Page 1
1 of 57
E-Vapour Sub-Group
Technical Report
2014 Preliminary Aerosol Proficiency Study
October 2017
Sub-Group Coordinator:
Chuck Garner, Ph.D., R.J. Reynolds, U.S.A.
Sub-Group Secretary:
Gene Gillman, Ph.D., Enthalpy Analytical, U.S.A.
Authors:
Steve Alderman, Ph.D., R.J. Reynolds
Robert D. Stevens, Ph.D. & Rana Tayyarah, ITG Brands, LLC, U.S.A.
Statistician:
Walt Morgan, M.S., R.J. Reynolds, U.S.A.
Page 2
Table of Contents
Summary ....................................................................................................................... 3 1.
Introduction ................................................................................................................... 3 2.
Organisation .................................................................................................................. 4 3.
3.1 Participants ........................................................................................................... 4
3.2 Protocol ................................................................................................................ 4
3.3 Deviations from Protocol ...................................................................................... 5
Data - Raw ..................................................................................................................... 5 4.
Data - Statistical Analysis .............................................................................................. 6 5.
5.1 Exclusion of Outliers ............................................................................................ 6
5.2 Calculation of r & R ............................................................................................. 7
Data Interpretation ....................................................................................................... 11 6.
6.1 Aerosol Collection .............................................................................................. 11
6.2 Methods Comparison .......................................................................................... 11
6.3 Reporting Units .................................................................................................. 11
6.4 Lab to Lab Consistency ...................................................................................... 12
Recommendations........................................................................................................ 12 7.
Acknowledgements ...................................................................................................... 12 8.
Appendix A: Study Protocol and Data Template .................................................................. 13
Appendix B: Laboratory Method Summaries ....................................................................... 27
Appendix C: Raw Data ........................................................................................................ 31
Appendix D: Raw Data Plots ............................................................................................... 43
Appendix E. Mandel Charts ................................................................................................. 48
Page 3
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 3/65
Summary 1.
In 2014, the CORESTA E-cigarette Task Force, now known as the E-Vapour Sub- Group,
conducted a preliminary proficiency study to determine the inter-lab variability for the
quantification of the major constituents of e-cigarette aerosol using specified puffing
parameters of a 55 mL puff volume, a 3 second puff duration, a 30 second puff interval, and a
square puff profile. Fourteen laboratories from 7 different countries participated in this
proficiency study to evaluate aerosol generated from a common pool of e-cigarette products
(4 disposable and 4 rechargeable). The study included determination of puff count, trapped
aerosol, nicotine, propylene glycol (PG), glycerin and water. The test methods used for
quantification of specific analytes were left to the discretion of participating laboratories. The
laboratory testing phase of this study was completed in August-September 2014 and the
results were presented to the Task Force in October 2014.
The study results demonstrated that aerosol delivery for the study samples was relatively
variable and that the analyte deliveries for a given product tended to be proportional to
Aerosol Collected Mass (ACM) deliveries. Evaluation of analyte results normalized to ACM
delivery yielded acceptable r&R values. Based on these results, a follow-up study was
recommended and conducted in 2015 which resulted in CORESTA Recommended Method
No. 84.
Introduction 2.
At the time of this study, one of the objectives of the CORESTA E-cigarette Task Force was
“…to gather and share preliminary data on analysis relevant to e-cigarettes worldwide with a
view to making recommendations for product testing”. While there are no standardized
methods for analysis of nicotine, propylene glycol, glycerin, and water in e-liquids and
e-cigarette aerosols, the task force has initiated multiple preliminary proficiency studies to
prepare for future collaborative studies. Between November 2013 and May 2014, the Task
Force completed two proficiency studies to determine: (1) Major constituents in e-liquids and
(2) Puffing parameters for e-cigarette aerosol collection. Building on that experience, a
proficiency study was commissioned in May 2014 to quantify the major constituents in
e-cigarette aerosols using a common puffing profile, i.e. 55/3/30/square puff profile. A total
of eight “cigalike” e-cigarette products were evaluated by the participating laboratories using
analytical test methods. The results from puff count, trapped aerosol, nicotine, propylene
glycol, glycerin, and water were compared between the laboratories and the results are
presented in this document.
Page 4
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 4/57
Organisation 3.
3.1 Participants
A list of the participating laboratories is provided in Table 1. The laboratories are listed in the
alphabetical order. The laboratory codes used in this report do not correspond to the same
order as the list below.
Table 1. List of Participating Laboratories
Laboratory
Altria Client Services
Arista Laboratories
British American Tobacco
Enthalpy Analytical, Inc.
Global Laboratory Services
Japan Tobacco
Japan Tobacco International UK
Labstat International ULC
Liggett Tobacco Co.
Lorillard Tobacco Co.
Philip Morris International
R.J. Reynolds Tobacco Co.
Vivotecnia
Zhengzhou Tobacco Research Institute
3.2 Protocol
Commercial e-cigarette products were provided to each participating laboratory. Sufficient
products for the study along with batteries and USB chargers, as appropriate, were provided
by product suppliers listed in Table 2. Additional information about the products is listed in
Table 3. Samples were stored at room temperature in original packaging until time of use.
Rechargeable devices were fully charged before use. A single battery charge was used for
each new cartomizer.
Aerosol was collected in 50-puff puffing increments onto Cambridge filter pads. Each unit
was weighed before beginning collection and between each puffing increment to determine
device mass loss. The filter pads were weighed before and after collection to determine
aerosol collected mass (ACM). Collection was terminated when: 1) LED indications made it
clear that the disposable product has reached end of life, 2) LED indications made it clear that
a rechargeable product has completed one charge cycle, or 3) ACM collected for a complete
group of 50 puffs fell below 12.5 mg.
Page 5
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 5/57
The amount of nicotine, propylene glycol, glycerin, and water per sample was determined by
the method currently in use in each laboratory and recorded as mg/pad in the data template.
See Appendix A for the study protocol.
Table 2. List of Product Suppliers
Product Suppliers
Imperial Tobacco
Lorillard Tobacco Company
National Tobacco
Red Kiwi
White Cloud
Table 3. Sample Descriptions
Sample ID Device Type Nicotine Level Flavor
1 Disposable 1.6 % Classic Tobacco
2 Disposable 1.6 % Original
3 Rechargeable 1.6 % Original
4 Disposable 1.8 % Red Tobacco
5 Rechargeable 1.8 % Red Tobacco
6a Disposable 2.4 % Apache or Regular Full Nicotine
6b Disposable 1.2 % Apache or Regular Light Nicotine
7 Rechargeable 2.4 % Exotic Tobacco
8 Rechargeable 1.8 % Nevada Tobacco
Note: The labs received either product 6a or 6b, not both.
3.3 Deviations from protocol
Know deviations from the study protocol are described briefly. Product 6 was not a single lot
of one product but two distinct sub-samples (6a and 6b). Lab B reported results for only
3 replicates, rather than 5, for each test product. Lab I did not evaluate Product 1.
Laboratories 2 and 10 did not provide water data.
Data - Raw 4.
The raw data are displayed in Appendix C and Appendix D.
Missing values for replicates indicate non-reporting by the laboratory due to issues with
analysis or based on the deviations noted above. Product 6 was excluded from the analysis
since there were two distinct sub-samples (6a and 6b).
Page 6
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 6/57
Data - Statistical Analysis 5.
A statistical analysis was conducted following the recommendations given in ISO 5725-2.
This analysis was conducted on complete e-cigarette yields (i.e. yields summed across 50 puff
blocks and analyte per cent of ACM calculated from them) A summary of the results from
outlier detection and the calculated results for repeatability (r) and reproducibility (R) are
given in sections 5.1 and 5.2, respectively. The focus of ISO 5725-2 is to determine the
variation to be expected in measurements made by laboratories following a standard test
method. For this study each lab followed its own test methods for measurements of
e-cigarette yields rather than a standard test method. However, this analysis does provide
information on the current levels of e-cigarette yields and uncertainty that underlie values that
may be reported in future e-cigarette yield studies. The two main parts of the ISO 5725-2
analysis are:
1. Exclusion of data from laboratories whose mean level or standard deviation for a test
sample is inconsistent with those of the other laboratories
2. Estimation of test sample means, within-lab variability (repeatability) and between-lab
variability (reproducibility)
5.1 Exclusion of outliers
Graphical outlier detection was performed following the recommendations of ISO 5725-2.
MANDEL’s h is used to assess the inter-laboratory consistency and MANDEL’s k is used to
assess the intra-laboratory consistency. Both MANDEL’s h and MANDEL’s k plots use the
0.95 straggling and 0.99 outlying limits. The MANDEL’s h plots and the MANDEL’s k plots
are shown in Appendix E.
Outlier laboratories were identified first through evaluation of normalized laboratory means
and within-lab standard deviation across all the test samples with Mandel h and k charts (for
lab means and standard deviations, respectively). In these charts, horizontal lines associated
with p-values of 0.05 and 0.01 indicate laboratory means and standard deviations different
from the group as a whole. These charts are reviewed to determine if any lab is consistently
different from the rest to the extent that all data should be excluded for that endpoint.
According to ISO 5725-2, this is a subjective evaluation to be made by the statistician
analyzing the data.
After results from any lab judged to be different from the rest have been removed, an iterative
evaluation of results for each laboratory for each test sample is conducted. In each iteration,
Cochran’s test for outlier standard deviations is conducted, followed by Grubb’s test for
outlier means. The laboratory with the largest within-lab standard deviation is designated a
“standard deviation outlier” if the Cochran test statistic exceeds the 0.01 critical value, and a
“standard deviation straggler” if the Cochran test statistic exceeds the 0.05 critical value.
Data from “outlier” laboratories are removed from the data set but data from “straggler”
laboratories are not. If a laboratory is excluded as a standard deviation outlier, then the next
iteration begins with Cochran’s test for the reduced data set. If not, Grubbs’ test for the mean
is conducted. It includes tests for a single mean and also tests for outlier pairs of means. The
test for outlier pairs allows for detection of two mean outlier laboratories that differ from the
rest, since each of those laboratories would prevent identification of the other as an outlier. A
laboratory whose test statistic exceeds the 0.01 critical values is designated a “mean outlier”,
while a laboratory whose test statistic exceeds the 0.05 critical value is a “mean straggler”.
Again, data from “outlier” laboratories are removed from the data set but data from
“straggler” laboratories are not. Note that with this iterative approach, outlier labs that would
Page 7
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 7/57
be “masked” by a more extreme outlier can be identified (particularly for standard deviation
outliers). This is not the case with the Mandel charts, which look only at the data for all
laboratories as a group. ISO 5725-2 specifies that data from at most 2/9 of participating
laboratories can be excluded as “outliers” through this process. With 9-13 participating
laboratories, data from up to two laboratories can be excluded, but with 14 participating
laboratories, data from up to three laboratories can be excluded.
5.1.1 Outlier lab analysis with Cochran’s test and Grubb’s test:
Overall, more standard deviation outliers were identified than mean outliers. Table 4 shows
the number of laboratories (out of 14) for which data was used to estimate test sample means,
standard deviations, repeatability, and reproducibility. More standard deviation outliers were
noted for measures expressed as per cent of ACM because variation in ACM yields increased
the variation among individual e-cigarettes.
Table 4. Number of Laboratories with Data Used in Calculations of Test Sample Mean,
Repeatability, and Reproducibility
Measurement Product
1
Product
2
Product
3
Product
4
Product
5
Product
7
Product
8
Total Puffs 12 12 12 13 12 12 11
Total ACM, mg 12 13 13 13 13 13 12
Total PG, mg 11 13 14 14 14 14 14
PG, % of ACM 11 13 11 11 12 13 14
Total Glycerin 12 12 13 12 13 13 12
Glycerin, % of ACM 12 11 12 11 11 13 11
Total Nicotine, mg 12 14 14 14 14 14 13
Nicotine, % of ACM 12 11 11 11 12 11 11
Total Water, mg 11 10 11 12 12 12 11
Water, % of ACM 10 10 10 11 12 12 11
5.2 Calculation of r & R
After removal of outlying data based on numerical data consistency methods (GRUBBS’ test,
COCHRAN’s test), the final repeatability (r) and reproducibility (R) results were calculated.
These calculations are specified in ISO 5725-2 and make allowances for circumstances where
unequal numbers of replicate measurements are reported by different laboratories. These
variance components are used to estimate within-lab standard deviation (the standard
deviation among repeated measurements at the same laboratory) and between-lab standard
deviation (the standard deviation among repeated measurements at different laboratories), and
their associated repeatability and reproducibility. The r&R results are shown in Tables 5 - 14.
Page 8
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 8/57
Table 5. Estimates of test sample mean, standard deviations and repeatability and
reproducibility for total puffs.
Total Puffs No. of Labs Mean r R %r %R rSD RSD
Product1 12 290.9 20.1 30.1 7 % 10 % 7.17 10.75
Product2 12 314 19.7 43.2 6 % 14 % 7.03 15.43
Product3 12 401.4 28.9 52.4 7 % 13 % 10.31 18.70
Product4 13 194.5 31.4 38.4 16 % 20 % 11.22 13.73
Product5 12 197.4 24.6 42.4 12 % 21 % 8.77 15.14
Product7 12 265 51 56.6 19 % 21 % 18.23 20.20
Product8 11 195.5 19 66.8 10 % 34 % 6.8 23.84
Average -- -- -- -- 11 % 19 % -- --
Table 6. Estimates of test sample mean, standard deviations and repeatability and
reproducibility for total ACM.
Total ACM mg
No. of Labs
Mean r R %r %R rSD RSD
Product1 12 606.2 184.1 184.1 30 % 30 % 65.74 65.74
Product2 13 547.8 173.4 179.3 32 % 33 % 61.94 64.04
Product3 13 678.7 317.8 317.8 47 % 47 % 113.5 113.5
Product4 13 592.5 195.4 195.4 33 % 33 % 69.80 69.80
Product5 13 644.5 192.2 201.1 30 % 31 % 68.65 71.81
Product7 13 796.3 279.1 279.1 35 % 35 % 99.67 99.67
Product8 12 668.7 146.2 150 22 % 22 % 52.2 53.58
Average -- -- -- -- 33 % 33 % -- --
Table 7. Estimates of test sample mean, standard deviations and repeatability and
reproducibility for total PG.
Total PG
mg
No. of
Labs Mean r R %r %R rSD RSD
Product1 11 0.402 0.463 2.99 -- -- 0.166 1.066
Product2 13 298 108 114 36 % 38 % 38.7 40.6
Product3 14 362 191 204 53 % 56 % 68.3 72.7
Product4 14 351 120 120 34 % 34 % 42.7 42.7
Product5 14 384 115 157 30 % 41 % 41 56.1
Product7 14 427 165 178 39 % 42 % 58.9 63.7
Product8 14 326 79 149 24 % 46 % 28.3 53.3
Average -- -- -- -- 36 % 43 % -- --
Page 9
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 9/57
Table 8. Estimates of test sample mean, standard deviations and repeatability and
reproducibility for %PG.
PG % of ACM
No. of Labs
Mean r R %r %R rSD RSD
Product1 11 0.069 0.069 0.51 0.025 0.183
Product2 13 55.8 3.16 7.15 6 % 13 % 1.13 2.55
Product3 11 55.3 3.3 5.66 6 % 10 % 1.18 2.02
Product4 11 59.4 3.3 7.47 6 % 13 % 1.18 2.67
Product5 12 61.2 4.41 11.21 7 % 18 % 1.57 4
Product7 13 53.7 3.69 12.06 7 % 22 % 1.32 4.31
Product8 14 50.8 4.67 11.95 9 % 24 % 1.67 4.27
Average -- -- -- -- 7 % 17 % -- --
Table 9. Estimates of test sample mean, standard deviations and repeatability and
reproducibility for total Glycerin.
Total Glycerin mg
No. of Labs
Mean
r R %r %R rSD RSD
Product1 12 488 153 156 31 % 32 % 54.7 55.8
Product2 12 152 48.3 54.4 32 % 36 % 17.2 19.4
Product3 13 183 84 92.7 46 % 51 % 30.0 33.1
Product4 12 109 35.6 35.6 33 % 33 % 12.7 12.7
Product5 13 121 31.7 61.2 26 % 51 % 11.3 21.9
Product7 13 203 70.2 75.4 35 % 37 % 25.1 26.9
Product8 12 175 39.3 89.1 22 % 51 % 14.0 31.8
Average -- -- -- -- 32 % 41 % -- --
Table 10. Estimates of test sample mean, standard deviations and repeatability and
reproducibility for %Glycerin.
Glycerin
% of ACM
No. of
Labs Mean r R %r %R rSD RSD
Product1 12 80.4 4.16 9.74 5 % 12 % 1.49 3.48
Product2 11 28.6 1.18 3.04 4 % 11 % 0.42 1.09
Product3 12 27.5 1.72 4.84 6 % 18 % 0.62 1.73
Product4 11 18.3 1.28 1.73 7 % 9 % 0.46 0.62
Product5 11 18.5 1.57 2.54 8 % 14 % 0.56 0.91
Product7 13 25.5 2.2 5.33 9 % 21 % 0.78 1.9
Product8 11 26.9 2.14 8.93 8 % 33 % 0.77 3.19
Average -- -- -- -- 7 % 17 % -- --
Page 10
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 10/57
Table 11. Estimates of test sample mean, standard deviations and repeatability and
reproducibility for total Nicotine.
Total Nicotine mg
No. of Labs
Mean r R %r %R rSD RSD
Product1 12 8.92 2.96 3.12 33 % 35 % 1.06 1.12
Product2 14 7.36 2.49 4.09 34 % 56 % 0.89 1.46
Product3 14 8.94 4.39 5.21 49 % 58 % 1.57 1.86
Product4 14 7.12 2.43 2.86 34 % 40 % 0.87 1.02
Product5 14 7.81 2.38 3.39 30 % 43 % 0.85 1.21
Product7 14 15.21 5.69 6.66 37 % 44 % 2.03 2.38
Product8 13 8.23 2.01 2.62 24 % 32 % 0.72 0.93
Average -- -- -- -- 35 % 44 % -- --
Table 12. Estimates of test sample mean, standard deviations and repeatability and
reproducibility for % Nicotine.
Nicotine % of ACM
No. of Labs
Mean r R %r %R rSD RSD
Product1 12 1.47 0.12 0.276 8 % 19 % 0.043 0.098
Product2 11 1.35 0.065 0.212 5 % 16 % 0.023 0.076
Product3 11 1.33 0.117 0.349 9 % 26 % 0.042 0.125
Product4 11 1.19 0.08 0.211 7 % 18 % 0.029 0.075
Product5 12 1.24 0.103 0.199 8 % 16 % 0.037 0.071
Product7 11 1.88 0.075 0.367 4 % 20 % 0.027 0.131
Product8 11 1.26 0.065 0.152 5 % 12 % 0.023 0.054
Average -- -- -- -- 7 % 18 % -- --
Table 13. Estimates of test sample mean, standard deviations and repeatability and
reproducibility for total water.
Total Water
mg
No. of
Labs Mean r R %r %R rSD RSD
Product1 11 94.8 26.3 37.2 28 % 39 % 9.38 13.27
Product2 10 64.2 15.3 24.7 24 % 38 % 5.47 8.81
Product3 11 89.7 33.1 53.9 37 % 60 % 11.82 19.24
Product4 12 98.2 31.4 32.8 32 % 33 % 11.23 11.72
Product5 12 89.1 29.9 36.2 34 % 41 % 10.67 12.93
Product7 12 98.2 31.7 39.4 32 % 40 % 11.33 14.07
Product8 11 107.3 22.7 29.3 21 % 27 % 8.10 10.46
Average -- -- -- -- 30 % 40 % -- --
Page 11
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 11/57
Table 14. Estimates of test sample mean, standard deviations and repeatability and
reproducibility for %water.
Water
% of ACM
No. of Labs
Mean r R %r %R rSD RSD
Product1 10 15.7 1.75 3.67 11 % 23 % 0.63 1.31
Product2 10 11.7 1.64 3.91 14 % 33 % 0.59 1.4
Product3 10 12.8 2.42 5.71 19 % 45 % 0.87 2.04
Product4 11 16.3 2.26 3.45 14 % 21 % 0.81 1.23
Product5 12 13.9 4.62 5.27 33 % 38 % 1.65 1.88
Product7 12 12.4 1.49 3.03 12 % 24 % 0.53 1.08
Product8 11 16.2 1.67 3.35 10 % 21 % 0.60 1.2
Average -- -- -- -- 16 % 29 % -- --
Data Interpretation 6.
6.1 Aerosol collection
Aerosol collection can serve as an indicator of overall performance for the test session and the
devices tested. Aerosol collection was conducted under the puffing parameters specified in
CRM N° 811 and is determined gravimetrically. Simultaneous determination of device mass
loss is complementary in that the device loss and the trapping media uptake should be
approximately the same. Significant differences in these values can indicate experimental
error. Typically Device Weight loss and ACM yields were comparable. This indicates that
there was no significant loss of aerosol due to collection.
6.2 Methods comparison
Although laboratories were not provided with standardized methods for use with the study,
most aspects of the methodologies used were very similar. All laboratories used GC-FID for
analysis of nicotine, PG and glycerin. Most laboratories used GC-TCD for water analysis.
All laboratories used an alcohol solvent, such as isopropanol or ethanol, for dilution.
Differences included analytical column phase, dilution scheme, shake time, and the choice of
internal standard (e.g. anethole, octadecane, quinoline and methanol).
6.3 Reporting units
For studies intended to quantify device deliveries of the major aerosol constituents, reporting
analyte concentration on an absolute basis may be preferable, e.g. mg of nicotine per puff or
mg of nicotine per puff block. However, when performing an inter-laboratory study such as
that reported here, analyte yields should be normalized as a percentage or fraction of the
gravimetrically determined ACM. This takes into account the stick-to-stick variability in
ACM yields, which in turn significantly improve the r&R values reported here.
1 CORESTA Recommended Method No. 81 - Routine Analytical Machine for E-Cigarette Aerosol Generation
and Collection - Definitions and Standard Conditions, Issued June 2015
Page 12
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 12/57
Another consideration is that reporting yields normalized per puff will only be relevant if all
puffs actively produced aerosol. It was clear that some laboratories continued to take puffs
from the product beyond cartridge and/or battery depletion; after aerosol delivery ceased.
Thus, per puff values are less accurate a calculation for the last puff set(s) for a segmented
collection scheme.
6.4 Lab to lab consistency
ACM %r and %R are largely influenced by natural product variability. In order to understand
the variability of the analytical methods for the laboratories analyte %r and %R values were
calculated using ACM-normalized yields. A comparison of r&R values (summarized below
in Table 15), indicate high consistency of reported results among the laboratories.
Table 15. Estimated per cent repeatability and reproducibility values averaged across all
study products
%r %R
Total ACM, mg 33 % 33 %
PG, % of ACM 7 % 17 %
Glycerin, % of ACM 7 % 17 %
Nicotine, % of ACM 7 % 18 %
Water, % of ACM 16 % 29 %
Recommendations 7.
Results of this study were presented to the E-cigarette Task Force at the October 2014
meeting. The group was in agreement that the r&R values were acceptable and that continued
work to develop a CRM for analytical methodology was warranted. See the technical report
for “2015 Collaborative Study for Determination of Glycerin, Propylene Glycol, Water and
Nicotine in Collected Aerosol of E-Cigarettes” 2
for discussion of this follow-up study.
Acknowledgements 8.
The participating laboratories and the product suppliers that provided the e-cigarettes for
testing are greatly appreciated.
2 Issued March 2017
Page 13
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 13/57
Appendix A: Study Protocol and Data Template
CORESTA E-CIGARETTE ANALYTICAL TESTING SUB TEAM
Project Title: 2014 Preliminary Aerosol Proficiency Study: Major Constituents
Type of Document: Protocol
Team Leader Dr. Rob Stevens, (Lorillard Tobacco)
Date: June 09, 2014
Written by: Steven L. Alderman, Ph.D. (R.J.Reynolds)
Confidentiality Notice: All data generated in the course of this analysis should be handled
in the strictest of confidence by all participating laboratories and other Task Force
members.
Page 14
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 14/57
Study Protocol to Determine Inter-Laboratory Proficiency for the Quantification of the
Major Constituents in E-Cigarette
1. Objective
The main objective of this study is to examine inter-lab variability for the quantification of
the major constituents of e-cigarette aerosols. A common puffing profile, i.e. 55/30/3
square-wave, will be employed by all participating laboratories to generate aerosol from a
common pool of test products. The test methods used for quantification of specific analytes
will be left to the discretion of participating laboratories.
2. Study coordinator
Dr. Robert Stevens
Director, R&D Testing Services
Lorillard Tobacco Company, R&D
420 N. English Street
P.O. Box 21688
Greensboro, N.C. 27420-1688
Bus. (336) 335-6791
FAX (336) 335-6640
E-mail: [email protected]
3. Methods
3.1 Test products
A total of eight e-cigarette types will be provided to each laboratory and will include four
disposable products and four rechargeable products. Each laboratory will receive sufficient
product to initiate collection of five replicates for each e-cigarette type. See Table 1 for
additional information on e-cigarette products shipped to the participating laboratories.
3.2 Data resolution and puff count
Aerosol should be collected in 50 puff increments (puff groups), e.g. puffs 1-50 will be
collected on a single Cambridge pad and subjected to analysis, puffs 51-100 will be collected
on a second Cambridge pad and subjected to analysis, and so on. Although the target puff
count for each pad is 50, there will be instances where the puff count per pad varies, e.g. the
e-cigarette signals that end of life has been reached prior to completion of the current
sampling increment. Thus, actual puff count per pad should be reported.
A maximum puff count limit will not be assigned for this study. Aerosol collection should be
terminated when: 1) LED indications make it clear that the disposable product has reached
end of life, 2) LED indications make it clear that a rechargeable product has completed one
charge cycle, or 3) the total particulate matter (ACM) collected for a complete group of 50
puffs falls below 12.5 mg (0.25 mg ACM per puff).
3.3 Aerosol total particulate matter collection
The ACM for each sample will be determined gravimetrically by measuring the trapping
system before and after each collection event. The total amount of aerosol collected will be
determined by difference in mass (pad mass after collection – pad mass before collection).
Record ACM values as mg/pad in the data template, along with puff count per pad.
Page 15
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 15/57
3.4 E-cigarette mass loss
The amount of material lost from each e-cigarette will be determined by measuring the e-
cigarette mass just prior to the start aerosol collection and after each collection event (puff
group). The e-cigarette mass after collection of a puff group will be the starting e-cigarette
weight for the beginning of each subsequent puff group. Record mass loss as mg in the data
template. Puff count for e-cigarette mass loss should match the puff group for each ACM
collection event described above.
3.5 Sample handling
All samples should be stored at room temperature. Rechargeable devices should be fully
charged before use. A single battery charge will be used for each new cartomizer.
4. Analytes
4.1 Propylene Glycol
The amount of propylene glycol per sample will be determined by the method currently in use
in each laboratory. Record as mg/pad in the data template.
4.2 Nicotine
The amount of nicotine per sample will be determined by the method currently in use in each
laboratory. Record as mg/pad in the data template.
4.3 Glycerin
The amount of glycerin per sample will be determined by the method currently in use in each
laboratory. Record as mg/pad in the data template.
4.4 Water
The amount of water per sample will be determined by the method currently in use in each
laboratory. Record as mg/pad in the data template.
5. Experimental Plan
5.1 Sample preparation
All products should be stored at room temperature and remain in their original packaging until
testing is initiated. Each rechargeable battery should be fully charged according to
manufacturer instructions. Manufacturers will provide USB chargers specific for their
product. USB wall chargers (AC to USB adapters) may be provided, but if not, laboratories
may utilize any appropriate adapter.
5.2 Puffing regimen
All ACM collection should be carried out using a 55 mL puff volume, 3 second puff duration,
and 30 second inter-puff interval using a square wave puff profile. This is essentially
equivalent to a constant flow rate puff of 18.3 mL/s. This protocol does not specify room
conditions, although these parameters should be reported.
5.3 Replicates and puff count determination
Five replicates for each e-cigarette under each test condition is recommended. If a defective
product is encountered, that product should be removed from the test pool. Provided that at
least three replicates are successfully collected, the laboratory should report data for that
particular product. If less than three replicates are successfully collected, please contact
Naren Meruva [email protected] regarding the possibility of procuring
replacement product.
Page 16
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 16/57
It is expected that the puff count required to consume a disposable e-cigarettes, or to fully
exhaust a single battery charge for the rechargeable products will be variable, not only across
brand styles, but even for individual replicates for a common brand style. Thus, the e-
cigarettes will need to be carefully observed during testing so that that the correct number of
puffs required to deplete the products may be recorded. Generally, LED signals indicate
when a disposable product has been consumed, or a battery requires recharging, e.g. flashing
signals or absence of signal. Manufacturers will provide information specific to their product
to assist determination of end of life puff count. Furthermore, once it has been determined
that end of life has been reached, the aerosol trapping mechanism, e.g. Cambridge pad
holder, should be removed from the smoking machine as exposure to “blank” puffs could lead
to evaporation of pre-deposited material. Also recall from above that sampling of a given
replicate should be terminated if the total ACM catch for 50 cumulative puffs falls below12.5
mg.
5.4 Additional data collection and observations
Laboratories are asked to provide some detail on test methods employed, types of smoking
machine used, aerosol collection methodology, and any unusual or otherwise critical
observations noted during sample collection. The information should be provided in the
indicated cells on the data collection spreadsheet.
6. Data Submission
The attached template should be used for data submission. Please supply data in the
requested format without creating new cells or rows in the spreadsheet.
Results should be reported back to Rana Tayyarah [email protected] and Steve
Alderman [email protected] on or before August 29, 2014 in order to allow sufficient time
to evaluate the data.
7. Data Analysis
The data will be analyzed statistically according to ISO 57025.
8. Time Schedule
June-July 2014
Study protocol, reporting template and samples will be distributed to participating
laboratories
July-August 2014
Laboratories will perform the study
August 2014
The results must be sent to the data coordinator on or before Aug 29th
, 2014 in order to give
the statistician sufficient time to evaluate the data. Data received after Aug 29th
, will not be
included in the draft report discussed at the next Task Force meeting.
September 2014
The statistician will perform the data analysis and the Task Force coordinators will format the
data for presentation.
October 2014
The Task Force coordinators will assess and share the results of the collaborative study during
the Oct 12th
, 2014 CORESTA E-cigarette Task Force meeting.
Page 17
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 17/57
Table 1. E-cigarette product information sheet.
Sam
ple No.
Brand Device
Type
Nicoti
ne Level
Flavors
No. of
Devices Shipped
No. of USB
Chargers Shipped
Estimated No. of
50-Puff Collectio
ns
Estima
ted Total Puffs
1 Blu Disposable 1.6 % Classic Tobacco 6 N/A 6 300
2 Puritan
e Disposable 1.6 % Original
5 N/A 6.4 321
3 Puritan
e
Rechargea
ble 1.6 % Original
5 3 8.6 430
4 V2 Disposable 1.8 % Red Tobacco 6 N/A 4.2 209
5 V2 Rechargea
ble 1.8 % Red Tobacco
10 10 4.9 246
6a Fling Disposable 2.4 %
Apache or
Regular Full Nicotine
5 N/A 4.6 232
6b Fling Disposable 1.2 %
Apache or Regular Light
Nicotine
5 N/A 4.6 232
7 Bora
Bora
Rechargea
ble 2.4 % Exotic Tobacco
5 5 6.2 312
8 EasyCl
ick
Rechargea
ble 1.8 %
Nevada
Tobacco
5 3 4.4 221
Note:
1. The labs will receive product 6a or 6b, not both.
2. All cartridges with sample 2 and 3 have 1.6 % nicotine loading and not 1.1 % nicotine as
stated on the packaging.
3. The above estimates for total puff count and number of 50-puff collections for the e-
cigarette products were determined by smoking a single device and may vary significantly
from device to device for the same brand.
Page 18
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 18/57
Data Sheet for 2014 Aerosol Proficiency Study
Laboratory name
Company Representative (Title, Name)
Address
Tel
Fax
E-mail address
Note: Please don't modify formatted data sheet for the convenience of data analyses.
Note: Laboratory names will not be used for reporting. All labs will be coded. Each
lab will know their own code.
Note: In this spreadsheet, cells that are shaded blue require input. Cells that are not
shaded are calculations or information and should not be edited.
Page 19
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 19/57
Data Entry Instructions:
Notes Relevant Cells
1. This spreadsheet contains 8 data entry worksheets - one for each of the 8 products to be tested. Replicate data for a single product type will be entered within a single worksheet. Worksheets are also provided to capture laboratory contact
information, method information, and chromatogram images
Product and replicate ID - rows (3,4),(20,21),(37,38),(54,55), (71,72)
2. The spreadsheet is configured with the assumption that no disposable product or rechargeable battery will last for more than 600 puffs. Please contact the study sponsors if this is found not to be the case. Leave cells for which no ACM or aerosol former data is recorded blank (do not insert 0s)
NA
2. ACM calculations and e-cigarette mass loss calculations for each collection event (puff group) are not performed by this spreadsheet. Laboratories are asked to calculate those values
using their own methods and copy/paste values data here.
Puff group identifier - column B Puff group ACM mass - column D E-cigarette
mass loss - column E
3. Laboratories will insert data obtained from aerosol analyses of propylene glycol (PG), glycerin (GLY), nicotine (NIC), and water (WAT). These data will be reported on a mg per sample (mg per puff group) basis, along with puff count for that puff group.
PG - column F, GLY - column G NIC - column H, WAT - column I Puff count - column C
4. Some calculations are performed by this spreadsheet that will help ensure data quality. These include mass sum of the 4 components quantified, the ratio of this analyte sum to ACM, and the ratio of e-cig mass loss to ACM. Generally, the latter two ratios are expected to yield values of 1.0 ± 0.1. However, if a major aerosol constituent is present that is not PG or GLY, the ACM to analyte sum ratio could fall outside this range. Similarly, an e-cig mass loss to ACM collected ratio that differs significantly from the expected 1:1 ratio could indicate and
aerosol trapping efficiency issue.
Analyte Sum - column J Analyte sum:ACM - column K E-cig mass loss to ACM - column L
5. Other relevant information will be provided in the indicated cells.
Columns N and O
Page 20
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 20/57
Lab
Method Synopsis: please type an overall summary of your method in this box and provide specific details below
Method Details (example) ACM Nicotine Water Glycerin PG
Sample Handling
Storage prior to testing
unopened at 65 % RH 72F
Additional Details
Type of Aerosol Collection Machine
Style (Include a description of features if non-standard equipment
was used)
Linear Smoking
Machine
Make Cerulean
SM450
Vaping was Concurent for Which
analytes?
All were
concurrent
Room Conditions during aerosol
collection
65 %RH, 72F
Additional Details for Aerosol Collection
Trapping System
Filter Pad / Diameter CFP 44 mm
Were filter pads
conditioned?
Yes, 62+/-
%RH, 75F
Trap Type + Number of Traps
Fritted Impinger
Solvent 20 mL MeOH (sub-ambient)
Extraction wrist-action
shaker, 30min
Additional Filtration PTFE: 0.45um
Additional sample processing prior to
analysis
extracts were diluted 1:2 for
Gly/PG
Additional Details
extracts analyzed same day for Nic/Water next day for Gly/PG
Page 21
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 21/57
Analytical Equipment
Description
Agilent GC/MS, EI in SIM mode using deutuerated IS; D-5 pyridine (84), pyridine(79) & D-7 quinoline(136) & quinoline(129);
Detection Systems + Conditions
Column: DBWax 30mX0.25mmX0.25Um, 50oC for 6min, 4oC/min to 160oc, 30oC to 250oC for 5.5min: 10:1 split, flow 15mL/min, total flow 20ml/min,
1ul injection
Additional Details extracts were stored 4C prior
to analysis
Reference --
Quantitation Information
Limit of Quantitation
(mg/pad)
Limit of Detection (mg/pad)
Number of standards
Concentration of
each Standard
Internal Standard Ethanol (water), Anethole (others)
Calibration Type linear, with IS
r2
Additional Details
*Note: the example listed is not an e-cig method. It is just meant to show the requested level of detail for you to list for your aerosol method.
Page 22
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 22/57
Lab
Please paste in a picture of an example chromatogram for a calibration standard and for one or more samples for chromatographic methods
Please paste pictures relevant to any unusual observations noted during testing. Please include text explanation as necessary.
Page 23
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 23/57
Raw Data Tables (Example):
Aerosol Collection Date
Temperature (ºC)
% Relative Humidity
Sample Extraction Date
Analysis Date
Other observations
Rep1:
Rep2:
Rep3:
Rep4:
Rep5:
Product 1
Replicate 1
Puff
Group
Group Puff
Count
Collected ACM
(mg)
E-cig mass loss
(mg)
PG
(mg)
GLY
(mg)
NIC
(mg)
WAT
(mg)
Analyte Sum
(mg)
Analyte Sum:ACM
ratio
E-cig mass loss:ACM
ratio
1-50 0 #DIV/0! #DIV/0!
51-100 0 #DIV/0! #DIV/0!
101-150 0 #DIV/0! #DIV/0!
151-200 0 #DIV/0! #DIV/0!
201-250 0 #DIV/0! #DIV/0!
251-300 0 #DIV/0! #DIV/0!
301-350 0 #DIV/0! #DIV/0!
351-400 0 #DIV/0! #DIV/0!
401-450 0 #DIV/0! #DIV/0!
451-500 0 #DIV/0! #DIV/0!
501-550 0 #DIV/0! #DIV/0!
551-600 0 #DIV/0! #DIV/0!
Total 0 0 0 0 0 0 0
Page 24
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 24/57
Product 1
Replicate 1
Puff Group
Group Puff
Count
Collected ACM
(mg)
E-cig mass loss
(mg)
PG (mg)
GLY (mg)
NIC (mg)
WAT (mg)
Analyte Sum
(mg)
Analyte Sum:ACM
ratio
E-cig mass loss:ACM
ratio
Product 1
Replicate 2
Puff Group
Group Puff Count
Collected ACM (mg)
E-cig mass loss (mg)
PG (mg)
GLY (mg)
NIC (mg)
WAT (mg)
Analyte Sum (mg)
Analyte Sum:ACM ratio
E-cig mass loss:ACM ratio
1-50 0 #DIV/0! #DIV/0!
51-100 0 #DIV/0! #DIV/0!
101-150 0 #DIV/0! #DIV/0!
151-200 0 #DIV/0! #DIV/0!
201-250 0 #DIV/0! #DIV/0!
251-300 0 #DIV/0! #DIV/0!
301-350 0 #DIV/0! #DIV/0!
351-400 0 #DIV/0! #DIV/0!
401-450 0 #DIV/0! #DIV/0!
451-500 0 #DIV/0! #DIV/0!
501-550 0 #DIV/0! #DIV/0!
551-600 0 #DIV/0! #DIV/0!
Total 0 0 0 0 0 0 0
Product 1
Replicate 3
Puff Group
Group Puff Count
Collected ACM (mg)
E-cig mass loss (mg)
PG (mg)
GLY (mg)
NIC (mg)
WAT (mg)
Analyte Sum (mg)
Analyte Sum:ACM ratio
E-cig mass loss:ACM ratio
1-50 0 #DIV/0! #DIV/0!
51-100 0 #DIV/0! #DIV/0!
101-150 0 #DIV/0! #DIV/0!
151-200 0 #DIV/0! #DIV/0!
201-250 0 #DIV/0! #DIV/0!
251-300 0 #DIV/0! #DIV/0!
301-350 0 #DIV/0! #DIV/0!
351-400 0 #DIV/0! #DIV/0!
401-450 0 #DIV/0! #DIV/0!
Page 25
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 25/57
Product 1
Replicate 1
Puff Group
Group Puff
Count
Collected ACM
(mg)
E-cig mass loss
(mg)
PG (mg)
GLY (mg)
NIC (mg)
WAT (mg)
Analyte Sum
(mg)
Analyte Sum:ACM
ratio
E-cig mass loss:ACM
ratio
451-500 0 #DIV/0! #DIV/0!
501-550 0 #DIV/0! #DIV/0!
551-600 0 #DIV/0! #DIV/0!
Total 0 0 0 0 0 0 0
Product 1
Replicate 4
Puff Group
Group Puff Count
Collected ACM (mg)
E-cig mass loss (mg)
PG (mg)
GLY (mg)
NIC (mg)
WAT (mg)
Analyte Sum (mg)
Analyte Sum:ACM ratio
E-cig mass loss:ACM ratio
1-50 0 #DIV/0! #DIV/0!
51-100 0 #DIV/0! #DIV/0!
101-150 0 #DIV/0! #DIV/0!
151-200 0 #DIV/0! #DIV/0!
201-250 0 #DIV/0! #DIV/0!
251-300 0 #DIV/0! #DIV/0!
301-350 0 #DIV/0! #DIV/0!
351-400 0 #DIV/0! #DIV/0!
401-450 0 #DIV/0! #DIV/0!
451-500 0 #DIV/0! #DIV/0!
501-550 0 #DIV/0! #DIV/0!
551-600 0 #DIV/0! #DIV/0!
Total 0 0 0 0 0 0 0
Product 1
Replicate 5
Puff
Group
Group Puff Count
Collected ACM (mg)
E-cig mass loss (mg)
PG
(mg)
GLY
(mg)
NIC
(mg)
WAT
(mg)
Analyte Sum (mg)
Analyte Sum:ACM ratio
E-cig mass loss:ACM ratio
1-50 0 #DIV/0! #DIV/0!
51-100 0 #DIV/0! #DIV/0!
101-150 0 #DIV/0! #DIV/0!
151-200 0 #DIV/0! #DIV/0!
Page 26
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 26/57
Product 1
Replicate 1
Puff Group
Group Puff
Count
Collected ACM
(mg)
E-cig mass loss
(mg)
PG (mg)
GLY (mg)
NIC (mg)
WAT (mg)
Analyte Sum
(mg)
Analyte Sum:ACM
ratio
E-cig mass loss:ACM
ratio
201-250 0 #DIV/0! #DIV/0!
251-300 0 #DIV/0! #DIV/0!
301-350 0 #DIV/0! #DIV/0!
351-400 0 #DIV/0! #DIV/0!
401-450 0 #DIV/0! #DIV/0!
451-500 0 #DIV/0! #DIV/0!
501-550 0 #DIV/0! #DIV/0!
551-600 0 #DIV/0! #DIV/0!
Total 0 0 0 0 0 0 0
Note: the example tables listed above were used to collect the raw data from the
participating laboratories for the various e-cigarette products evaluated.
Page 27
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 27/57
Appendix B: Laboratory Method Summaries
Vaping Instrument and Aerosol Collection System:
Lab Code
Outlier Info
Observations Machine RH/Temp CFP Conditione
d Pads pad holder
A
Prod 3, rep 5, prod5rep3,
prod8rep3: SM450 F1 machine locked up in CPU synchronization mode after final clearing puff. Transitioned to
SM450 F2 machine to complete testing. Prod7 rep2:The battery fully charged and glowed
when puffed but did not deliver any aerosol. The tip was checked and tightened again but the e-
cigarette still did not work.
Linear
(SM450) 60/72 F 44 mm ISO
B
a lot of liquid in smoke
channel for products 4, 6, 7, 8
Linear
(LM4X) 60/22 C 44 mm ISO metal
C low for
nicotine
Product 3,rep3:No LED
signals >>> Removed from the test pool Prod 4, rep3:LED signal is very weak Prod 6 rep2: no nic
Linear
(SM450) 60/22 C 44 mm ISO
D
Linear
(SM450) 61/22 C 44 mm ISO
E high for
glycerin Rotary
40 +/- 10
%/25 C 44 mm
40 +/- 10
%/25 C
F
Prod7, rep2,4:
handprimed
Linear
(SM450) 65/72 F 44 mm ISO plastic
G
Linear
(LM20X) 65/72 F 44 mm ISO
H
noted diff between
blinking and ACM drop off
Linear (SM450)
varied 44 mm ISO
I
PG
maybe low
Prod 1: lost; Prod 2 - last
pads 170 puffs
Linear
(Borg LX20)
65/72 F 44 mm ISO
J
maybe
low for water
Linear
(SM451) 65/72 F 44 mm ISO
K
no
method info
provided
no
method info
provided
no
method info
provided
no method info
provided
no
method info
provided
Page 28
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 28/57
Lab Code
Outlier Info
Observations Machine RH/Temp CFP Conditione
d Pads pad holder
L
Linear
(SM450) 65/72 F 44 mm ISO
M
prod 4, 8: requested
remove rep 1
Linear (SM450
RH) 60/22 C 44 mm ISO
N
maybe
high for water
Linear
(SM450 RH)
65/72 F 44 mm ISO
Analytical Method Parameters:
Analytical
Lab Extraction Solvent NIC WAT GLY PG
A wrist 60 min IPA Agilent GC with a
FID detector. Agilent GC with a TCD detector.
Agilent GC with a FID detector.
Agilent GC with a FID detector.
B orbital 30
min 20 ml IPA
Agilent 7890 GC
with FID and TCD detector
Agilent 7890
GC with FID and TCD detector
Agilent 7890
GC with FID and TCD detector
Agilent 7890 GC
with FID and TCD detector
C wrist 20 min 25 ml IPA GC-FID GC-TCD GC-FID GC-FID
D wrist 60 min 20 ml IPA Agilent GC-FID Agilent GC-
TCD Agilent GC-FID Agilent GC-FID
E orbital 20
min
20mL solution (n-
heptadecane/EtOH + 2-propanol)
Agilent GC 7890A
Agilent GC
7890A Agilent GC 7890A
F 20 min
10 ml Low water
isopropanol (99.54 %): Ethanol (0.40 %):trans-anethole
(0.06 %)
GC-FID
GC-TCD (dual column with Nic
analysis) GC-FID GC-FID
G wrist 30 min
(in holder) 10 ml IPA
GC Thermo Trace GC Ultra flame
ionization detection (FID)
250 ͦ C IS: n-heptadecane
GC Thermo Trace GC Ultra
thermal conductivity
detection (TCD) IS: ethanol
C Perkin Elmer
Clarus 500 flame ionization detection (FID)
GC Thermo Trace GC Ultra flame
ionization detection (FID)
250 ͦ C IS: n-heptadecane
H mixer 30 min 10 ml IPA Agilent 6890 GC
FID
Agilent 6890
GC TCD
Agilent 6890
GC FID
Agilent 6890 GC
FID
Page 29
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 29/57
Analytical
I orbital 30
min
20 ml IPA (see my
note on tab i)
Perkin Elmer GC-
FID/TCD, ISTD
Perkin Elmer
GC-FID/TCD
Perkin Elmer
GC-FID/TCD
Perkin Elmer GC-
FID/TCD
J wrist 30 min 20 ml IPA Agilent GC-FID AgilentGC-TCD Agilent GC-FID Agilent GC-FID
K no method
info provided
no method info
provided
no method info
provided
no method info
provided
no method info
provided
no method info
provided
L wrist 30 min 10 mL 2-Propanol Agilent 5890 GC
Series II FID/TCD
Agilent 5890
GC Series II FID/TCD
Agilent 5890
GC Series II FID/TCD
Agilent 5890 GC
Series II FID/TCD
M lateral 45
min 20 ml IPA Agilent GC-FID Agilent GC-TCD Varian GC-FID Varian GC-FID
N orbital 30
min 20 ml IPA GC FID GC TCD GC FID GC FID
Page 30
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 30/57
Limit of Quantitation (LOQ):
LOQ
Lab NIC WAT GLY PG
A 0.0372 mg/pad 1.21 mg/pad 0.556 mg/pad 0.158 mg/pad
B 0.01 mg/ml (low
standard)
0.5 mg/ml (low
standard)
0.51 mg/ml (low
standard)
0.1 mg/ml (low
standard)
C
D 0.007265mg/ml (low
standard)
10 ug/mL (low
standard)
10 ug/mL (low
standard)
E 0.025 mg/ml? (low
standard)
0.050 mg/ml? (low standard)
0.050 mg/ml? (low standard)
F (mg/mL) 0.05 (low
standard) mg/ml 0.25 (low
standard) (mg/mL) 0.025 (low standard)
(mg/mL) 0.00064 (low standard)
G 0.494 1.0 mg/ml 0.58 0.2
H 0.0093 mg/pad 0.020 mg/pad 0.0714 mg/pad 0.0723 mg/mL
I 0.1 mg/pad 1 mg/pad 0.2 mg/pad 0.2 mg/pad
J 0.02 mg/pad 8 mg/pad 0.3 mg/pad 0.08 mg/pad
K no method info
provided
no method info
provided
no method info
provided
no method info
provided
L 0.0514 0.4952 0.3312 0.2548
M 0.023 mg/mL (low
standard) 0.045 mg/mL (low
standard) 0.008 mg/mL (low
standard) 0.002 mg/mL (low
standard)
N 0.33 mg/pad 3.33 mg/pad 0.33 mg/pad 0.33 mg/pad
Page 31
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 31/57
Appendix C: Raw Data
Measure Lab Rep Prod 1 Prod 2 Prod 3 Prod 4 Prod 5 Prod 7 Prod 8
Puff Count A 1 295 312 393 179 186 283 200
Puff Count A 2 284 316 397 188 188 200
Puff Count A 3 284 316 400 183 194 259 200
Puff Count A 4 284 311 3753 177 193 259 200
Puff Count A 5 294 308 394 177 200 225 200
Puff Count B 1 323 363 449 204 232 295 230
Puff Count B 2 311 349 461 200 222 285 222
Puff Count B 3 312 350 433 200 213 280 216
Puff Count B 4
Puff Count B 5
Puff Count C 1 279 284 396 195 208 294 190
Puff Count C 2 286 299 404 194 189 274 195
Puff Count C 3 298 304 216 244 195
Puff Count C 4 296 288 395 160 190 274 193
Puff Count C 5 286 305 189 190 244 188
Puff Count D 1 292 308 395 198 190 249 198
Puff Count D 2 311 307 406 197 203 293 185
Puff Count D 3 288 309 362 194 195 255 196
Puff Count D 4 284 314 392 177 182 258 182
Puff Count D 5 296 312 379 204 189 227 195
Puff Count E 1 277 306 393 184 185 297 172
Puff Count E 2 276 299 399 198 199 266 155
Puff Count E 3 285 294 393 200 260 234
Puff Count E 4 276 299 386 216 200 250 196
Puff Count E 5 278 286 384 198 195 270 202
Puff Count F 1 287 300 400 194 200 278 196
Puff Count F 2 300 300 392 188 199 263 190
Puff Count F 3 285 317 392 200 198 250 196
Puff Count F 4 285 300 400 196 198 277 199
Puff Count F 5 300 326 400 178 200 250 199
Puff Count G 1 303 334 429 210 188 342 199
Puff Count G 2 289 331 242 197 328 300
Puff Count G 3 294 333 408 202 231 234 233
Puff Count G 4 303 416 212 300 347 233
Puff Count G 5 305 335 407 201 232 349 231
Puff Count H 1 286 321 394 183 203 241 198
Puff Count H 2 292 310 395 184 168 275 177
Puff Count H 3 286 315 399 185 192 244 212
Page 32
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 32/57
Measure Lab Rep Prod 1 Prod 2 Prod 3 Prod 4 Prod 5 Prod 7 Prod 8
Puff Count H 4 277 310 404 193 197 224 213
Puff Count H 5 277 307 403 183 195 258 211
Puff Count I 1 320 394 192 220 281 201
Puff Count I 2 326 425 208 224 289 213
Puff Count I 3 327 440 216 210 259 210
Puff Count I 4 282 415 225 227 272 205
Puff Count I 5 313 421 198 216 287 222
Blank spaces indicate non-reported values
Measure Lab Rep Prod 1 Prod 2 Prod 3 Prod 4 Prod 5 Prod 7 Prod 8
Puff Count J 1 305 350 450 250 250 350 250
Puff Count J 2 350 450 250 250 350 250
Puff Count J 3 305 350 450 250 250 250
Puff Count J 4 305 400 350 250 250 350 250
Puff Count J 5 305 350 250 250 350 250
Puff Count K 1 203 210 206
Puff Count K 2 297 322 424 196 211 276 212
Puff Count K 3 297 322 416 184 187 284 208
Puff Count K 4 297 315 207 218 288 212
Puff Count K 5 310 340 203 308 212
Puff Count L 1 307 378 206 171 254 208
Puff Count L 2 288 317 399 195 206
Puff Count L 3 295 305 391 195 167 259 199
Puff Count L 4 288 310 382 174 172 272 197
Puff Count L 5 287 317 396 179 176 265 204
Puff Count M 1 283 310 450 192 257
Puff Count M 2 283 321 450 194 270 120
Puff Count M 3 285 321 396 191 181 265 127
Puff Count M 4 280 319 403 193 177 204 125
Puff Count M 5 291 319 190 188 265 127
Puff Count N 1 299 307 399 179 208 275 192
Puff Count N 2 275 317 391 206 210 257 206
Puff Count N 3 300 307 398 181 191 254 192
Puff Count N 4 287 314 382 188 278 193
Puff Count N 5 283 318 396 208 194 256 194
ACM, mg A 1 614 596 757 548 628 843 670
ACM, mg A 2 630 575 640 642 728 726
ACM, mg A 3 660 526 611 632 749 750 680
ACM, mg A 4 675 610 558 552 575 762 720
ACM, mg A 5 505 586 704 676 664 765 542
ACM, mg B 1 612 546 622 546 589 834 703
Page 33
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 33/57
Measure Lab Rep Prod 1 Prod 2 Prod 3 Prod 4 Prod 5 Prod 7 Prod 8
ACM, mg B 2 549 428 616 533 629 808 674
ACM, mg B 3 597 541 664 604 565 714 638
ACM, mg B 4
ACM, mg B 5
ACM, mg C 1 641 640 482 735 742 880 644
ACM, mg C 2 670 523 658 627 710 750 668
ACM, mg C 3 539 521 487 767 666
ACM, mg C 4 573 423 746 416 633 800 699
ACM, mg C 5 600 587 575 759 653 596
ACM, mg D 1 580 524 745 493 689 705 700
ACM, mg D 2 545 519 772 648 665 973 655
ACM, mg D 3 553 509 660 604 696 777 629
ACM, mg D 4 582 577 555 598 614 764 598
ACM, mg D 5 651 572 745 580 610 554 644
Blank spaces indicate non-reported values
Measure Lab Rep Prod 1 Prod 2 Prod 3 Prod 4 Prod 5 Prod 7 Prod 8
ACM, mg E 1 557 511 430 460 384 723 500
ACM, mg E 2 575 378 641 489 492 797 434
ACM, mg E 3 486 410 523 408 728 527
ACM, mg E 4 493 466 650 530 540 697 539
ACM, mg E 5 587 376 602 520 527 503 586
ACM, mg F 1 552 447 833 614 614 894 711
ACM, mg F 2 582 468 692 592 670 852 702
ACM, mg F 3 557 524 755 661 742 839 724
ACM, mg F 4 635 555 814 661 715 865 742
ACM, mg F 5 600 576 759 519 620 805 673
ACM, mg G 1 665 659 710 621 476 904 596
ACM, mg G 2 615 520 651 559 778 766
ACM, mg G 3 508 682 734 595 643 725 620
ACM, mg G 4 500 782 594 534 795 647
ACM, mg G 5 585 592 699 568 685 924 644
ACM, mg H 1 715 559 529 572 698 732 618
ACM, mg H 2 616 659 724 596 693 905 592
ACM, mg H 3 614 558 830 590 667 776 688
ACM, mg H 4 524 612 612 648 499 682 615
ACM, mg H 5 696 573 716 632 658 918 690
ACM, mg I 1 540 559 561 542 796 571
ACM, mg I 2 576 495 617 700 796 680
ACM, mg I 3 562 534 578 579 811 624
Page 34
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 34/57
Measure Lab Rep Prod 1 Prod 2 Prod 3 Prod 4 Prod 5 Prod 7 Prod 8
ACM, mg I 4 542 829 466 463 788 676
ACM, mg I 5 498 596 587 582 878 755
ACM, mg J 1 605 508 629 620 573 906 645
ACM, mg J 2 489 820 580 668 798 686
ACM, mg J 3 660 400 831 454 651 663
ACM, mg J 4 604 648 574 567 668 851 796
ACM, mg J 5 526 471 546 579 847 744
ACM, mg K 1 745 664 696
ACM, mg K 2 536 443 613 518 685 791 783
ACM, mg K 3 622 620 737 555 725 544 629
ACM, mg K 4 644 507 546 721 694 748
ACM, mg K 5 560 566 603 867 640
ACM, mg L 1 538 745 606 672 777 666
ACM, mg L 2 579 398 710 618 598
ACM, mg L 3 673 624 740 701 587 859 651
ACM, mg L 4 728 546 663 518 720 902 586
ACM, mg L 5 703 503 399 436 654 718 654
ACM, mg M 1 680 530 645 717 999
ACM, mg M 2 501 687 832 723 638 352
ACM, mg M 3 688 479 736 667 631 843 430
ACM, mg M 4 607 576 606 627 675 633 405
ACM, mg M 5 485 565 635 677 682 412
Blank spaces indicate non-reported values
Measure Lab Rep Prod 1 Prod 2 Prod 3 Prod 4 Prod 5 Prod 7 Prod 8
ACM, mg N 1 694 564 863 519 569 755 713
ACM, mg N 2 517 578 637 596 646 658 723
ACM, mg N 3 573 570 370 621 740 803 674
ACM, mg N 4 679 568 745 654 961 652
ACM, mg N 5 739 539 702 697 698 901 654
Total PG, mg A 1 0 320 410 316 362 445 338
Total PG, mg A 2 0 313 333 368 428 367
Total PG, mg A 3 0 283 324 362 457 386 342
Total PG, mg A 4 0 326 305 317 345 396 357
Total PG, mg A 5 0 321 390 387 394 394 275
Total PG, mg B 1 10.16 302 357 325 372 471 357
Total PG, mg B 2 11.40 228 368 331 389 458 344
Total PG, mg B 3 11.78 310 383 355 346 412 316
Total PG, mg B 4
Total PG, mg B 5
Page 35
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 35/57
Measure Lab Rep Prod 1 Prod 2 Prod 3 Prod 4 Prod 5 Prod 7 Prod 8
Total PG, mg C 1 0 366 262 435 460 478 323
Total PG, mg C 2 0 293 361 388 443 416 343
Total PG, mg C 3 0 295 299 424 336
Total PG, mg C 4 0 235 421 255 391 441 357
Total PG, mg C 5 0 332 352 479 356 305
Total PG, mg D 1 3.09 283 416 288 400 360 340
Total PG, mg D 2 3.36 280 432 375 387 499 319
Total PG, mg D 3 3.46 275 363 344 387 390 306
Total PG, mg D 4 3.32 315 295 347 343 387 292
Total PG, mg D 5 4.11 311 402 326 350 281 315
Total PG, mg E 1 0 291 221 345 265 424 301
Total PG, mg E 2 0 221 377 332 331 523 234
Total PG, mg E 3 0 250 275 305 405 314
Total PG, mg E 4 0 285 381 369 376 439 298
Total PG, mg E 5 0 225 380 381 382 308 348
Total PG, mg F 1 0.83 240 453 379 415 501 360
Total PG, mg F 2 0.43 256 371 364 417 467 355
Total PG, mg F 3 0.11 286 419 429 499 447 389
Total PG, mg F 4 0.03 317 449 416 420 508 403
Total PG, mg F 5 0.09 311 389 321 400 462 339
Total PG, mg G 1 0 376 394 377 298 503 301
Total PG, mg G 2 0 294 391 350 426 355
Total PG, mg G 3 0 392 412 369 408 404 314
Total PG, mg G 4 0 438 365 324 448 324
Total PG, mg G 5 0 332 387 347 402 508 289
Total PG, mg H 1 0.85 340 282 338 424 397 311
Total PG, mg H 2 1.53 417 394 352 412 476 296
Total PG, mg H 3 0.77 411 448 352 389 414 346
Total PG, mg H 4 1.52 478 328 376 287 359 313
Total PG, mg H 5 2.30 540 395 378 394 487 352
Blank spaces indicate non-reported values
Measure Lab Rep Prod 1 Prod 2 Prod 3 Prod 4 Prod 5 Prod 7 Prod 8
Total PG, mg I 1 309 228 308 281 353 261
Total PG, mg I 2 323 220 314 302 376 293
Total PG, mg I 3 309 220 335 276 353 273
Total PG, mg I 4 316 407 300 267 332 277
Total PG, mg I 5 270 298 308 279 382 339
Total PG, mg J 1 0.32 292 360 420 366 538 355
Total PG, mg J 2 284 473 338 398 464 429
Page 36
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 36/57
Measure Lab Rep Prod 1 Prod 2 Prod 3 Prod 4 Prod 5 Prod 7 Prod 8
Total PG, mg J 3 0.28 222 482 384 391 402
Total PG, mg J 4 0.09 384 327 303 416 511 449
Total PG, mg J 5 0.45 266 297 373 495 423
Total PG, mg K 1 485 429 372
Total PG, mg K 2 0 262 364 313 456 467 428
Total PG, mg K 3 0 371 437 361 468 316 330
Total PG, mg K 4 0 309 336 483 446 406
Total PG, mg K 5 0 342 424 528 354
Total PG, mg L 1 301 420 350 406 419 336
Total PG, mg L 2 0 222 401 364 302
Total PG, mg L 3 0 350 416 421 350 474 322
Total PG, mg L 4 0 311 371 309 439 505 287
Total PG, mg L 5 0 283 214 256 394 379 328
Total PG, mg M 1 0.27 278 349 436 545
Total PG, mg M 2 0.14 377 460 424 334 174
Total PG, mg M 3 0.16 246 388 398 386 448 211
Total PG, mg M 4 0.14 303 310 371 389 340 199
Total PG, mg M 5 0.25 295 361 415 359 215
Total PG, mg N 1 0 294 458 286 307 385 331
Total PG, mg N 2 0 301 328 321 365 322 339
Total PG, mg N 3 0 293 196 340 412 409 309
Total PG, mg N 4 0 300 226 365 499 299
Total PG, mg N 5 0 281 370 386 388 470 297
Glycerin, mg A 1 486 168 207 105 111 222 202
Glycerin, mg A 2 507 166 180 113 131 213
Glycerin, mg A 3 531 152 168 114 135 198 203
Glycerin, mg A 4 548 171 160 104 104 199 216
Glycerin, mg A 5 412 169 206 120 122 203 163
Glycerin, mg B 1 502 171 184 105 111 224 208
Glycerin, mg B 2 445 131 184 99 118 210 195
Glycerin, mg B 3 475 165 190 112 106 189 183
Glycerin, mg B 4
Glycerin, mg B 5
Glycerin, mg C 1 515 180 136 127 133 235 191
Glycerin, mg C 2 540 149 180 112 127 195 192
Glycerin, mg C 3 426 147 92 196 194
Glycerin, mg C 4 460 119 205 77 117 207 202
Glycerin, mg C 5 485 164 102 140 170 173
Blank spaces indicate non-reported values
Measure Lab Rep Prod 1 Prod 2 Prod 3 Prod 4 Prod 5 Prod 7 Prod 8
Page 37
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 37/57
Measure Lab Rep Prod 1 Prod 2 Prod 3 Prod 4 Prod 5 Prod 7 Prod 8
Glycerin, mg D 1 415 148 185 89 115 170 181
Glycerin, mg D 2 414 151 180 112 113 229 172
Glycerin, mg D 3 424 146 155 105 120 180 160
Glycerin, mg D 4 457 160 131 108 104 175 154
Glycerin, mg D 5 506 162 181 100 104 129 164
Glycerin, mg E 1 823 252 297 183 151 391 296
Glycerin, mg E 2 864 207 392 175 172 421 237
Glycerin, mg E 3 680 244 316 160 368 292
Glycerin, mg E 4 708 267 387 193 199 373 354
Glycerin, mg E 5 923 211 347 187 209 284 359
Glycerin, mg F 1 442 123 210 112 120 213 203
Glycerin, mg F 2 427 131 183 102 126 198 194
Glycerin, mg F 3 442 146 201 124 140 208 207
Glycerin, mg F 4 488 157 209 119 126 222 215
Glycerin, mg F 5 469 157 188 89 116 214 181
Glycerin, mg G 1 548 184 200 111 96 237 176
Glycerin, mg G 2 508 146 114 113 208 268
Glycerin, mg G 3 418 190 214 110 126 194 183
Glycerin, mg G 4 409 226 107 103 205 190
Glycerin, mg G 5 486 166 202 103 125 247 221
Glycerin, mg H 1 545 331 149 104 128 186 171
Glycerin, mg H 2 480 278 199 108 128 225 163
Glycerin, mg H 3 457 212 224 108 117 196 190
Glycerin, mg H 4 408 174 175 116 91 174 170
Glycerin, mg H 5 529 195 197 116 118 229 191
Glycerin, mg I 1 126 118 108 81 181 127
Glycerin, mg I 2 133 108 120 84 185 128
Glycerin, mg I 3 128 109 110 78 163 141
Glycerin, mg I 4 124 193 88 74 166 129
Glycerin, mg I 5 111 145 110 92 185 147
Glycerin, mg J 1 513 152 178 166 161 246 139
Glycerin, mg J 2 147 232 129 167 219 165
Glycerin, mg J 3 561 121 240 152 166 156
Glycerin, mg J 4 510 187 168 116 183 231 177
Glycerin, mg J 5 441 138 114 168 234 168
Glycerin, mg K 1 141 127 212
Glycerin, mg K 2 471 136 188 95 130 228 246
Glycerin, mg K 3 556 186 221 107 137 151 190
Glycerin, mg K 4 556 153 105 142 212 227
Glycerin, mg K 5 492 172 125 243 200
Page 38
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 38/57
Measure Lab Rep Prod 1 Prod 2 Prod 3 Prod 4 Prod 5 Prod 7 Prod 8
Glycerin, mg L 1 149 206 113 130 205 181
Glycerin, mg L 2 471 114 197 116 162
Glycerin, mg L 3 544 172 205 124 109 221 175
Glycerin, mg L 4 583 157 184 93 140 230 155
Glycerin, mg L 5 570 146 116 81 123 185 175
Blank spaces indicate non-reported values
Measure Lab Rep Prod 1 Prod 2 Prod 3 Prod 4 Prod 5 Prod 7 Prod 8
Glycerin, mg M 1 553 144 175 131 255
Glycerin, mg M 2 405 187 228 131 168 102
Glycerin, mg M 3 565 135 198 122 114 222 119
Glycerin, mg M 4 484 158 163 111 123 162 115
Glycerin, mg M 5 376 152 127 121 172 94
Glycerin, mg N 1 557 157 232 94 104 196 197
Glycerin, mg N 2 411 160 171 111 128 169 194
Glycerin, mg N 3 459 161 103 113 130 188 178
Glycerin, mg N 4 545 157 201 121 230 172
Glycerin, mg N 5 596 152 196 130 124 221 175
Nicotine, mg A 1 8.94 8.07 10.27 6.42 7.20 16.22 8.43
Nicotine, mg A 2 9.53 7.79 8.34 6.97 8.55 9.18
Nicotine, mg A 3 9.82 7.14 8.15 6.95 9.16 14.25 8.62
Nicotine, mg A 4 10.39 8.16 7.69 6.39 6.90 14.37 8.96
Nicotine, mg A 5 7.47 8.05 9.97 7.43 8.02 14.61 6.87
Nicotine, mg B 1 8.58 7.34 8.29 6.26 7.23 15.22 8.50
Nicotine, mg B 2 7.88 5.35 8.21 5.95 7.17 14.84 8.19
Nicotine, mg B 3 8.52 7.06 8.88 6.59 6.67 13.17 7.61
Nicotine, mg B 4
Nicotine, mg B 5
Nicotine, mg C 1 9.03 8.37 5.94 8.14 8.81 17.15 8.09
Nicotine, mg C 2 9.67 6.83 8.27 7.20 8.55 14.65 8.43
Nicotine, mg C 3 7.42 6.87 5.81 14.86 8.38
Nicotine, mg C 4 7.88 5.44 9.78 4.88 7.19 15.31 8.83
Nicotine, mg C 5 8.45 7.49 6.38 9.19 12.63 7.55
Nicotine, mg D 1 8.35 6.67 9.71 5.88 8.37 13.03 8.63
Nicotine, mg D 2 7.57 6.76 10.20 7.32 8.02 18.42 8.09
Nicotine, mg D 3 7.78 6.46 8.67 6.88 8.21 14.47 7.80
Nicotine, mg D 4 8.46 7.51 6.89 7.00 7.26 14.23 7.31
Nicotine, mg D 5 9.52 7.28 9.83 6.69 7.25 10.22 7.89
Nicotine, mg E 1 5.68 5.78 5.76 6.20 4.76 13.90 7.12
Nicotine, mg E 2 5.68 4.26 9.08 5.72 6.06 16.86 5.14
Page 39
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 39/57
Measure Lab Rep Prod 1 Prod 2 Prod 3 Prod 4 Prod 5 Prod 7 Prod 8
Nicotine, mg E 3 4.72 5.02 5.94 5.42 13.06 6.98
Nicotine, mg E 4 4.80 5.72 8.12 6.20 6.96 14.42 7.28
Nicotine, mg E 5 6.50 4.94 8.26 6.58 6.76 10.08 7.82
Nicotine, mg F 1 9.05 6.43 12.32 8.01 8.10 18.77 9.47
Nicotine, mg F 2 9.91 6.54 10.24 7.50 9.32 18.06 9.45
Nicotine, mg F 3 8.80 7.48 11.11 8.52 10.18 17.67 9.82
Nicotine, mg F 4 11.01 8.12 11.51 8.45 9.47 17.94 10.05
Nicotine, mg F 5 9.42 8.27 11.14 6.61 8.20 17.46 9.19
Nicotine, mg G 1 10.90 9.85 10.34 8.09 6.82 19.62 8.11
Nicotine, mg G 2 9.89 7.73 8.40 8.05 16.33 10.05
Nicotine, mg G 3 7.80 10.20 11.36 8.01 9.20 15.43 8.24
Nicotine, mg G 4 7.62 8.83 7.97 6.79 19.42 8.45
Nicotine, mg G 5 9.14 8.32 10.59 7.61 8.03 19.58 8.37
Blank spaces indicate non-reported values
Measure Lab Rep Prod 1 Prod 2 Prod 3 Prod 4 Prod 5 Prod 7 Prod 8
Nicotine, mg H 1 9.00 10.78 7.35 6.56 8.85 13.65 7.72
Nicotine, mg H 2 8.73 10.82 10.05 6.82 8.83 16.47 7.27
Nicotine, mg H 3 8.31 9.66 11.16 6.92 7.90 14.31 8.67
Nicotine, mg H 4 7.42 9.77 8.66 7.23 6.03 12.56 7.76
Nicotine, mg H 5 9.49 10.92 10.12 7.30 8.12 16.82 8.80
Nicotine, mg I 1 7.54 5.43 6.88 5.22 12.85 7.35
Nicotine, mg I 2 8.07 5.23 7.70 5.91 12.75 7.71
Nicotine, mg I 3 7.72 5.20 7.12 5.41 13.45 6.62
Nicotine, mg I 4 7.71 9.20 5.59 5.15 12.66 6.74
Nicotine, mg I 5 6.93 6.78 7.11 6.30 14.16 8.16
Nicotine, mg J 1 8.22 6.48 8.22 10.43 7.86 17.23 7.41
Nicotine, mg J 2 6.29 10.96 8.06 8.37 15.07 8.81
Nicotine, mg J 3 9.49 4.99 11.12 9.91 8.15 8.11
Nicotine, mg J 4 8.71 8.34 7.66 7.13 8.95 16.12 9.37
Nicotine, mg J 5 7.31 5.90 7.05 7.94 16.16 8.67
Nicotine, mg K 1 8.55 8.33 7.00
Nicotine, mg K 2 8.23 6.16 8.90 6.14 8.59 15.92 10.03
Nicotine, mg K 3 9.91 8.72 10.71 7.02 9.09 11.23 8.12
Nicotine, mg K 4 9.91 7.40 6.65 8.93 16.00 9.40
Nicotine, mg K 5 8.66 8.16 8.23 18.58 8.32
Nicotine, mg L 1 7.41 10.58 7.46 8.76 15.77 8.56
Nicotine, mg L 2 8.73 5.34 10.28 7.54 7.48
Nicotine, mg L 3 10.56 8.57 10.56 8.38 7.41 17.03 8.25
Nicotine, mg L 4 11.41 7.45 9.54 6.17 9.56 18.33 7.32
Page 40
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 40/57
Measure Lab Rep Prod 1 Prod 2 Prod 3 Prod 4 Prod 5 Prod 7 Prod 8
Nicotine, mg L 5 10.86 6.80 5.39 5.48 8.72 14.16 8.37
Nicotine, mg M 1 9.75 6.66 8.92 8.42 17.97
Nicotine, mg M 2 7.11 8.67 10.37 8.02 11.54 4.25
Nicotine, mg M 3 9.73 5.99 9.47 7.27 7.29 15.15 5.09
Nicotine, mg M 4 8.57 7.23 7.74 7.07 7.66 11.35 4.86
Nicotine, mg M 5 6.69 7.04 7.19 7.97 12.05 4.68
Nicotine, mg N 1 9.47 7.48 11.90 5.42 7.05 13.78 9.23
Nicotine, mg N 2 7.53 7.64 6.98 7.14 8.18 12.58 9.11
Nicotine, mg N 3 7.78 7.60 5.64 7.53 9.49 15.55 8.69
Nicotine, mg N 4 9.33 6.40 9.63 7.90 18.96 8.42
Nicotine, mg N 5 10.71 5.91 8.85 8.25 9.02 17.29 8.40
Water, mg A 1 90.4 63.4 81.8 88.6 85.3 99.5 112.0
Water, mg A 2 90.7 61.1 78.8 103.8 83.9 114.5
Water, mg A 3 94.8 58.9 68.3 101.3 74.9 88.5 109.1
Water, mg A 4 95.3 63.9 70.5 90.3 72.5 95.4 112.2
Water, mg A 5 79.4 59.1 82.1 114.5 79.2 88.5 91.9
Water, mg B 1 94.3 66.5 88.6 96.3 90.4 109.4 112.3
Water, mg B 2 86.8 54.3 78.1 91.1 79.4 98.3 116.4
Water, mg B 3 90.2 66.1 79.8 97.3 75.2 83.6 102.2
Water, mg B 4
Water, mg B 5
Blank spaces indicate non-reported values
Measure Lab Rep Prod 1 Prod 2 Prod 3 Prod 4 Prod 5 Prod 7 Prod 8
Water, mg C 1 108.0 71.4 62.4 116.4 103.6 107.3 104.0
Water, mg C 2 104.2 62.8 88.2 106.6 98.4 89.4 107.8
Water, mg C 3 89.1 62.8 69.1 89.9 112.5
Water, mg C 4 89.6 53.7 90.5 67.3 86.4 97.6 110.7
Water, mg C 5 91.6 69.2 91.7 105.3 81.4 98.3
Water, mg D 1 82.0 59.0 85.6 79.7 97.7 89.2 107.5
Water, mg D 2 98.5 54.3 93.4 106.6 85.4 121.2 98.8
Water, mg D 3 77.9 56.3 81.3 96.0 73.1 99.2 99.2
Water, mg D 4 80.8 61.3 68.3 98.3 93.1 93.1 92.1
Water, mg D 5 91.9 59.9 98.2 94.2 85.3 76.9 101.0
Water, mg E 1
Water, mg E 2
Water, mg E 3
Water, mg E 4
Water, mg E 5
Water, mg F 1 87.0 58.2 100.7 96.5 92.7 110.9 120.9
Page 41
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 41/57
Measure Lab Rep Prod 1 Prod 2 Prod 3 Prod 4 Prod 5 Prod 7 Prod 8
Water, mg F 2 95.8 62.2 94.5 105.9 93.0 106.1 106.5
Water, mg F 3 90.8 68.0 94.8 118.5 102.6 99.3 125.4
Water, mg F 4 99.1 68.0 105.9 121.1 99.2 110.8 123.7
Water, mg F 5 96.2 73.9 98.6 80.8 101.7 99.3 115.4
Water, mg G 1 94.0 67.5 95.8 86.2 66.3 116.9 108.3
Water, mg G 2 86.2 58.9 86.9 79.9 110.8 123.7
Water, mg G 3 74.6 70.8 101.6 81.0 83.4 102.3 110.4
Water, mg G 4 74.3 81.2 94.4 98.4 121.0 119.1
Water, mg G 5 84.0 67.3 98.5 84.5 114.1 122.1 112.4
Water, mg H 1 120.8 146.6 89.7 98.0 102.8 108.6 110.8
Water, mg H 2 110.2 150.8 111.5 103.4 98.9 128.4 108.6
Water, mg H 3 107.5 136.5 133.5 104.2 111.3 112.8 123.6
Water, mg H 4 98.7 134.3 100.0 108.1 90.6 102.3 114.0
Water, mg H 5 118.9 144.3 121.2 107.2 101.9 125.7 123.8
Water, mg I 1 62.0 60.9 99.0 73.6 96.3 103.2
Water, mg I 2 72.0 61.5 105.0 73.5 95.4 107.2
Water, mg I 3 66.1 61.3 103.9 59.9 93.1 91.2
Water, mg I 4 64.7 92.3 84.4 72.4 91.5 97.4
Water, mg I 5 67.0 74.1 101.4 88.9 104.1 112.0
Water, mg J 1 74.2 21.8 12.3 88.5 56.7 76.6 83.8
Water, mg J 2 20.8 31.6 77.0 68.5 68.5 82.0
Water, mg J 3 79.4 9.2 38.1 58.0 73.4 79.6
Water, mg J 4 72.2 42.2 21.0 74.3 79.8 76.6 98.9
Water, mg J 5 64.4 11.7 72.1 57.6 75.9 89.8
Water, mg K 1 111.7 87.2 114.0
Water, mg K 2 72.5 44.0 46.7 85.0 103.5 91.2 122.1
Water, mg K 3 89.0 51.5 61.3 98.8 108.7 62.1 92.6
Water, mg K 4 89.0 46.9 86.1 82.7 80.2 126.1
Water, mg K 5 77.6 48.1 86.2 89.3 97.1
Blank spaces indicate non-reported values
Measure Lab Rep Prod 1 Prod 2 Prod 3 Prod 4 Prod 5 Prod 7 Prod 8
Water, mg L 1 64.7 91.0 103.4 77.7 93.4 103.6
Water, mg L 2 90.6 58.3 119.3 104.1 93.5
Water, mg L 3 106.2 72.5 101.7 121.6 77.9 96.2 99.0
Water, mg L 4 106.3 61.1 103.6 87.8 77.2 104.7 87.0
Water, mg L 5 121.3 104.6 128.6 116.9 83.2 86.5 100.1
Water, mg M 1 105.1 67.2 98.6 85.0 120.2
Water, mg M 2 80.2 84.9 112.3 102.4 84.1 55.1
Water, mg M 3 103.0 63.6 102.8 111.9 89.3 98.6 71.9
Page 42
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 42/57
Water, mg M 4 95.2 69.4 85.8 106.8 111.1 73.4 65.8
Water, mg M 5 76.0 70.1 99.6 84.5 84.3 66.0
Water, mg N 1 122.6 80.4 155.1 86.0 96.4 90.3 105.1
Water, mg N 2 91.5 82.8 84.2 87.3 93.1 77.6 103.5
Water, mg N 3 102.3 74.0 87.5 87.3 112.0 91.1 92.9
Water, mg N 4 113.9 72.1 118.0 94.6 109.8 95.9
Water, mg N 5 118.3 66.9 158.7 105.9 89.1 104.5 93.3
Blank spaces indicate non-reported values
Page 43
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 43/57
Appendix D: Raw Data Plots
Figure 1. Replicate Values for Total Puff Count
Figure 2. Replicate Values for Total ACM, mg
Tota
l AC
M, m
g
Total ACM, mg Replicate Data
Page 44
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 44/57
Figure 3. Replicate Values for Total Propylene Glycol, mg
Figure 4. Replicate Values for Propylene Glycol, % of ACM
Pro
pyl
en
e G
lyco
l, %
of
AC
M, m
g
Propylene Glycol, % of ACM Replicate Data
Page 45
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 45/57
Figure 5. Replicate Values for Total Glycerin, mg
Figure 6. Replicate Values for Glycerin, % of ACM
Gly
ceri
n, %
of
AC
M
Glycerine, % of ACM Replicate Data
Page 46
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 46/57
Figure 7. Replicate Values for Total Nicotine, mg
Figure 8. Replicate Values for Nicotine, % of ACM
Nic
oti
ne
, % o
f A
CM
Nicotine, % of ACM Replicate Data
Page 47
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 47/57
Figure 9. Replicate Values for Total Water, mg
Figure 10. Replicate Values for Water, % of ACM
Wat
er,
% o
f A
CM
Water, % of ACM Replicate Data
Page 48
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 48/57
Appendix E: Mandel Charts
Figure 11. Total Puffs, Mandel h Chart for Lab Means
Figure 12. Total Puffs, Mandel k Chart for Lab Standard Deviations
-3.00
-2.00
-1.00
0.00
1.00
2.00
3.00
LabA
LabB
LabC
LabD
LabE
LabF
LabG
LabH
LabI
LabJ
LabK
LabL
LabM
LabN
Man
del
h S
tati
stic
Test Laboratory
Total Puffs Mandel h Chart for Means
Product 1
Product 2
Product 3
Product 4
Product 5
Product 7
Product 8
Man. 0.01 U
Man. 0.05 U
Man. 0.05 L
Man. 0.01 L
0.00
0.50
1.00
1.50
2.00
2.50
3.00
LabA
LabB
LabC
LabD
LabE
LabF
LabG
LabH
Lab ILab J LabK
LabL
LabM
LabN
Man
del
k S
tati
stic
Test Laboratory
Total Puffs Mandel k Chart for Std. Dev.
Product 1
Product 2
Product 3
Product 4
Product 5
Product 7
Product 8
Man. 0.01
Man. 0.05
Page 49
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 49/57
Figure 13. Total ACM mg, Mandel h Chart for Lab Means
Figure 14. Total ACM mg, Mandel k Chart for Lab Standard Deviations
-3.00
-2.00
-1.00
0.00
1.00
2.00
3.00
LabA
LabB
LabC
LabD
LabE
LabF
LabG
LabH
Lab I LabJ
LabK
LabL
LabM
LabN
Man
del
h S
tati
stic
Test Laboratory
Total ACM (mg) Mandel h Chart for Means
Product 1
Product 2
Product 3
Product 4
Product 5
Product 7
Product 8
Man. 0.01 U
Man. 0.05 U
Man. 0.05 L
Man. 0.01 L
0.00
0.20
0.40
0.60
0.80
1.00
1.20
1.40
1.60
1.80
2.00
LabA
LabB
LabC
LabD
LabE
LabF
LabG
LabH
Lab I LabJ
LabK
LabL
LabM
LabN
Man
del
k S
tati
stic
Test Laboratory
Total ACM (mg) Mandel k Chart for Std. Dev.
Product 1
Product 2
Product 3
Product 4
Product 5
Product 7
Product 8
Man. 0.01
Man. 0.05
Page 50
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 50/57
Figure 15. Total Propylene Glycol mg, Mandel h Chart for Lab Means
Figure 16. Total Propylene Glycol mg, Mandel k Chart for Lab Standard Deviations
-3.00
-2.00
-1.00
0.00
1.00
2.00
3.00
4.00
LabA
LabB
LabC
LabD
LabE
LabF
LabG
LabH
Lab I LabJ
LabK
LabL
LabM
LabN
Man
del
h S
tati
stic
Test Laboratory
Total PG (mg) Mandel h Chart for Means
Product 1
Product 2
Product 3
Product 4
Product 5
Product 7
Product 8
Man. 0.01 U
Man. 0.05 U
Man. 0.05 L
Man. 0.01 L
0.00
0.50
1.00
1.50
2.00
2.50
3.00
LabA
LabB
LabC
LabD
LabE
LabF
LabG
LabH
Lab I LabJ
LabK
LabL
LabM
LabN
Man
de
l k S
tati
stic
Test Laboratory
Total PG (mg) Mandel k Chart for Std. Dev.
Product 1
Product 2
Product 3
Product 4
Product 5
Product 7
Product 8
Man. 0.01
Man. 0.05
Page 51
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 51/57
Figure 17. Propylene Glycol, % of ACM, Mandel h Chart for Lab Means
Figure 18. Propylene Glycol, % of ACM, Mandel k Chart for Lab Standard Deviations
-3.00
-2.00
-1.00
0.00
1.00
2.00
3.00
4.00
LabA
LabB
LabC
LabD
LabE
LabF
LabG
LabH
Lab I LabJ
LabK
LabL
LabM
LabN
Man
del
h S
tati
stic
Test Laboratory
PG % of ACM Mandel h Chart for Means
Product 1
Product 2
Product 3
Product 4
Product 5
Product 7
Product 8
Man. 0.01 U
Man. 0.05 U
Man. 0.05 L
Man. 0.01 L
0.00
0.50
1.00
1.50
2.00
2.50
3.00
3.50
4.00
LabA
LabB
LabC
LabD
LabE
LabF
LabG
LabH
Lab I LabJ
LabK
LabL
LabM
LabN
Man
del
k S
tati
stic
Test Laboratory
PG % of ACM Mandel k Chart for Std. Dev.
Product 1
Product 2
Product 3
Product 4
Product 5
Product 7
Product 8
Man. 0.01
Man. 0.05
Page 52
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 52/57
Figure 19. Total Glycerin mg, Mandel h Chart for Lab Means
Figure 20. Total Glycerin mg, Mandel k Chart for Lab Standard Deviations
-3.00
-2.00
-1.00
0.00
1.00
2.00
3.00
4.00
LabA
LabB
LabC
LabD
LabE
LabF
LabG
LabH
Lab I LabJ
LabK
LabL
LabM
LabN
Man
del
h S
tati
stic
Test Laboratory
Total Glycerin (mg) Mandel h Chart for Mean
Product 1
Product 2
Product 3
Product 4
Product 5
Product 7
Product 8
Man. 0.01 U
Man. 0.05 U
Man. 0.05 L
Man. 0.01 L
0.00
0.50
1.00
1.50
2.00
2.50
3.00
LabA
LabB
LabC
LabD
LabE
LabF
LabG
LabH
Lab I LabJ
LabK
LabL
LabM
LabN
Man
del
k S
tati
stic
Test Laboratory
Total Glycerin (mg) Mandel k Chart for SD
Product 1
Product 2
Product 3
Product 4
Product 5
Product 7
Product 8
Man. 0.01
Man. 0.05
Page 53
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 53/57
Figure 21. Glycerin, % of ACM, Mandel h Chart for Lab Means
Figure 22. Glycerin, % of ACM, Mandel k Chart for Lab Standard Deviations
-3.00
-2.00
-1.00
0.00
1.00
2.00
3.00
4.00
LabA
LabB
LabC
LabD
LabE
LabF
LabG
LabH
Lab I LabJ
LabK
LabL
LabM
LabN
Ma
nd
el h
Sta
tist
ic
Test Laboratory
Glycerin % of ACM Mandel h Chart for Means
Product 1
Product 2
Product 3
Product 4
Product 5
Product 7
Product 8
Man. 0.01 U
Man. 0.05 U
Man. 0.05 L
Man. 0.01 L
0.00
0.50
1.00
1.50
2.00
2.50
3.00
3.50
4.00
LabA
LabB
LabC
LabD
LabE
LabF
LabG
LabH
Lab I LabJ
LabK
LabL
LabM
LabN
Man
de
l k S
tati
stic
Test Laboratory
Glycerin % of ACM Mandel k Chart for SD
Product 1
Product 2
Product 3
Product 4
Product 5
Product 7
Product 8
Man. 0.01
Man. 0.05
Page 54
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 54/57
Figure 23. Total Nicotine mg, Mandel h Chart for Lab Means
Figure 24. Total Nicotine mg, Mandel k Chart for Lab Standard Deviations
-3.00
-2.00
-1.00
0.00
1.00
2.00
3.00
LabA
LabB
LabC
LabD
LabE
LabF
LabG
LabH
Lab I LabJ
LabK
LabL
LabM
LabN
Man
del
h S
tati
stic
Test Laboratory
Total Nicotine (mg) Mandel h Chart for Mean
Product 1
Product 2
Product 3
Product 4
Product 5
Product 7
Product 8
Man. 0.01 U
Man. 0.05 U
Man. 0.05 L
Man. 0.01 L
0.00
0.20
0.40
0.60
0.80
1.00
1.20
1.40
1.60
1.80
2.00
LabA
LabB
LabC
LabD
LabE
LabF
LabG
LabH
Lab I LabJ
LabK
LabL
LabM
LabN
Man
de
l k S
tati
stic
Test Laboratory
Total Nicotine (mg) Mandel k Chart for SD
Product 1
Product 2
Product 3
Product 4
Product 5
Product 7
Product 8
Man. 0.01
Man. 0.05
Page 55
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 55/57
Figure 25. Nicotine, % of ACM, Mandel h Chart for Lab Means
Figure 26. Nicotine, % of ACM, Mandel k Chart for Lab Standard Deviations
-3.00
-2.00
-1.00
0.00
1.00
2.00
3.00
LabA
LabB
LabC
LabD
LabE
LabF
LabG
LabH
Lab I LabJ
LabK
LabL
LabM
LabN
Man
del
h S
tati
stic
Test Laboratory
Nicotine % of ACM Mandel h Chart for Mean
Product 1
Product 2
Product 3
Product 4
Product 5
Product 7
Product 8
Man. 0.01 U
Man. 0.05 U
Man. 0.05 L
Man. 0.01 L
0.00
0.50
1.00
1.50
2.00
2.50
3.00
3.50
4.00
LabA
LabB
LabC
LabD
LabE
LabF
LabG
LabH
Lab I LabJ
LabK
LabL
LabM
LabN
Man
de
l k S
tati
stic
Test Laboratory
Nicotine % of ACM Mandel k Chart for SD
Product 1
Product 2
Product 3
Product 4
Product 5
Product 7
Product 8
Man. 0.01
Man. 0.05
Page 56
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 56/57
Figure 27. Total Water mg, Mandel h Chart for Lab Means
Figure 28. Total Water mg, Mandel k Chart for Lab Standard Deviations
-3.00
-2.00
-1.00
0.00
1.00
2.00
3.00
LabA
LabB
LabC
LabD
LabE
LabF
LabG
LabH
Lab I LabJ
LabK
LabL
LabM
LabN
Man
del
h S
tati
stic
Test Laboratory
Total Water (mg) Mandel h Chart for Means
Product 1
Product 2
Product 3
Product 4
Product 5
Product 7
Product 8
Man. 0.01 U
Man. 0.05 U
Man. 0.05 L
Man. 0.01 L
0.00
0.50
1.00
1.50
2.00
2.50
3.00
LabA
LabB
LabC
LabD
LabE
LabF
LabG
LabH
Lab I LabJ
LabK
LabL
LabM
LabN
Man
de
l k S
tati
stic
Test Laboratory
Total Water (mg) Mandel k Chart for SD
Product 1
Product 2
Product 3
Product 4
Product 5
Product 7
Product 8
Man. 0.01
Man. 0.05
Page 57
EVAP-089-CTR 2014 Preliminary Aerosol Proficiency Study – October 2017 57/57
Figure 29. Water, % of ACM, Mandel h Chart for Lab Means
Figure 30. Water, % of ACM, Mandel k Chart for Lab Standard Deviations
-3.00
-2.00
-1.00
0.00
1.00
2.00
3.00
LabA
LabB
LabC
LabD
LabE
LabF
LabG
LabH
Lab I LabJ
LabK
LabL
LabM
LabN
Man
del
h S
tati
stic
Test Laboratory
Water % of ACM Mandel h Chart for Means
Product 1
Product 2
Product 3
Product 4
Product 5
Product 7
Product 8
Man. 0.01 U
Man. 0.05 U
Man. 0.05 L
Man. 0.01 L
0.00
0.50
1.00
1.50
2.00
2.50
3.00
3.50
4.00
LabA
LabB
LabC
LabD
LabE
LabF
LabG
LabH
Lab I LabJ
LabK
LabL
LabM
LabN
Man
de
l k S
tati
stic
Test Laboratory
Water % of ACM Mandel k Chart for SD
Product 1
Product 2
Product 3
Product 4
Product 5
Product 7
Product 8
Man. 0.01
Man. 0.05