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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.

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

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.


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.


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).


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


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.


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 % -- --


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 % -- --


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 % -- --



reproducibility for %PG.

PG % of ACM

No. of Labs


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 % -- --


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 % -- --


reproducibility for %Glycerin.

Glycerin

% of ACM

No. of


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 % -- --



reproducibility for total Nicotine.

Total Nicotine mg

No. of Labs


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 % -- --


reproducibility for % Nicotine.

Nicotine % of ACM

No. of Labs


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 % -- --


reproducibility for total water.

Total Water

mg

No. of


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 % -- --



reproducibility for %water.

Water

% of ACM

No. of Labs


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


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


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.


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.


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


4.4 Water

The amount of water per sample will be determined by the method currently in use in each


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.


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.


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.


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.


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


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


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.


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.


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


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)


PG (mg)

GLY (mg)

NIC (mg)

WAT (mg)

Analyte Sum (mg)



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!


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)


PG (mg)

GLY (mg)

NIC (mg)

WAT (mg)

Analyte Sum (mg)



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)


PG

(mg)

GLY

(mg)

NIC

(mg)

WAT

(mg)

Analyte Sum (mg)



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!


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.


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


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


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


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)

N 0.33 mg/pad 3.33 mg/pad 0.33 mg/pad 0.33 mg/pad


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



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


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



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



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



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



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



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



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



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





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



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



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



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



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



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



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



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



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


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



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


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


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


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


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


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

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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


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

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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


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

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LabM

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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

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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


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

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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

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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


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

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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

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LabC

LabD

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LabH

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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


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

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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


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

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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

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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


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

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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

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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


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

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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


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

technical report 2014 preliminary aerosol proficiency study · 2014 preliminary aerosol proficiency...

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