the Cochran and Grubbs tests until no further outliers are detected or until a drop of more than
222 (for this study =29) in the original number of laboratories would occur (see flowchart
in Appendix F)
First apply the Cochran outlier test and if an outlying laboratory is identified then a single
value Grubbs test is performed on the individual values of this outlying laboratory (Individual
Grubbs) If no individual value is identified as outlier the outlying laboratory is removed
When an individual value is identified as an outlier only this value is removed
Afterwards single-value Grubbs test is applied and outlying laboratories are removed If no
laboratory is identified as outlier the pair-value test is applied (two values at the same end)
Remove any laboratory(ies) flagged by these tests but stop removal if more than 222 (2 of
9 laboratories) would be removed
The test was performed with both linear and rotary smoking machines together but also with
rotary respectively linear smoking machines separately The results provided in the report for
all smoking machines respectively with linear or rotary only smoking machines are obtained
after exclusion of the outliers for those respective categories
Note
The paired value Grubbsrsquo test is an extension of the single value Grubbs test for pairs of
outliers The use is advised in ISO 5725 to detect pairs of outlier undetectable sequentially by
using single value Grubbs test
The outlying laboratories are provided in the Tables 18 to 23
Repeatability and reproducibility estimation 42
Repeatability and reproducibility limits are calculated for both smoking regimes each
parameter and for both smoking machine types The results are summarized in tables 18 to 23
with all machines grouped respectively with linear or rotary machines only both with ISO
and intense smoking regimes Outlying laboratories are provided in the same tables The
corresponding graphs named ldquoindividual valuesrdquo are given in Part 5 of this report
1 ISO 5725-21994 Accuracy (trueness and precision) of measurement methods and results ndash Part 2 Basic
method for the determination of repeatability and reproducibility of a standard measurement method
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 2077
Table 18 r amp R estimations for CM8 under ISO smoking regime (all machines)
p n Global Mean Sr CVr[] r SR CVR [] R C GG2 Stragglers Parameter
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1777
Table 16 Intense smoking regime CO mean and standard deviation per laboratory code
Lab Code Machine Type Mean (mgtp) SD CV [] Sample size
1B L 2478 034 137 5
2B L 2472 027 111 5
6B L 2367 039 165 5
9A L 2423 065 270 5
10 L 2373 018 077 5
11 L 2568 029 114 5
12C L 2497 028 113 5
17 L 2321 032 139 5
19 L 2488 022 086 5
20 L 2489 056 227 5
21 L 2523 045 177 5
24 L 2470 052 211 5
25 L 2399 089 369 5
1A R 2505 033 131 5
2A R 2485 037 149 5
3 R 2605 031 119 5
4A R 2513 031 125 5
4B R 2542 047 185 5
5B R 2480 022 088 5
6A R 2570 024 092 5
8 R 2532 047 185 5
9B R 2457 044 181 5
12A R 2506 023 093 5
12B R 2523 018 069 5
15 R 2547 039 154 5
22A R 2470 034 138 5
22B R 2466 032 130 5
23 R 2508 030 119 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1877
Table 17 Intense smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 1138 022 191 5
2B L 1154 019 162 5
6B L 1170 008 068 5
9A L 1095 013 114 5
10 L 1138 023 199 5
11 L 1127 016 138 5
12C L 1115 022 199 5
17 L 1110 009 079 5
19 L 1059 011 101 5
20 L 1087 019 176 5
21 L 1121 019 169 5
24 L 1106 027 248 5
25 L 1102 012 105 5
1A R 1111 018 159 5
2A R 1059 014 130 5
3 R 1152 013 110 5
4A R 1078 008 070 5
4B R 1105 016 143 5
5B R 1134 030 267 5
6A R 1136 004 034 5
8 R 1075 015 142 5
9B R 1077 006 054 5
12A R 1102 020 186 5
12B R 1097 016 148 5
15 R 1084 010 091 5
22A R 1112 016 147 5
22B R 1106 014 122 5
23 R 1066 009 088 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1977
Statistical Analysis 4
Exclusion of outliers 41
411 Numerical outlier technique Cochran amp Grubbs test
The statistical evaluation of data for this collaborative study followed the methods provided
by ISO 5725-21 For outlier testing the Grubbs and Cochran methods were used
ISO 5725-2 Tests Consistency
Cochranrsquos ndash test Within-laboratory variability Suitable for detecting whether the highest value in a set of laboratory standard deviations is an outlier or not
Grubbsrsquo ndash test Between-laboratory variability Suitable for detecting whether the highest (or lowest) laboratories averages are outliers or not
The protocol ldquoHarmonized statistical procedurerdquo defined by IUPAC (International Union of
Pure and Applied Chemistry) has been applied as well It consists of sequential applications of
the Cochran and Grubbs tests until no further outliers are detected or until a drop of more than
222 (for this study =29) in the original number of laboratories would occur (see flowchart
in Appendix F)
First apply the Cochran outlier test and if an outlying laboratory is identified then a single
value Grubbs test is performed on the individual values of this outlying laboratory (Individual
Grubbs) If no individual value is identified as outlier the outlying laboratory is removed
When an individual value is identified as an outlier only this value is removed
Afterwards single-value Grubbs test is applied and outlying laboratories are removed If no
laboratory is identified as outlier the pair-value test is applied (two values at the same end)
Remove any laboratory(ies) flagged by these tests but stop removal if more than 222 (2 of
9 laboratories) would be removed
The test was performed with both linear and rotary smoking machines together but also with
rotary respectively linear smoking machines separately The results provided in the report for
all smoking machines respectively with linear or rotary only smoking machines are obtained
after exclusion of the outliers for those respective categories
Note
The paired value Grubbsrsquo test is an extension of the single value Grubbs test for pairs of
outliers The use is advised in ISO 5725 to detect pairs of outlier undetectable sequentially by
using single value Grubbs test
The outlying laboratories are provided in the Tables 18 to 23
Repeatability and reproducibility estimation 42
Repeatability and reproducibility limits are calculated for both smoking regimes each
parameter and for both smoking machine types The results are summarized in tables 18 to 23
with all machines grouped respectively with linear or rotary machines only both with ISO
and intense smoking regimes Outlying laboratories are provided in the same tables The
corresponding graphs named ldquoindividual valuesrdquo are given in Part 5 of this report
1 ISO 5725-21994 Accuracy (trueness and precision) of measurement methods and results ndash Part 2 Basic
method for the determination of repeatability and reproducibility of a standard measurement method
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 2077
Table 18 r amp R estimations for CM8 under ISO smoking regime (all machines)
p n Global Mean Sr CVr[] r SR CVR [] R C GG2 Stragglers Parameter
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1877
Table 17 Intense smoking regime Puff count mean and standard deviation per laboratory code
Lab Code Machine Type Mean (pufftp) SD CV [] Sample size
1B L 1138 022 191 5
2B L 1154 019 162 5
6B L 1170 008 068 5
9A L 1095 013 114 5
10 L 1138 023 199 5
11 L 1127 016 138 5
12C L 1115 022 199 5
17 L 1110 009 079 5
19 L 1059 011 101 5
20 L 1087 019 176 5
21 L 1121 019 169 5
24 L 1106 027 248 5
25 L 1102 012 105 5
1A R 1111 018 159 5
2A R 1059 014 130 5
3 R 1152 013 110 5
4A R 1078 008 070 5
4B R 1105 016 143 5
5B R 1134 030 267 5
6A R 1136 004 034 5
8 R 1075 015 142 5
9B R 1077 006 054 5
12A R 1102 020 186 5
12B R 1097 016 148 5
15 R 1084 010 091 5
22A R 1112 016 147 5
22B R 1106 014 122 5
23 R 1066 009 088 5
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1977
Statistical Analysis 4
Exclusion of outliers 41
411 Numerical outlier technique Cochran amp Grubbs test
The statistical evaluation of data for this collaborative study followed the methods provided
by ISO 5725-21 For outlier testing the Grubbs and Cochran methods were used
ISO 5725-2 Tests Consistency
Cochranrsquos ndash test Within-laboratory variability Suitable for detecting whether the highest value in a set of laboratory standard deviations is an outlier or not
Grubbsrsquo ndash test Between-laboratory variability Suitable for detecting whether the highest (or lowest) laboratories averages are outliers or not
The protocol ldquoHarmonized statistical procedurerdquo defined by IUPAC (International Union of
Pure and Applied Chemistry) has been applied as well It consists of sequential applications of
the Cochran and Grubbs tests until no further outliers are detected or until a drop of more than
222 (for this study =29) in the original number of laboratories would occur (see flowchart
in Appendix F)
First apply the Cochran outlier test and if an outlying laboratory is identified then a single
value Grubbs test is performed on the individual values of this outlying laboratory (Individual
Grubbs) If no individual value is identified as outlier the outlying laboratory is removed
When an individual value is identified as an outlier only this value is removed
Afterwards single-value Grubbs test is applied and outlying laboratories are removed If no
laboratory is identified as outlier the pair-value test is applied (two values at the same end)
Remove any laboratory(ies) flagged by these tests but stop removal if more than 222 (2 of
9 laboratories) would be removed
The test was performed with both linear and rotary smoking machines together but also with
rotary respectively linear smoking machines separately The results provided in the report for
all smoking machines respectively with linear or rotary only smoking machines are obtained
after exclusion of the outliers for those respective categories
Note
The paired value Grubbsrsquo test is an extension of the single value Grubbs test for pairs of
outliers The use is advised in ISO 5725 to detect pairs of outlier undetectable sequentially by
using single value Grubbs test
The outlying laboratories are provided in the Tables 18 to 23
Repeatability and reproducibility estimation 42
Repeatability and reproducibility limits are calculated for both smoking regimes each
parameter and for both smoking machine types The results are summarized in tables 18 to 23
with all machines grouped respectively with linear or rotary machines only both with ISO
and intense smoking regimes Outlying laboratories are provided in the same tables The
corresponding graphs named ldquoindividual valuesrdquo are given in Part 5 of this report
1 ISO 5725-21994 Accuracy (trueness and precision) of measurement methods and results ndash Part 2 Basic
method for the determination of repeatability and reproducibility of a standard measurement method
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 2077
Table 18 r amp R estimations for CM8 under ISO smoking regime (all machines)
p n Global Mean Sr CVr[] r SR CVR [] R C GG2 Stragglers Parameter
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 1977
Statistical Analysis 4
Exclusion of outliers 41
411 Numerical outlier technique Cochran amp Grubbs test
The statistical evaluation of data for this collaborative study followed the methods provided
by ISO 5725-21 For outlier testing the Grubbs and Cochran methods were used
ISO 5725-2 Tests Consistency
Cochranrsquos ndash test Within-laboratory variability Suitable for detecting whether the highest value in a set of laboratory standard deviations is an outlier or not
Grubbsrsquo ndash test Between-laboratory variability Suitable for detecting whether the highest (or lowest) laboratories averages are outliers or not
The protocol ldquoHarmonized statistical procedurerdquo defined by IUPAC (International Union of
Pure and Applied Chemistry) has been applied as well It consists of sequential applications of
the Cochran and Grubbs tests until no further outliers are detected or until a drop of more than
222 (for this study =29) in the original number of laboratories would occur (see flowchart
in Appendix F)
First apply the Cochran outlier test and if an outlying laboratory is identified then a single
value Grubbs test is performed on the individual values of this outlying laboratory (Individual
Grubbs) If no individual value is identified as outlier the outlying laboratory is removed
When an individual value is identified as an outlier only this value is removed
Afterwards single-value Grubbs test is applied and outlying laboratories are removed If no
laboratory is identified as outlier the pair-value test is applied (two values at the same end)
Remove any laboratory(ies) flagged by these tests but stop removal if more than 222 (2 of
9 laboratories) would be removed
The test was performed with both linear and rotary smoking machines together but also with
rotary respectively linear smoking machines separately The results provided in the report for
all smoking machines respectively with linear or rotary only smoking machines are obtained
after exclusion of the outliers for those respective categories
Note
The paired value Grubbsrsquo test is an extension of the single value Grubbs test for pairs of
outliers The use is advised in ISO 5725 to detect pairs of outlier undetectable sequentially by
using single value Grubbs test
The outlying laboratories are provided in the Tables 18 to 23
Repeatability and reproducibility estimation 42
Repeatability and reproducibility limits are calculated for both smoking regimes each
parameter and for both smoking machine types The results are summarized in tables 18 to 23
with all machines grouped respectively with linear or rotary machines only both with ISO
and intense smoking regimes Outlying laboratories are provided in the same tables The
corresponding graphs named ldquoindividual valuesrdquo are given in Part 5 of this report
1 ISO 5725-21994 Accuracy (trueness and precision) of measurement methods and results ndash Part 2 Basic
method for the determination of repeatability and reproducibility of a standard measurement method
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 2077
Table 18 r amp R estimations for CM8 under ISO smoking regime (all machines)
p n Global Mean Sr CVr[] r SR CVR [] R C GG2 Stragglers Parameter
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3377
APPENDIX B ndash Experimental Protocol
PT_SS_Collaborative_Proficiency Study Protocol Template_Jan 2016_RAC_REV3pdf
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
Page 1 of 14
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR TEST PIECE CM8 - 2016
EXPERIMENTAL PROTOCOL
Linda A Crumpler Cerulean USA
08 January 2016
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
Page 2 of 14
1 Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified as important for describing elements of an experimental protocol for a collaborative study or a proficiency study as defined below (Horwitz 862)
bull Collaborative study
ldquoA collaborative study is an interlaboratory study in which each laboratory uses the defined method of analysis to analyse identical portions of homogeneous materials to assess the performance characteristics obtained for that method of analysisrdquo
CORESTA recognizes that collaborative studies require considerable effort and should be conducted only on methods that have received adequate prior testing
bull Proficiency Study
ldquoA proficiency study is an interlaboratory study consisting of one or more assays-conducted by a group of laboratories on one or more identical materials by whatever method is in use in each laboratory for the purpose of comparing the results of each laboratory with those of other laboratories with the objective of evaluating or improving performancerdquo
Proficiency studies often serve as pre-work for selecting a method for a full collaborative study
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
Page 3 of 14
2 Table of Contents 1 Foreword 2
1 Introduction 4
2 Objectives 4
3 Study Coordinator(s) 4
4 Normative References 4
5 Methods 5
51 General Guidance 5
52 Test Specimen(s) 5
53 Sampling 5
54 Ventilation Zone Blocking 6
55 Butt Marking 6
56 Conditioning 6
57 Test Piece Weight 6
58 Smoking Machine 6
59 Smoking Plans 7
6 Target Variables and Data Reporting 10
7 Study Time Table 11
8 Data Submission 12
9 Explanation of Statistics to be Applied for a Collaborative Study 12
91 Repeatability and Reproducibility Estimation 12
Bibliography 13
Appendix A ndash Systegraveme International (SI) Units and their Symbols 14
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
Page 4 of 14
1 Introduction The CORESTA Routine Analytical Chemistry Sub Group has been given the responsibility to organize the annual testing of the CORESTA Monitor test piece This year the study will include CM8
2 Objectives This yearrsquos study will have expanded objectives that include smoking the monitor test piece under both ISO and a specified intense smoking regime The study objectives are
bull To measure mainstream smoke yields of nicotine-free dry particulate matter (NFDPM) nicotine and carbon monoxide (CO) when smoked under ISO and a specified intense smoking regime
bull To establish the conditioned weight of CM8 prior to smoking bull To determine intra- and inter-laboratory variability for the measured smoke yields
and to continue this comparison over time bull To obtain statistical information about possible differences in smoke yields from
different smoking machines
3 Study Coordinator(s)
4 Normative References The relevant Standards for ISO smoking are
The relevant Standards for Intense smoking include the ISO Standards above and
Tar and Nicotine and CO T-115e4pdf
Note T-115 has been removed from the Health Canada website and therefore is embedded here
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
Page 5 of 14
5 Methods
51 General Guidance
As a general guide experiments conducted under each puffing regime should be conducted according to ISO standard requirements Exceptions to this guiding principle include the puffing parameters applied for intense smoking regime the vent blocking applied the number of cigarettes smoked per sample and the butt length for smoking The study (the smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm
Please note that any operating conditions (a) not specified in the above ISO standards or regarded as optional (b) not specified in the intense method documents provided as guidelines and (c) any circumstances that may have influenced test results should be noted in the test report
Puffing parameter and vent blocking specifications for each puffing regime are summarized in Table 1 Note Although the CORESTA Monitor Test Pieces are unventilated it is advised to follow the Health Canada procedures exactly and tape the filter ventilation zone
Table 1 Smoking Regime Specifications
plusmn plusmn plusmn
plusmn plusmn plusmn
52 Test Specimen(s)
53 Sampling The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine included in the study A composite of all packs should be prepared for conditioning according to ISO 82432006 If a substantial period of
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
Page 6 of 14
time is expected to occur between the times when the test pieces are smoked with the different smoking regimes then two separate composite samples should be prepared one for each smoking regime
54 Ventilation Zone Blocking The blocking of the filter ventilation zone will be achieved by wrapping a single layer of invisible tape 190 mm wide or equivalent around the complete circumference of the filter and tipping paper of the test articles
55 Butt Marking For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of 33 mm
56 Conditioning The composite samples shall be conditioned for at least 48 hours but no more than 10 days under the following conditions
Temperature 22 plusmn 1degC Relative humidity 60 plusmn 3
Temperature and relative humidity of the conditioning enclosure shall be checked and recorded for every smoking run
Test cigarettes to be smoked for the determination of NFDPM nicotine and CO should be selected at random from the conditioned cigarettes
Any test pieces with visible defects shall be discarded
57 Test Piece Weight The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape applied for intense smoking may vary between laboratories The weight of the test piece after conditioning is to be determined by weighing all test pieces to be smoked just before they are placed at the smoking machine The result is reported as the mean weight of the 20 test pieces for linear or rotary smoking machine at ISO puffing parameters
58 Smoking Machine Where smoking laboratories have more than one type of smoking machine (ie linear and rotary variants) they are encouraged to include as many types in the study as possible
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
Page 7 of 14
59 Smoking Plans The smoking plans will incorporate one product (CM8) shown as M in the smoking plans These plans are designed to smoke the CM8 in all ports for each puffing regime spread over a number of days If possible each participating laboratory should use only one operator (for each smoking machine type) throughout the course of the study
For ISO smoking one test result is defined as the mean yield obtained from smoking 20 test pieces in a single smoking machine run therefore from a rotary machine it is the result from one run smoking 20 test pieces and from a linear machine it is the average of four ports smoking five test pieces per port This is repeated on five separate days resulting in 100 test pieces being smoked (Tables 2-3)
For Intense smoking the number of test pieces smoked per filter pad is reduced to avoid overloading the pad As a consequence the number of smoking runsports has to be increased so that the same nominal numbers of test pieces are smoked Thus a test result from a rotary machine is the mean of two runs each of 10 test pieces and from a linear machine it is the average of eight ports smoking three test pieces per port (Tables 4-5)
Note that the side seam of the test pieces should be positioned at random and not in a fixed position since it has been observed that some laboratory staff habitually place cigarettes in a particular orientation Ports not occupied by the test pieces are left blank which may be assigned to any other cigarette that is to be smoked by the laboratory or the ports may be left empty
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
Page 8 of 14
Table 2 Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)
Table 3 Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
Page 9 of 14
Table 4 Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per pad)
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
Page 10 of 14
Table 5 Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per pad)
6 Target Variables and Data Reporting The variables to be reported fall into two categories those which will form the basis of the statistical evaluation of the data and those that are ancillary to the test The variables to be reported for statistical analysis are bull Mean weight of the Monitor after conditioning (just prior to smoking) bull Mean puff number per test piece bull Mean TPM per test piece bull Mean nicotine delivery per test piece bull Mean water delivery per test piece bull Mean NFDPM delivery per test piece bull Mean CO delivery per test piece The ancillary variables are bull Date of test bull Type of smoking machine used bull Temperature (Cdeg) and relative humidity (RH) of conditioning enclosure bull Temperature (Cdeg) and relative humidity (RH) of smoking environment bull Atmospheric pressure in the laboratory during smoking bull Ambient air flow in the smoking machine before smoking (mmsec)
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
Page 11 of 14
Dimensions and rounding of test results Analytical variables
Weight of Monitor mg per test piece
Puff number number
TPM mg per test piece
Nicotine mg per test piece
Water mg per test piece
NFDPM mg per test piece
Carbon Monoxide mg per test piece
Ancillary variables
Date of test DDMMYY
Conditioning temperature degrees Celsius
Conditioning humidity percent RH
Air velocity mms
Laboratory temperature degrees Celsius
Laboratory humidity percent RH
Laboratory barometric pressure
kPa
Please note that the rounding of the data to the formats specified above must take place after any calculations that may be involved All calculations will use the laboratory data as recorded using the maximum number of digits available All data arising from this study will be made available to the laboratories participating in the study The distribution of data will be done after collation and statistical evaluation To facilitate the statistical evaluation all data must be reported using the attached spreadsheets and must be submitted via e-mail Please use the attached spreadsheets as provided without changing the format
7 Study Time Table
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
Page 12 of 14
The smoking should be performed during January and February 2016 Strict adherence to the timeline is very important for the data to be compiled for an initial assessment at the next Sub-Group meeting on April 2016 Data not received by February 26 2016 will be excluded from the formal statistical analysis Please review your data carefully before submitting as the statistical analysis is very labour intensive
The statistical analysis of the results will follow as closely as possible the recommendations of ISO 5725
Should any questions arise please contact the study coordinator Linda Crumpler
All results must be sent via e-mail to
Linda A Crumpler lindacrumplerceruleancom
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
Page 13 of 14
Bibliography
Chem Pure Appl QUALITY ASSURANCE SCHEMES THE INTERNATIONAL HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL CHEMISTRY LABORATORIES (nd) n pag Web
Council of Science Editors 8th ed Np Council of Science Editors nd Print
Form and Style for ASTM Standards West Conshohocken PA ASTM INTERNATIONAL 2015 Print
Horwitz William Protocol for the Design Conduct and Interpretation of Collaborative Studies Pure and Applied Chemistry 606 (1988) 855-64 ShareGate International Union of Pure and Applied Chemistry De Gruyter Jan 1988 Web 30 July 2015
ISO 5725 Standard And Reference Laboratories Errorpdf ISO 5252 ISO 5725 Standard And Reference Laboratories Error (nd) n pag Web
IUPAC 2006 IUPAC Pure and Applied Chemistry 78 145ndash196 Np nd Web 25 Aug 2015
Numbers Units Mathematicial Expressions and Statistics Scientific Style and Format The CSE Manual for Authors Editors and Publishers 8th ed Chicago The University of Chicago 2014 157-91 Print
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
Page 14 of 14
Appendix A ndash Systegraveme International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol Length meter m Mass kilogram Kg Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1 Force newton N mmiddotkgmiddots-2 Pressure pascal Pa Nm2 Energy joule J Nmiddotm Power watt W Js Electric charge coulomb C smiddotA Electric potential volt V WA Electric resistance ohm Ω VA Celsius temperature Degrees Celsius degC K Unit degree Celsius is equal in magnititude to unit kelvin
SI prefixes
Factor Name Symbol Numerical Value 1012 tera T 1 000 000 000 000 109 giga G 1 000 000 000 106 mega M 1 000 000 103 kilo k 1 000 102 hecto h 100 101 deka da 10 10-1 deci d 01 10-2 centi c 001 10-3 milli m 0001 10-6 micro micro 0000 001 10-9 nano n 0000 000 001 10-12 pico p 0000 000 000 001
1 Foreword
1 Introduction
2 Objectives
3 Study Coordinator(s)
4 Normative References
5 Methods
51 General Guidance
52 Test Specimen(s)
53 Sampling
54 Ventilation Zone Blocking
55 Butt Marking
56 Conditioning
57 Test Piece Weight
58 Smoking Machine
59 Smoking Plans
6 Target Variables and Data Reporting
7 Study Time Table
8 Data Submission
9 Explanation of Minimum Statistics to be Applied for a Collaborative Study
91 Repeatability and Reproducibility Estimation
Bibliography
Appendix A ndash Systegraveme International (SI) Units and their Symbols
CORESTA
Piegravece jointe
RAC-103-CTR_Protocol-CM8-Coll-Study-2016pdf
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3477
APPENDIX C ndash Departures from Experimental Protocol
One Laboratory (Lab 9A) smoked 2 cigarettes per port on linear smoking machine for the
analyses performed with intense smoking regime
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 3577
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4277
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
21 12C L LX20 1 4690 1082 339 32680 2486 1122
12C L LX20 2 4622 1046 343 32330 2530 1139
12C L LX20 3 4654 1078 340 32360 2494 1110
12C L LX20 4 4642 1060 337 32450 2518 1080
12C L LX20 5 4612 1039 342 32310 2458 1125
13 22 13A R RM20H 1 NA NA NA NA NA NA
13A R RM20H 2 NA NA NA NA NA NA
13A R RM20H 3 NA NA NA NA NA NA
13A R RM20H 4 NA NA NA NA NA NA
13A R RM20H 5 NA NA NA NA NA NA
23 13B R RM20H 1 NA NA NA NA NA NA
13B R RM20H 2 NA NA NA NA NA NA
13B R RM20H 3 NA NA NA NA NA NA
13B R RM20H 4 NA NA NA NA NA NA
13B R RM20H M2
5 NA NA NA NA NA NA
14 24 14 R RM200A 1 NA NA NA NA NA NA
14 R RM200A 2 NA NA NA NA NA NA
14 R RM200A 3 NA NA NA NA NA NA
14 R RM200A 4 NA NA NA NA NA NA
14 R RM200A 5 NA NA NA NA NA NA
15 25 15 R RM200A 1 3949 827 3220 2800 2538 1085
15 R RM200A 2 3933 845 3234 2764 2502 1079
15 R RM200A 3 4041 856 3414 2843 2606 1101
15 R RM200A 4 3961 797 3375 2827 2562 1079
15 R RM200A 5 3902 791 3423 2769 2526 1076
16 26 16 L SM450 1 NA NA NA NA NA NA
16 L SM450 2 NA NA NA NA NA NA
16 L SM450 3 NA NA NA NA NA NA
16 L SM450 4 NA NA NA NA NA NA
16 L SM450 5 NA NA NA NA NA NA
17 27 17 L SM450 1 4280 1054 3590 4540 2350 1101
17 L SM450 2 4400 1049 3650 4540 2285 1124
17 L SM450 3 4323 995 3580 4540 2313 1105
17 L SM450 4 4498 1039 3740 4540 2359 1108
17 L SM450 5 4229 999 3550 4540 2298 1111
18 28 18 L SM450 1 NA NA NA NA NA NA
18 L SM450 2 NA NA NA NA NA NA
18 L SM450 3 NA NA NA NA NA NA
18 L SM450 4 NA NA NA NA NA NA
18 L SM450 5 NA NA NA NA NA NA
19 29 19 L SM450 1 4657 1142 3520 3162 2463 1061
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4377
Lab Count
Machine Count
Lab
Code
Machine Class
Machine Type
Run No
TPM (mgtp)
Water (mgtp)
Nicotine (mgtp)
NFDPM (mgtp)
CO (mgtp)
Puff count
19 L SM450 2 4526 1120 3520 3054 2501 1053
19 L SM450 3 4446 1085 3530 3008 2468 1073
19 L SM450 4 4561 1042 3530 3166 2497 1064
19 L SM450 5 4642 1086 3500 3205 2512 1045
20 30 20 L SM450 1 4612 1199 3480 3065 2472 1085
20 L SM450 2 4519 1127 3190 3074 2410 1076
20 L SM450 3 4474 1154 3610 2959 2476 1080
20 L SM450 4 4754 1273 3760 3105 2544 1120
20 L SM450 5 4722 1326 3720 3024 2544 1073
21 31 21 L SM450 1 5070 1282 3750 3413 2536 1136
21 L SM450 2 5029 1284 3710 3374 2511 1098
21 L SM450 3 4874 1259 3670 3248 2455 1126
21 L SM450 4 5029 1329 3730 3326 2577 1105
21 L SM450 5 5038 1272 3700 3396 2536 1141
22 32 22A R RM20H 1 4059 959 3205 2780 2511 1137
22A R RM20H 2 4019 957 3155 2746 2485 1097
22A R RM20H 3 4086 948 3295 2809 2478 1098
22A R RM20H 4 4022 949 3215 2752 2456 1115
22A R RM20H 5 4043 954 3240 2766 2420 1113
33 22B R RM200A 1 3995 938 3205 2737 2450 1119
22B R RM200A 2 3956 935 3135 2707 2455 1116
22B R RM200A 3 4005 871 3220 2812 2476 1084
22B R RM200A 4 4059 974 3220 2763 2435 1106
22B R RM200A 5 4062 912 3270 2823 2518 1107
23 34 23 R RM20H 1 3859 1602 6575 1599 2551 1076
23 R RM20H 2 3940 1630 6750 1636 2527 1067
23 R RM20H 3 3820 1656 6465 1517 2491 1053
23 R RM20H 4 3771 1616 6585 1496 2496 1062
23 R RM20H 5 3759 1489 6675 1603 2477 1074
24 35 24 L SM450 1 4741 1200 3510 3190 2431 1110
24 L SM450 2 4688 1177 3450 3166 2424 1110
24 L SM450 3 4776 1202 3620 3213 2454 1096
24 L SM450 4 4938 1315 3530 3270 2550 1068
24 L SM450 5 4769 1282 3510 3137 2493 1144
25 36 25 L SM450 1 4423 1002 3030 3117 2437 1091
25 L SM450 2 4431 1021 3050 3106 2463 1097
25 L SM450 3 4343 969 2930 3082 2401 1107
25 L SM450 4 4410 981 2970 3133 2246 1096
25 L SM450 5 4565 1046 2950 3224 2448 1120
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4477
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB
(G)
SINGLE
GRUBBS
OUTLIER
(G2)
PAIRED
GRUBBS
OUTLIER
END REPORT
ORIGINAL amp LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 29
NO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4577
APPENDIX F ndash Linear - Rotary Comparisons
Figure 1 CM8 under ISO smoking regime ndash r and R values (conditioned weight)
Figure 2 CM8 under ISO smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4677
Figure 3 CM8 under ISO smoking regime ndash r and R values (Water)
Figure 4 CM8 under ISO smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4777
Figure 5 CM8 under ISO smoking regime ndash r and R values (NFDPM)
Figure 6 CM8 under ISO smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4877
Figure 7 CM8 under ISO smoking regime ndash r and R values (Puff count)
Figure 8 CM8 under intense smoking regime ndash r and R values (TPM)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 4977
Figure 9 CM8 under intense smoking regime ndash r and R values (Water)
Figure 10 CM8 under intense smoking regime ndash r and R values (Nicotine)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5077
Figure 11 CM8 under intense smoking regime ndash r and R values (NFDPM)
Figure 12 CM8 under intense smoking regime ndash r and R values (CO)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5177
Figure 13 CM8 under intense smoking regime ndash r and R values (Puff count)
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5277
APPENDIX G ndash Rotary Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5377
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5477
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5577
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5677
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5777
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5877
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 5977
APPENDIX H ndash Linear Smoking Machines
1 ISO smoking regime
Figure 1 CM8 Individual observations of mainstream ldquoISOrdquo conditioned WEIGHT
Figure 2 CM8 Individual observations of mainstream ldquoISOrdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6077
Figure 3 CM8 Individual observations of mainstream ldquoISOrdquo WATER
Figure 4 CM8 Individual observations of mainstream ldquoISOrdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6177
Figure 5 CM8 Individual observations of mainstream ldquoISOrdquo NFDPM
Figure 6 CM8 Individual observations of mainstream ldquoISOrdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6277
Figure 7 CM8 Individual observations of mainstream ldquoISOrdquo PUFF Count
2 Intense smoking regime
Figure 8 CM8 Individual observations of mainstream ldquoIntenserdquo TPM
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6377
Figure 9 CM8 Individual observations of mainstream ldquoIntenserdquo WATER
Figure 10 CM8 Individual observations of mainstream ldquoIntenserdquo Nicotine
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6477
Figure 11 CM8 Individual observations of mainstream ldquoIntenserdquo NFDPM
Figure 12 CM8 Individual observations of mainstream ldquoIntenserdquo CO
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6577
Figure 13 CM8 Individual observations of mainstream ldquoIntenserdquo PUFF Count
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-STR-CM8 Coll Study 2016 ndash February 2017 6677
APPENDIX I ndash Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
1A RM200A Borgwaldt Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Octadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Measuring Unit Model No70700050 Borgwaldt
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
1B SM450 Cerulean Agilent 7890A
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase HP-20M Carbowax
Nicotine IS n-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
COA205Cerulean
Water Column Length 15m Film thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
2A RM200A Borgwaldt Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Anemometer Type g4403s-181 Schiltknecht Water Column
Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
2B SM450 Cerulean Agilent 68907890
Nic Column Length 25m id 032mm Film Thickness 03microm Stationary Phase Polyethylenglycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4452s-146 Schiltknecht
Cerulean COA205 Water Column Length 15m id 032mm Film Thickness 020microm Stationary Phase Polystrene - divinylbenzene
Water IS Ethanol
3 RM200 Borgwaldt 6890A Agilent
Nicotine Column Length 30m Id 032mm Film Thickness 025microm Stationary Phase Agilent 10191N-113 HP-INNOWAX
Nicotine IS n-Heptadecane
80709500Borgwaldt 70700050Borgwaldt Water Column Length 30m id 032 Film Thickness 020microm Stationary Phase JampW 1909 IP-Q04 bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
4A RM200A Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6877
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
4B RM20D Borgwaldt Agilent 6890
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Schiltknecht CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase Porapak Q cross-linked
Water IS Ethanol
5A RM20 Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine IS n-Heptadecane
Anemometer Type g 4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
5B RM200A Borgwaldt Agilent 6890 7890
A
Nic Column Length 5m id 020 Film Thickness 040microm Stationary Phase DB-WAXetr high polarity polyethylene glycol (PEG)
Nicotine ISn-Heptadecane
Anemometer Type g4403s-113 Schiltknecht
CO-Analyser Borgwaldt
Water Column Length 6 Stainless Steel Packed id 2mm Stationary Phase JampW Porapak QS 80-100 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 6977
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
6A RM20D Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine ISn-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
6B LX20 Borgwaldt 7890 B Agilent
Nic Column INNO Steel Packed Length 18m id 20mm Stationary Phase 75 Carbowax 2 KOH 80100 Chromosorb-WAW
Nicotine IS n-Heptadecane
Schiltknecht C24 Borgwaldt Water Column INNO Steel packed column Length 360m id 20mm Stationary Phase 6080 Hayesep-Q porous polymer
Water IS Methanol
7A SM450 Cerulean Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine IS n-Heptadecane
Schiltknecht Cerulean COA205 Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7077
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
7B RM200A Borgwaldt Agilent 7890
Nic Column Capillary HP-20M Length 25m id 032mm Film Thickness 030microm Stationary Phase Polyethylene Glycol
Nicotine ISn-Heptadecane
Schiltknecht Borgwaldt Water Column Capillary Length 15m id 032mm Film Thickness 020microm Stationary Phase HP Plot-Q bonded polystyrene-divinyl benzene (DVB)
Water IS Ethanol
8 RM20H Borgwaldt Agilent 6890
Nic Column Length 18m id 2mm Film Thickness Stationary Phase 10 Carbowax 2M 2 KOH
Nicotine IS n-Heptadecane
Schiltknecht C24Borgwaldt
Water Column Porapak Q 2m packed
Water IS Ethanol
9A SM450RH Cerulean Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine IS n-Heptadecane
ThermoAire3 Schiltknecht Cerulean COA200 Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7177
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
9B RM200A Borgwaldt Agilent 7890
Nic Column Capillary Agilent CP7424 Length id Film Thickness Stationary Phase CP-Wax
Nicotine ISn-Heptadecane
RM200A Schiltknecht Integrated NDIR analyser Water Column Capillary Agilent CP7554 Length id Film Thickness Stationary Phase PoraPLOT Q
Water IS Ethanol
10 SM450 Cerulean Agilent 7890
Nic Column Capillary Length 5m id 0200mm Film Thickness 040microm Stationary Phase DB-Wax ETR
Nicotine IS Octadecane
ThermoAire2 Schiltknecht Cerulean COA
Water Column Packed 6 ft x 18 in x 21mm 80-100 mesh Porapak Q
Water IS Ethanol
11 SM450 Cerulean Agilent 6890
Nic Column Capillary CP WAX 52 CB Length id 053mm Film Thickness 1microm Stationary PhaseCP-Wax
Nicotine IS Decanol
Schiltknecht Cerulean COA205
Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7277
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
12A RM200A Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12B RM200A2 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary PhaseCP-Wax
Nicotine IS Heptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
12C KC LX20 Borgwaldt HP 6890
Nic Column Length 30m id 032mm Film Thickness 025microm Stationary Phase CP-Wax
Nicotine ISHeptadecane
Schiltknecht SibenchSiemens Water Column Capillary Length id 053mm Film Thickness 20microm Stationary Phase PoraPLOT Q
Water IS Methanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7377
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
13A RM20H Borgwaldt M1 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403S-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Water IS Ethanol
13B RM20H Borgwaldt M2 Agilent 7890B
Nic Column Length 5m id Film Thickness 04microm Stationary Phase DB-WAXETR
Nicotine IS n-Heptadecane
Schiltknecht g4403s-113
Built in RM20H Water Column Length 30m id Film Thickness 40microm Stationary Phase PoraPLOT Q
Ethanol
14 RM200A Borgwaldt Nicotine Agilent
6890 Water Agilent 7890
Nic Column Length 30 id 0320mm Film thickness 025 Stationary Phase HP-INNOWAX
Nicotine IS n-Heptadecane
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 30m id 0320mm Film Thickness 20microm Stationary Phase HP-PLOTQ
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7477
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
15 RM200A Borgwaldt Agilent 7890B
Nic Column Length 2m id 18in Film thickness Stationary Phase 80-100 mesh Carbowax 20M 2 KOH
Nicotine IS Quinaldine
Schiltknecht g4403s-176
Borgwaldt COCO2 Analyser Water Column Length 2m id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
16 SM450 Cerulean Agilent 6890
Nic Column Length 6ft Stainlees Steel id 18in Film thickness Stationary Phase 80100 mesh2 Versamid + 1 KOH on Chromasorb 750
Nicotine ISn-Heptadecane
ThermoAire2 SchiltknechtVMD100 Filtrona
Cerulean COA 205
Water Column Length 6ft Stainlees Steel id 18in Film Thickness Stationary Phase 80100 mesh Porapak Q
Water IS Methanol
17 SM450 Cerulean Agilent 6890N
Nic Column Length 10m id 018mm Film thickness 03microm Stationary Phase DB Wax
Nicotine IS Anethole
VPS 103 Schiltknecht
Cerulean COA 205 Water Column Length 3ft Stainlees Steel id 025in Film Thickness Stationary Phase Haye SepQ 6080 mesh
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7577
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
18 SM450 Cerulean Agilent 6890
Nic Column Length 30m id 053mm Film Thickness 1microm Stationary Phase Restek Stabilwax
Nicotine IS Anethole
ThermoAire2 Schiltknecht Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
Water IS Ethanol
19 SM450 Cerulean 598 2200 8821
int297
Nic Column Polyethylene glycol 20 M + 10 KOH + 2 Chromosorb W80100 AW-DMCS Shimadzu 20 m x 30 m
Nicotine IS Heptadecane
996 ThermoAire2 Schiltknecht Cerulean COA 205
Water Column PorapakQ 80100 Shimadzu 20m x 30m
Water IS Ethanol 998
20 SM450 Cerulean HP 5890
Nic Column Length 30m id 053mm Film thickness 01microm Stationary Phase Restek Stabilwax
Nicotine IS n-Heptadecane
Schiltknecht 1 Air Flow meter
Cerulean COA 205
Water Column Supelco 80100 mesh Porapak R 18x 21mm
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
435-2Testo Cerulean COA 205 Water Column Length 2m id 2mm Film Thickness Stationary Phase 80100 mesh Porapak QS
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS
ThermoAire2 Schiltknecht Cerulean COA 205 Water Column SS 18OD Stationary Phase Porapak QS 80100 mesh
Water IS Ethanol
1 Introduction
2 Organisation
21 Participants
22 Protocol
3 Raw Data
4 Statistical Analysis
41 Exclusion of outliers
411 Numerical outlier technique Cochran amp Grubbs test
42 Repeatability and reproducibility estimation
5 Data Representation
51 ISO smoking regime
52 Intense smoking regime
6 Comparison
61 Comparisons of Linear with Rotary smoking machines for test piece CM8
62 Comparison with previous studies
7 Conclusion
APPENDIX A - List of Participating Laboratories
APPENDIX B ndash Experimental Protocol
APPENDIX C ndash Departures from Experimental Protocol
APPENDIX D ndash Raw Data Set
APPENDIX E ndash IUPAC 1994 Harmonized Statistical Procedure
APPENDIX F ndash Linear - Rotary Comparisons
APPENDIX G ndash Rotary Smoking Machines
APPENDIX H ndash Linear Smoking Machines
APPENDIX I ndash Equipment Survey
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7677
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
22A RM20H Borgwaldt
Model No 70740010 Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
22B RM20D Borgwaldt Model No70750020
Agilent 7890A
Nic Column Length 2m id 18 Film thickness 21mm Stationary Phase 10 Carbowax 20M + 2 KOH
Nicotine IS Heptadecane
Schiltknecht g4403s-176
70740050Borgwaldt Water Column Length 2m id 18 Film Thickness 20mm Stationary Phase 80100 mesh Porapak Q
Water IS Ethanol
23 RM20H Borgwaldt Agilent 7890B
Nic Column Length 30m id Film thickness 025microm Stationary Phase HP-5MS Crosslinked 5 PHME Siloxane
Nicotine IS Heptadecane
Schiltknecht Flow Meter Borgwaldt CO Analyzer Water Column Length 30m id Film Thickness 20microm Stationary Phase HP-Plot Q Divenylbenzenestyrene porous polymer
Water IS Ethanol
RAC-103-CTR CM8 Coll Study 2016 ndash February 2017 7777
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph ModelManufacturerColumn Internal Standards
Airlflow Meter ModelManufacturer
NDIR analyser ModelManufacturer
24 SM450 Cerulean Agilent 7890B
Nic Column Length 15m + 5m guard id 032mm Film thickness 025microm Stationary Phase Restek 10821 Stabilwax-DB
Nicotine IS Heptadecane
Schiltknecht Messtechnik ThermoAire6
Cerulean COA 205 Water Column Length 10 id 18 Film Thickness Stationary Phase 80100 mesh Porapak-QS