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Coresta Sub Group Monitoring and Maintenance of Physical Test Methods Interlaboratory Proficiency Test 2009 Page 1 of 42 CORESTA Monitoring and Maintenance of Physical Test Methods Sub - Group 2009 Interlaboratory Proficiency Test Issued by: Graham Errington R & D Centre British American Tobacco Regents Park Road Millbrook Southampton United Kingdom SO15 8TL Phone: 02380 793540 e-mail: [email protected]
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MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

Oct 06, 2020

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Page 1: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

Coresta Sub Group

Monitoring and Maintenance of Physical Test Methods

Interlaboratory Proficiency Test 2009

Page 1 of 42

CORESTA Monitoring and Maintenance of Physical Test Methods Sub - Group

2009 Interlaboratory Proficiency Test

Issued by:

Graham Errington

R & D Centre

British American Tobacco

Regents Park Road

Millbrook

Southampton

United Kingdom

SO15 8TL

Phone: 02380 793540

e-mail: [email protected]

Page 2: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

Coresta Sub Group

Monitoring and Maintenance of Physical Test Methods

Interlaboratory Proficiency Test 2009

Page 2 of 42

Page 3: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

Coresta Sub Group

Monitoring and Maintenance of Physical Test Methods

Interlaboratory Proficiency Test 2009

Page 3 of 42

PARTICIPATING LABORATORIES British American Tobacco (Germany) GmbH, Weistrasse 26, 95448 Bayreuth, Germany

British American Tobacco, Denmark

Cerulean, Rockingham Drive, Linford Wood East, Milton Keynes, MK14 6LY, UK

Hauni

Imperial Tobacco - HH

Imperial Tobacco - LA

Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku,

Tokyo 130-8603, Japan

JT International Germany GmbH, Zentrale Warenaufnahme, R & D Building/GQA-Laboratories,

Diedenhofener Str. 20, D-54294 Trier, Germany

Rhodia Acetow GmbH, Engesserstr. 8, D-79123 Freiburg, Germany

SODIM SA, 4 rue André Dessaux, 45404 Fleury les Aubrais cedex, France

ST Poland, 32-400 Myslenice, Jawornik 360, Poland

Papierfabrik Wattens GmbH & Co KG, Ludwig-Lassl-Strasse 15, A-6112 Wattens, Austria

Zhengzhou Tobacco Research Institute of CNTC, No. 2 Fengyang St., Zhengzhou New & High-Tech Industries, Development Zone, Henan 450001, China

Page 4: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

Coresta Sub Group

Monitoring and Maintenance of Physical Test Methods

Interlaboratory Proficiency Test 2009

Page 4 of 42

2009 CORESTA MMPTM SUB – GROUP INTERLABORATORY PROFICIENCY TEST

Introduction The purpose of an interlaboratory proficiency testing scheme

1 is to provide participating laboratories

with an objective means of assessing and demonstrating the reliability of the data they are producing, and is an important component of any laboratory quality assurance scheme. The importance of proficiency testing is recognised in ISO/IEC Guide 17025

2 where “participation in interlaboratory

comparison or proficiency testing programmes” is listed as an important component of quality assurance results.

Outline of Test Protocol Five filter types and five cigarette brands were selected to cover the range of interest for Individual Weight, Circumference, Pressure Drop and Ventilation.

The samples used in the study are presented in Table 1.

Table 1.

SAMPLE TYPE

SAMPLE ID VARIANT Pressure Drop

Type

Monoaceate

Filter

F1 Semi - Slim

F2 Slim

F3 King Size/ Regular High

F4 King Size/ Regular Low

F5 King Size/ Regular Medium

Cigarette

C1 King Size/ Regular

C2 King Size/ Regular

C3 Slim

C4 Super Slim

C5 Super Slim

Participating laboratories were instructed to measure a sub – group of 10 specimens under their normal operating conditions, repeated 3 times for each sample. Mean values of each replicate were reported in an Excel spreadsheet supplied with the protocol.

After completion, the spreadsheets were returned to the author for data analysis.

Data Analysis Statistical analysis was carried out using Microsoft Excel and MINITAB v15. All graphs were produced with MINITAB v15.

Page 5: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

Coresta Sub Group

Monitoring and Maintenance of Physical Test Methods

Interlaboratory Proficiency Test 2009

Page 5 of 42

Summary statistics were calculated for each sample, followed by individual value plots by laboratory, to identify potential outliers.

Precision Statistics

Following identification and removal of outliers, Reproducibility, R, and repeatability, r, were calculated for each sample and tabulated at the beginning of each section.

Mandel Plots

h statistics for between laboratory consistency, and k statistics for within laboratory consistency were calculated and plotted according to ISO 5725 – 2

3, for each product characteristic

Repeatability Variation (Cochran’s Test)

Cochran’s test4 was used to evaluate the within – laboratory performance of each laboratory

where smax is the highest standard deviation in a set of p laboratories. The following criteria were used to asses each laboratory:

If the test statistic, c, is:

- ≤ 5% critical value Accept

- > 5% critical value ‹ 10% critical value Straggler

- > 10% critical value Outlier

Z - scores

After removal of outliers, robust estimates of means of all laboratories were used as the reference for computing z – scores

Z – scores are plotted in ascending order. Laboratory performance is indicated using the following criteria:

|z| < 1 = good

1< |z| < 2 = satisfactory

2< |z| < 3 = questionable

|z| > 3 = highly questionable

Results are presented separately for Filters and cigarettes.

p

i

is

sc

1

2

2

max

outliers for adjusted deviation standard overall

value mean Total

value mean Single

-

s

X

x

s

XxZ

)(

Page 6: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

Coresta Sub Group

Monitoring and Maintenance of Physical Test Methods

Interlaboratory Proficiency Test 2009

Page 6 of 42

FILTER DATA ANALYSIS

Table 2. Filter Summary Statistics

Instrument Manufacturer/ Type Codes for Individual Value Plots

Instrument Manufacturer/Type Code

Borgwaldt 1

Cerulean 2

Sodiline 3

Sodimat 4

Sodimax 5

Sodimax CCD 6

VariableSample

IDN N* Mean StDev CoefVar Minimum Median

Maximu

mRange

F2 42 0 461.45 3.660 0.79 452.50 462.73 466.00 13.500

F1 41 1 510.45 3.770 0.74 501.30 512.00 518.00 16.700

F4 42 0 798.88 6.490 0.81 784.60 800.00 810.50 25.900

F5 42 0 894.37 6.400 0.72 878.40 895.23 903.00 24.600

F3 42 0 1044.20 8.000 0.77 1025.30 1047.00 1055.80 30.500

F2 42 0 18.00 0.028 0.16 17.93 18.01 18.04 0.117

F1 41 1 21.18 0.034 0.16 21.10 21.19 21.24 0.143

F5 42 0 24.47 0.037 0.15 24.39 24.47 24.55 0.165

F4 42 0 24.43 0.038 0.15 24.34 24.45 24.49 0.146

F3 42 0 24.43 0.049 0.20 24.23 24.45 24.49 0.260

F4 39 3 243.54 6.070 2.49 222.80 244.00 253.00 30.200

F1 38 4 396.98 12.760 3.21 351.90 396.60 414.30 62.400

F2 36 6 412.96 13.300 3.22 370.90 416.00 429.00 58.100

F5 39 3 538.44 25.480 4.73 432.40 544.70 565.00 132.600

F3 39 3 779.62 47.290 6.07 598.60 791.40 818.00 219.400

Individual Wt Mean mg

Circum Mean mm

PD (fully encapsulated)

Page 7: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

Coresta Sub Group

Monitoring and Maintenance of Physical Test Methods

Interlaboratory Proficiency Test 2009

Page 7 of 42

Filter Rod Individual Weights

Laboratory N did not measure weights on any filter samples.

Precision Statistics Individual weights data were screened for outliers and precision statistics calculated for each filter sample.

Table 3. Filter Rod Individual Weights Precision Statistics.

Individual value plots for each sample are shown in Fig.1. Individual data points are represented by solid symbols, and laboratory means by open circles.

Mandel Plots

The h statistic Mandel Plots (Fig.2) show that no laboratory is significantly different.

There are no apparent exceptional values in the k – statistic plots in Fig. 3.

Repeatability Variation

Cochran’s test did not identify any exceptional variances.

Z – scores (Fig.4)

Results for Laboratory C are questionable for all filters.

Filter Type Sample ID Mean sr sR r R CoV

SemiSlim F1 510.5 1.48 3.77 4.14 10.56 0.74

Slim F2 461.5 1.27 3.66 3.56 10.25 0.79

KS F3 1044.2 2.92 8.00 8.18 22.40 0.77

KS F4 798.9 3.36 6.49 9.41 18.17 0.81

KS F5 894.4 2.54 6.40 7.11 17.92 0.72

Page 8: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

Coresta Sub Group

Monitoring and Maintenance of Physical Test Methods

Interlaboratory Proficiency Test 2009

Page 8 of 42

Figure 1. Filter Rod Individual Weights – Individual Value Plots

Individual Values represented by solid symbols, mean values represented by open circles.

NJMIFEAHGPKDCBL

520

510

500

Indiv

idual W

t M

ean m

g

1

2

3

4

5

6

Inst_Code

NJMIFEAHGPKDCBL

465

460

455

Indiv

idual W

t M

ean m

g

1

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Inst_Code

NJMIFEAHGPKDCBL

1050

1040

1030

Indiv

idual W

t M

ean m

g

1

2

3

4

5

6

Inst_Code

NJMIFEAHGPKDCBL

810

800

790

Indiv

idual W

t M

ean m

g1

2

3

4

5

6

Inst_Code

NJMIFEAHGPKDCBL

900

890

880

Indiv

idual W

t M

ean m

g

1

2

3

4

5

6

Inst_Code

Sample_ID = F1 Sample_ID = F2

Sample_ID = F3 Sample_ID = F4

Sample_ID = F5

Page 9: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

Coresta Sub Group

Monitoring and Maintenance of Physical Test Methods

Interlaboratory Proficiency Test 2009

Page 9 of 42

Figure 2. Filter Rod Individual Weights – h statistic Mandel Plots

Sample F5F4F3F2F1

2

1

0

-1

-2

h

kcrit

kcrit

J

K

L

M

P

A

B

C

D

E

F

G

H

I

C ode

Lab

Lab C ode PMLKJIHGFEDCBA

2

1

0

-1

-2

h

hcrit

hcritF 1

F2

F3

F4

F5

Sample

Individual Weight h statistics - Labs within Samples

Individual Weight h statistics - Samples within Labs

Page 10: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

Coresta Sub Group

Monitoring and Maintenance of Physical Test Methods

Interlaboratory Proficiency Test 2009

Page 10 of 42

Figure 3. Filter Rod Individual Weights – k statistic Mandel Plots

Sample F5F4F3F2F1

2.0

1.5

1.0

0.5

0.0

k

kcrit

J

K

L

M

P

A

B

C

D

E

F

G

H

I

C ode

Lab

Lab C ode PMLKJIHGFEDCBA

2.0

1.5

1.0

0.5

0.0

k

kcritF 1

F2

F3

F4

F5

Sample

Individual Weight k statistics - Labs within Samples

Individual Weight k Statistics - Samples within Labs

Page 11: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

Coresta Sub Group

Monitoring and Maintenance of Physical Test Methods

Interlaboratory Proficiency Test 2009

Page 11 of 42

Figure 4. Filter Rod Individual Weights – z -Score Plots

CKBMFAJHEDLPGI

3

2

1

0

CBKMIDFPALHGJE

3

2

1

0

CBKMDAIFPJGLHE

3

2

1

0

CKBDIMFJEAHGLP

3

2

1

0

CKMBADPFGIHLEJ

3

2

1

0

F1 F2

F3 F4

F5

Page 12: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

Coresta Sub Group

Monitoring and Maintenance of Physical Test Methods

Interlaboratory Proficiency Test 2009

Page 12 of 42

Filter Circumference

Table 4. Filter Circumference Precision Statistics.

Results for Lab N excluded. One outlier removed sample F3, laboratory J.

Individual value plots for each sample are shown in Fig.5. Individual data points are represented by solid symbols, and laboratory means by open circles.

Mandel Plots

Mandel plots do not show any laboratories beyond critical values (Note Laboratory N was not included in any of the filter analysis, and one measurement removed from sample F3, laboratory J).

Repeatability Variation

Cochran’s test did not show any labs as outliers (one measurement removed form laboratory J).

Z – scores

Results for Laboratory C (Fig.8) are questionable for Filters F1 and F2.

Results for Laboratory B, Filters F2 and F4 are questionable.

Laboratories with missing data points did not, or were unable to, measure the samples.

Filter Type Sample ID Mean sr sR r R CoV

SemiSlim F1 21.180 0.015 0.034 0.041 0.096 0.16

Slim F2 18.000 0.009 0.028 0.024 0.078 0.16

KS F3 24.440 0.016 0.037 0.044 0.104 0.15

KS F4 24.430 0.014 0.038 0.039 0.106 0.15

KS F5 24.470 0.019 0.037 0.052 0.102 0.15

Page 13: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

Coresta Sub Group

Monitoring and Maintenance of Physical Test Methods

Interlaboratory Proficiency Test 2009

Page 13 of 42

Figure 5. Filter Rod Circumference – Individual Value Plots

JMIFEAHGPKDCBL

21.20

21.15

21.10

Circum

Mean m

m

1

2

3

4

5

Inst_Code

JMIFEAHGPKDCBL

18.05

18.00

17.95

Circum

Mean m

m

1

2

3

4

5

Inst_Code

JMIFEAHGPKDCBL

24.45

24.40

24.35

Circum

Mean m

m

1

2

3

4

5

Inst_Code

JMIFEAHGPKDCBL

24.45

24.40

24.35

Circum

Mean m

m

1

2

3

4

5

Inst_Code

JMIFEAHGPKDCBL

24.56

24.48

24.40

Circum

Mean m

m

1

2

3

4

5

Inst_Code

Sample_ID = F1 Sample_ID = F2

Sample_ID = F3 Sample_ID = F4

Sample_ID = F5

Page 14: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

Coresta Sub Group

Monitoring and Maintenance of Physical Test Methods

Interlaboratory Proficiency Test 2009

Page 14 of 42

Figure 6. Filter Rod Circumference: h – statistic Mandel Plots

Sample F5F4F3F2F1

2

1

0

-1

-2

h

hcrit

hcrit

J

K

L

M

P

A

B

C

D

E

F

G

H

I

C ode

Lab

Lab C ode PMLKJIHGFEDCBA

2

1

0

-1

-2

h

hcrit

hcritF 1

F2

F3

F4

F5

Sample

Filter Circumference h Statistics - Labs within Samples

Filter Circumference h Statistics - Samples within Labs

Page 15: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

Coresta Sub Group

Monitoring and Maintenance of Physical Test Methods

Interlaboratory Proficiency Test 2009

Page 15 of 42

Figure 7. Filter Rod Circumference: k – statistic Mandel Plots

Sample F5F4F3F2F1

2.0

1.5

1.0

0.5

0.0

k

kcrit

J

K

L

M

P

A

B

C

D

E

F

G

H

I

C ode

Lab

Lab C ode PMLKJIHGFEDCBA

2.0

1.5

1.0

0.5

0.0

k

kcritF 1

F2

F3

F4

F5

Sample

Filter Circumference k - Statistics - Labs within samples

Filter Circumference k - Statistics - Samples within labs

Page 16: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

Coresta Sub Group

Monitoring and Maintenance of Physical Test Methods

Interlaboratory Proficiency Test 2009

Page 16 of 42

Figure 8. Filter Rod Circumference z -score Plots

CBAKDPMHEFLGIJ

2

1

0

Z_F1

BCDFAMKPLHJIGE

2

1

0

Z_F2

CBKHGMEADJPILF

2

1

0

Z_F3

BCKAPFMDGHILJE

2

1

0

Z_F4

CMAKGLBFPIHDJE

2

1

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LAB ID_F5

Z_F5

F1 F2

F3 F4

F5

Page 17: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

Coresta Sub Group

Monitoring and Maintenance of Physical Test Methods

Interlaboratory Proficiency Test 2009

Page 17 of 42

FILTER ROD PRESSURE DROP

Table 5. Filter Rod Pressure Drop Precision Statistics

Laboratories N and B not included.

Filter Type Sample ID Mean sr sR r R CoV

SemiSlim F1 400.030 2.603 6.770 7.288 18.956 1.69

Slim F2 416.170 2.297 7.720 6.432 21.616 1.86

KS F3 792.420 5.513 12.880 15.436 36.064 1.63

KS F4 244.620 2.519 3.960 7.053 11.088 1.62

KS F5 545.230 3.266 6.950 9.145 19.460 1.27

Individual value plots for each sample are shown in Fig.9. Individual data points are represented by solid symbols, and laboratory means by open circles.

Mandel Plots

The h statistic Mandel Plots (Fig.10) show that Laboratory B is significantly different from the grand mean for all filters.

The k statistic plot (Fig.11) shows that Laboratory B’s within – laboratory variation is significantly different for all samples

Repeatability Variation

Cochran’s test identifies the results for all filters for laboratory B as outliers.

Z – scores

Results for all filters for Laboratory B were identified as outliers

Laboratories with missing data points did not, or were unable to, measure the samples.

Page 18: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

Coresta Sub Group

Monitoring and Maintenance of Physical Test Methods

Interlaboratory Proficiency Test 2009

Page 18 of 42

Figure 9. Filter Rod Pressure Drop – Individual Value Plots

PMLKJIHGFEDCBA

400

375

350

PD

(fu

lly e

ncapsula

ted)

Mean m

m

J

K

L

M

P

A

B

C

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F

G

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Lab_Code

PMLKJIHGFEDCBA

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400

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PD

(fu

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ted)

Mean m

m

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PMLKJIHGFEDCBA

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(fu

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Mean m

m

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PMLKJIHGFEDCBA

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(fu

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ted)

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m

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PMLKJIHGFEDCBA

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500

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(fu

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ted)

Mean m

m

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G

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Lab_Code

Sample_ID = F1 Sample_ID = F2

Sample_ID = F3 Sample_ID = F4

Sample_ID = F5

Page 19: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

Coresta Sub Group

Monitoring and Maintenance of Physical Test Methods

Interlaboratory Proficiency Test 2009

Page 19 of 42

Figure 10. Filter Rod Pressure Drop: h - statistic Mandel Plots

F5F4F3F2F1

2

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-4

h

hcrit

hcrit

J

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P

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Lab

PMLKJIHGFEDCBA

2

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-4

h

hcrit

hcrit

F 1

F2

F3

F4

F5

Sample

Filter PD h Statistics - Labs within Samples

Filter PD h Statistics -Samples within Labs

Page 20: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

Coresta Sub Group

Monitoring and Maintenance of Physical Test Methods

Interlaboratory Proficiency Test 2009

Page 20 of 42

Figure 11. Filter Rod Pressure Drop: k - statistic Mandel Plots

F5F4F3F2F1

2.4

1.8

1.2

0.6

0.0

k

kcrit

J

K

L

M

P

A

B

C

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F

G

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C ode

Lab

PMLKJIHGFEDCBA

2.4

1.8

1.2

0.6

0.0

k

kcrit

F 1

F2

F3

F4

F5

Sample

Filter PD k Statistics - Labs within Samples

Filter PD k Statistics - Samples within Labs

Page 21: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

Coresta Sub Group

Monitoring and Maintenance of Physical Test Methods

Interlaboratory Proficiency Test 2009

Page 21 of 42

Filter Rod Pressure Drop – Repeatability Variation

Laboratory G did not submit data. All samples from Laboratory B were outliers.

Figure 12. Filter Rod Pressure Drop: z – score Plots

GBPAMICDHFLJEK

3

2

1

0

Z_Score

LGBICAMPDKHEFJ

3

2

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Z_Score

GBAIMPDKFLJHEC

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Z_Score

GBACILHMJEFPDK

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GBAIMPEKFCDHJL

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Z_Score

F1 F2

F3 F4

F5

Page 22: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

Coresta Sub Group

Monitoring and Maintenance of Physical Test Methods

Interlaboratory Proficiency Test 2009

Page 22 of 42

CIGARETTE DATA ANALYSIS

Laboratory P did not measure cigarettes. Laboratory N only measured circumference, but the values are not included in the analysis because they are wildly different from the rest of the laboratories. Laboratory I did not report PDo or Ventilation results.

Table 6. Cigarette Summary Statistics

Instrument Manufacturer/ Type Codes for Individual Value Plots

Instrument Manufacturer/Type Code

Borgwaldt 1

Cerulean 2

Sodiline 3

Sodimat 4

Sodimax 5

Variable Sample_ID N N* Mean StDev CoefVar Minimum Median Maximum

C1 39 0 954.86 13.410 1.4 921.00 954.00 993.90

C2 39 0 958.76 12.270 1.3 936.00 959.00 986.00

C3 39 0 716.26 10.620 1.5 688.00 717.00 741.60

C4 39 0 664.49 14.390 2.2 636.00 666.00 695.50

C5 39 0 657.69 12.580 1.9 633.00 661.00 680.70

C1 39 0 24.98 0.488 2.0 24.80 24.90 27.92

C2 39 0 25.01 0.491 2.0 24.84 24.94 27.97

C3 39 0 21.46 0.075 0.4 21.24 21.45 21.71

C4 39 0 18.02 0.027 0.2 17.97 18.01 18.08

C5 39 0 18.05 0.324 1.8 17.93 17.99 19.97

C1 36 3 118.71 6.200 5.2 100.10 119.75 127.80

C2 36 3 108.61 4.270 3.9 95.90 108.95 117.50

C3 36 3 120.00 3.130 2.6 115.00 119.50 126.80

C4 36 3 182.98 9.100 5.0 175.00 180.05 212.40

C5 36 3 98.32 31.250 31.8 85.00 88.75 204.10

C1 36 3 20.86 6.580 31.5 17.43 19.00 42.70

C2 36 3 29.53 5.780 19.6 26.53 27.84 48.70

C3 36 3 42.58 2.844 6.7 40.60 41.80 52.30

C4 36 3 46.10 4.570 9.9 41.85 45.05 61.20

C5 36 3 81.17 0.836 1.0 78.80 81.40 82.60

Individual Wt Mean mg

Circum Mean mm

PD open Mean mmWG

Vent % Mean

Page 23: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

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Page 23 of 42

CIGARETTE INDIVIDUAL WEIGHTS

Table 7. Cigarette Individual Weights – Precision Statistics

Individual value plots for each sample are shown in Fig.13. Individual data points are represented by open circles, and laboratory means by solid circles.

Mandel Plots

The h statistic Mandel Plots (Fig.14) do not show any laboratories significantly different from the reference value.

The k statistic plot (Fig.15) does not suggest exceptional variation for any single laboratory.

Repeatability Variation

Cochran’s test shows repeatability variation is acceptable for all laboratories.

Z – scores

Results for Laboratory D (Fig.16), cigarette 1 and 3 are questionable. Results for Laboratory C are questionable.

There are no questionable results for cigarettes 2, 4 and 5.

Laboratories with missing data points did not, or were unable to, measure the samples.

Cigarette Type Sample ID Mean sr sR r R CoV

SuperSlim C5 657.7 4.53 12.58 12.68 35.22 1.9

SuperSlim C4 664.5 6.57 14.39 18.40 40.29 2.2

Slim C3 715.7 4.38 6.53 12.26 18.28 0.9

KS C1 955.5 7.09 9.86 19.85 27.61 1.0

KS C2 958.8 0.57 12.27 1.59 34.36 1.3

Page 24: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

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Figure 13. Cigarette Individual Weights – Individual Value Plot

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Page 25: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

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Figure 14. Cigarette Individual Weights: h – statistic Mandel Plots

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Individual Weights h statistics - Labs within Samples

Individual Weights h statistics - Samples within Labs

Page 26: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

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Figure 15. Cigarette Individual Weights: k – statistic Mandel Plots

C 5C 4C 3C 2C 1

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Individual Weight k statistics - Labs within Samples

Individual Weight k statistics- Samples within Labs

Page 27: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

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Cigarette Individual Weights; Repeatability Variation

Cochran’s test did not show any laboratories with exceptional variation.

Figure 16. Cigarette Individual Weights: z -score Plots

DCBMKJLIEHFGA

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Sample C1 Sample C2

Sample C3 Sample C4

Sample C5

Page 28: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

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Page 28 of 42

CIGARETTE CIRCUMFERENCE

Table 8. Cigarette Circumference Precision Statistics

Individual value plots for each sample are shown in Fig. 17. Individual data points are represented by open circles, and laboratory means by solid circles.

Mandel Plots

The h statistic Mandel Plots (Fig.18) shows that Laboratory L is significantly different for cigarette C5

The k statistic plot (Fig.19) identifies Laboratory A as significantly different for cigarette C3, and Laboratory L for cigarette C5.

Repeatability Variation

Cochran’s test shows Laboratory A cigarette C3, and Laboratory L, cigarette C5 as outliers, and Laboratory A cigarette C4 as straggler.

Z – scores

Results for Laboratory L, cigarette C5 (Fig.20) are highly questionable, results for Laboratory A cigarettes C1 and C2, are questionabel.

Laboratories with missing data points did not, or were unable to, measure the samples.

Cigarette Type Sample ID Mean sr sR r R CoV

SuperSlim C5 17.99 0.020 0.026 0.057 0.072 0.14

SuperSlim C4 18.02 0.024 0.027 0.066 0.076 0.15

Slim C3 21.45 0.022 0.046 0.063 0.129 0.21

KS C1 24.90 0.037 0.058 0.104 0.162 0.23

KS C2 24.92 0.040 0.051 1.588 0.143 0.21

Page 29: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

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Figure 17. Cigarette Circumference Individual Value Plots

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Sample_ID = C1 Sample_ID = C2

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Page 30: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

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Figure 18. Cigarette Circumference: h – statistics Mandel Plots

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Cigarette Circumference h Statistics - Labs within Samples

Cigarette Circumference h Statistics - Samples within Labs

Page 31: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

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Figure 19. Cigarette Circumference: k – statistics Mandel Plots

Lab C ode MLKJIHGFEDCBA

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Cigarette Circumference k -Statistics - Labs within Samples

Page 32: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

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Cigarette Circumference – Repeatability Variation

Laboratory A cigarette C3 and Laboratory L, cigarette C3 as outliers, and Laboratory A cigarette C4 as a straggler.

Figure 20. Cigarette Circumference: z -score Plots

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Plot of Z Score Cigarette C3 Plot of Z Score Cigarette C4

Plot of Z Score Cigarette C5

Page 33: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

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CIGARETTE PRESSURE DROP (OPEN)

Table 9. Cigarette Pressure Drop (Open) – Precision Statistics

The Individual values plots for cigarette pressure drop identified Laboratory C as different enough to distort the scale on the graphs. The plots were redrawn without these values (Fig.21).

Mandel Plots

The h statistic Mandel Plots (Fig.22) shows that Laboratory C is significantly different from the reference value, for all cigarettes except C3.

The k statistic plot (Fig.23) does not suggest exceptional variation for any single laboratory.

Repeatability Variation

Cochran’s test did not identify any outliers.

Z – scores

Laboratory C gave questionable results for cigarettes C1, C2, C4 and C5 (Fig.24). There were no questionable results for cigarette C3

Laboratories with missing data points did not, or were unable to, measure the samples.

Cigarette Type Sample ID Mean sr sR r R CoV

SuperSlim C5 88.8 1.40 2.95 3.92 8.26 3.32

SuperSlim C4 180.6 3.35 4.35 9.38 12.18 2.41

Slim C3 120.0 1.57 3.13 4.40 8.76 2.61

KS C1 120.3 1.48 3.18 4.14 8.90 2.64

KS C2 109.4 1.19 2.23 3.33 6.24 2.04

Page 34: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

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Figure 21. Cigarette Pressure Drop: Individual Value Plots

Labs N. I. P did not measure cig Pressure Drop, Lab C results removed from individual value plots.

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Page 35: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

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Figure 22. Cigarette Pressure Drop: h – statistics Mandel Plots

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Pressure Drop (open) h statistics - Labs within Samples

Pressure Drop (open) h statistics - Samples within Labs

Page 36: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

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Figure 23. Cigarette Pressure Drop: k – statistics Mandel Plots

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Pressure Drop (open) k statistics - Labs within Samples

Page 37: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

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Cigarette Pressure Drop (open) – Repeatability Variation: Cochran’s Test

Cochran’s test identified Labs B and C as stragglers for sample C5. There were no unusual results for the other 4 samples

Figure 24. Cigarette Pressure Drop: z - score Plots

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Cig C1 Cig C2

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Page 38: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

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CIGARETTE VENTILATION

Table 10. Cigarette Ventilation: Precision Statistics

The Individual values plots for cigarette pressure drop identified Laboratory C as different enough to distort the scale on the graphs. The plots were redrawn without these values (Fig.25).

Mandel Plots

Laboratory C was excluded from the Mandel plotsbecause of distortion of the graphs.

The h statistic Mandel Plots (Fig.26) shows that Laboratory B is significantly different from the reference value, for cigarettes C4 and C5. Laboratories A and B, in general, show a greater deviation form the reference values

The k statistic plot (Fig.27) does not shows any exceptional variation

Repeatability Variation

Cochran’s test did not suggest any exceptional variation.

Z – scores

Results for Laboratory C (Fig.28) are highly questionable for C1, C2 , C3 and C4, and questionable for C5.

Results for Laboratory A , cigarette C2 are questionable.

Results for Laboratory B cigarette C4 are questionable.

Laboratories with missing data points did not, or were unable to, measure the samples, or had extreme values which distorted the plots.

Cigarette Type Sample ID Mean sr sR r R CoV

SuperSlim C5 81.4 0.394 0.498 1.103 1.394 0.61

SuperSlim C4 44.9 0.643 0.938 1.800 2.626 2.09

Slim C3 41.8 0.334 0.428 0.935 1.198 1.02

KS C2 27.8 0.567 0.861 1.588 2.411 3.09

KS C1 18.9 0.399 0.573 1.117 1.604 3.03

Page 39: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

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Figure 25. Cigarette Ventilation: Individual Value Plots

Laboratory C excluded from graphs because of wildly different results.

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Page 40: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

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Figure 26. Cigarette Ventilation: h – statistics Mandel Plots

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Ventilation h Statistic - Samples within Labs

Page 41: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

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Figure 27. Cigarette Ventilation: k – statistics Mandel Plots

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Ventilation k Statistic - Samples within Labs

Page 42: MMPTM Proficiency Test 2009(2) · Product Research Division, Japan Tobacco Inc., JT Sumida Building, 17-7, Yokogawa 1-chome, Sumida-ku, Tokyo 130-8603, Japan JT International Germany

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Cigarette Ventilation: Repeatability Variation

All results were acceptable using Cochran’s test.

Figure 28. Cigarette Ventilation: z –score Plots

1 ISO/IEC Guide 43 – 1: 1997: Proficiency testing by interlaboratory comparisons – Part 1:

Development and operation of proficiency testing schemes

2 ISO/IEC 17025: 2005 General requirements for establishing the competence of calibration and

testing laboratories

3 ISO 5725 – 2 Accuracy (trueness and precision) of measurement methods and results — Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method

4 ibid.

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Plot of C1 Z Scores Plot of C2 Z Scores

Plot of C3 Z Scores Plot of C4 Z Scores

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