e-cigarette task force - coresta · in 2014, the coresta e-cigarette task force (tf) conducted a...

E-Cigarette Task Force

Technical Report

2014 Electronic Cigarette Aerosol

Parameters Study

March 2015

Task Force Coordinator: Chuck Garner, Ph.D.

R. J. Reynolds, U.S.A.

Task Force Secretary: Robert D. Stevens, Ph.D.

Lorillard Tobacco Company, U.S.A.

Author: Rana Tayyarah

Lorillard Tobacco Company, U.S.A

ECIG-CTR Aerosol Parameters – March 2015 2/89

Table of Contents

1. Summary 3

2. Introduction 3

3. Organisation 4

3.1 Participants 4

3.2 Protocol 4

4. Data - Raw 6

5. Data - Statistical Analysis 6

5.1 Exclusion of Outliers 7

5.2 Calculation of Repeatability and Reproducibility 7

5.3 Calculation of Z-Scores 7

6. Data Interpretation 8

6.1 Machine or product performance issues 8

6.2 Impact of regime on overall yields 8

6.3 Impact on relative yields of analytes 10

6.4 Impact of regime on cumulative yield or puff trending 11

6.5 Trend with flow rate among the test parameters 11

7. Recommendations 12

8. Additional Considerations 12

9. Acknowledgements 12

APPENDIX A: Study Protocol and Data Template 13

APPENDIX D: Total Yield Graphs 80

APPENDIX E: Puff Set Graphs 84

APPENDIX F: ACM Variability - Percent Relative Standard Deviation for Puff Sets 88


1. Summary

In 2014, the CORESTA E-Cigarette Task Force (TF) conducted a collaborative study that included testing of commercial electronic cigarette products. This study was referred to as E-

Cigarette Aerosol Parameters Study. The laboratory phase of this study was conducted from late 2013 to early 2014 and the results were presented to the Task Force in May 2014. The study included determinations of puff count, trapped aerosol, propylene glycol, nicotine, water, glycerin, and product weight loss. Four laboratories participated in the study. Each laboratory tested two products of choice. The goal of this work was to compare results from cigarette-machine puffing of e-cigarettes under a range of puffing parameters to make a recommendation for standardized parameters. From the previous TF meeting, parameters of 55mL volume taken over 3s every 30s using a square profile shape were favored. Thus, the more specific objective was to determine if this regime should be recommended as the standard or if any of the other regimes included in this study should be recommended. The study results demonstrate that any of the regimes evaluated would be suitable for machine-testing of e-cigarettes of a conventional design1 for the determination of major constituents in trapped aerosol. Parameters of 55mL/3s/30s/square will be used for an upcoming proficiency test. These parameters will serve as a recommended machine regime for e-cigarette aerosol collection.

2. Introduction Though electronic cigarettes do not specifically contain tobacco, this is a relatively new product category that is of interest to many CORESTA members. A task force related to electronic cigarettes was formed by the Scientific Commission after a November 2012 workshop. One of the short term objectives of the Task Force is “…to gather and share preliminary data on analysis relevant to e-cigarettes worldwide with a view to making recommendations for product testing”. As yet, there is no standardized method for puffing electronic cigarettes. Thus, evaluation of published literature and conductance of collaborative studies is hindered. At the September 2013 Task Force meeting, there was extensive discussion regarding puffing parameters2. From this discussion it was clear that parameters of 55mL volume taken over 3s every 30s using a square profile shape were favored by the majority of the TF members but that there may be some benefit to an alternate volume (70mL) or an alternate puff duration (4s). Though typical for cigarette smoking, 35 mL puff volume, bell-shaped profiles, and 2s puff duration were each recommended against by researchers as being problematic from some e-cigarette products. The primary concerns discussed related to insufficient product trigger (time/heat), insufficient overlap between the machine (bell) profile and/or machine duration and the start and end times for some products’ puff time. Puff durations of 5s or longer were recommended against as being too long from some products. In order to prepare for a future proficiency study, the Task Force commissioned a study to determine the effect of puff profile on the yield of the major constituents in e-cigarette aerosols in order to recommend puffing parameters for aerosol collection. The study involved comparison of puffing parameters combinations including 55mL and 70mL puff volumes of 3s or 4s duration. Each participating laboratory tested two products of choice for glycerin, propylene glycol, water, and nicotine using six regimes. Since laboratories did not necessarily test the same products, no comparisons were made between any of the products’

1 Self-actuating electronic cigarettes, approximately 25mm circumference with a cylindrical mouth-end 2 See Task Force meeting minutes from the September 2013 meeting for additional detail.


results. Comparisons were limited to understanding the impact of the regimes on yield, consistency of results, and reliability of the testing equipment for each product sample. Essentially, the study data were treated as eight individual studies of the impact of puffing parameters.

3. Organisation

3.1 Participants A list of the participating laboratories is provided in Table 1. The laboratories are listed in alphabetical order. The numerical laboratory codes (1-4) used in this report do not necessarily correspond to the same order as the list below.

Table 1: List of Participating Laboratories

Laboratory

Altria Client Services, Inc.

Arista Laboratories

Enthalpy Analytical, Inc.

Lorillard Tobacco Company

3.2 Protocol Participating laboratories supplied their own samples for testing. White Cloud and Red Kiwi supplied two of the laboratories with products. It was requested that two models, one disposable and one rechargeable, be tested. Sample identification was withheld with data reporting; samples were only identified as “rechargeable” or “disposable”. Participants were directed to store products at room temperature and that batteries be fully charged prior to use for the rechargeable products. Each laboratory conducted five replicate determinations for each product (Table 2) under each of the six regimes (Table 3). Test 1 (ISO) and Test 2 (Health Canada) were included in the study for informational purposes only. Products were tested for one battery charge to a maximum 300 puffs. Puffs were collected in 25 puff increments in a manner typical for each laboratory for e-cigarette aerosol collection. e-Cigarettes were weighed between each set of 25 puffs for calculation of weight loss. Each laboratory tested the samples for the specified analytes using methods of choice. See Appendix A for the study protocol.


Table 2: Sample Identification

Sample ID Description

Lab1-Rechargeable Rechargeable product tested by Laboratory 1

Lab1-3 piece Rechargeable 3 piece-style product tested by Laboratory 1


Lab2-Disposable Disposable product tested by Laboratory 2





Table 3: Collection Puffing Parameters

Regime Code Puff Vol (mL) Duration (s) Shape Frequency Mean Flow

(mL/s) Test 1 * 35/2/60/B 35 2 Bell Every 60s 17.5

Test 2 * 55/2/30/B 55 2 Bell Every 30s 27.5

Test 3 55/3/30/Sq 55 3 Square Every 30s 18.3




*Note: Regime 1 and Regime 2 were not under evaluation because of previously reported issues with some products, but were included for informational purposes because they are based on standardized methods (ISO 3308 and HC-T-115) for traditional cigarette smoking. Where a bell shape profile has a non-constant flow and a square profile has constant flow


The study included determination of trapped aerosol, propylene glycol, nicotine, water, glycerin, and product weight loss. The aerosol collected mass (ACM) which is the measure of total particulates collected and the weight loss of the e-cigarette were determined gravimetrically. Analytes were determined using the method of choice by each laboratory. A comparison of the methods is shown below in Table 4. See Appendix B for summaries of each lab’s methods. Table 4: Analytical Methods Overview In Common Unique Procedures

Collection

• Cerulean SM450 • Standard Puff Engines (≤70mL

puff) • 44mm CFP, Conditioned to

ISO std • Room conditioned to ISO

smoking std

Lab 4 – used smaller labyrinth seals

Sample Prep

• Organic Solvent 10-20mL • Shake to extract • Possible additional dilution for

Gly/PG

Lab 1 – IPA (10mL) 30min Lab 2 – EtOAc (20mL) 30min Lab 3 – IPA (10mL) 20min Lab 4 – n-Propanol (20mL) 30min

Analysis

• GC-TCD for water • Packed column (most)

• GC-FID for other analytes • Capillary column • DB-Wax columns for

most • 6 – 12 calibration standards • Linear (IS) calibration (most) • r

2 >0.99

Lab 1 – Internal Standard: EtOH (water), heptadecane (other analytes) Stabilwax column (nicotine, glycerin, PG) Lab 2 – Internal Standard: 1,3-butanediol DBWax column for water Lab 3 – Internal Standard: EtOH (water), anethole (other analytes), 3 GC runs, Linear (Ext) calibration for glycerin, PG Lab 4 – Internal Standard: quinoline (nic); 1,4-butanediol (other analytes), quadratic (IS) calibration for water, glycerin

4. Data - Raw The summary descriptive statistics data are listed in Appendix C where each mean represents five replicates. Raw data plots are given in Appendix D. The data are displayed as mean with error bars representing one standard deviation.

5. Data - Statistical Analysis The purpose of the study was to gather information in preparation for a proficiency study. This study was not a formal proficiency test; there were four participating laboratories testing samples which were not in common using methodology which were not in common. Thus, many of the statistical analyses typically conducted following the recommendations given in ISO 5725-2 (1994) were not applicable to this data set.


5.1 Exclusion of Outliers Traditional outlier tests were not applied as discussed above. Data for devices that clearly did not function were removed by visual observation. When collecting puff-by-puff (or puff sets, in this case), puffs near the end of the device lifetime, as indicated by significant decrease in ACM yields or from a physical signal (such as a blinking LED) from the product, are typically of a very high variability. End-of-life puff sets yields were included in total yield calculations but the variability information was not included in the overall assessment of the product’s variability under a given regime. In general, for puff set collection if a product or device had a lower than typical yield for a puff set the next puff set would have a higher than typical yield. Therefore, even though there may be puff set to puff set variability for a device, the cumulative yields may be consistent with the other replicates. This must be taken into account when reviewing the results. Also, analytes tend to track with total ACM; if the ACM is low for a measurement all other analytes are low by a similar magnitude. Thus, data were normalized to ACM in order to note any values that did not track with ACM for outlier investigation. Sample Lab1-3 piece was more variable overall compared to the other samples. The laboratory reported an experimental issue that was likely to be the cause of the apparent lower reliability of this sample. The sample’s raw data are included here but the sample’s results were not as heavily considered with regard to the overall conclusions drawn from the study.

5.2 Calculation of Repeatability and Reproducibility

Each laboratory tested unique samples using non-standardized methodology. Thus, repeatability (r) and reproducibility (R) results were not calculated for this data set.

5.3 Calculation of Z-Scores Z-score values cannot be calculated for the data set.


6. Data Interpretation

The objective of the study was to determine if 55mL of a 3s taken every 30s in a square profile (55/3/30/Sq) should be recommended as the standard OR if any of the other regimes should be recommended. To that end, we posed several questions to answer as we evaluated the data.

6.1 ISO and Canadian Intense

Testing using ISO (Test 1) and Canadian Intense (Test 2) puffing parameters were included in the study for informational purposes but were not included in the evaluation for recommending a regime. Exclusion of these regimes was based on discussion at the September 2013 task force meeting during which multiple task force members discussed experience with device failure3 when using bell shape puff profiles. In this study, there were no issues with product performance with either of these regimes. Simply based on the results of this study, either of these regimes would be viable choices if appropriate for a particular study design and product type. The 25 puff block yields were lower for these regimes. Thus, life-time puffing experiments with these parameters would require more puffs (longer collection times) than would be required for testing with the other regimes evaluated in this study.

6.2 Machine or product performance issues At least until e-cigarette-specific aerosol collection machines become more in use, it is important to ensure that the recommended regime will be compatible with conventional smoking machines. Indeed in this study, each participant used conventional 20-port linear smoking machines equipped with standard puff engines capable of a maximum puff volume of 70mL. No technical issues were noted with 55mL puff volume or with either duration used. There were a few technical issues noted for tests with 70mL puff volumes possibly because this is the maximum volume for the puff engines used. One lab reported issues with machine failure with 70mL puff volumes. Two laboratories reported that smoking machine modifications, such as air pressure modifications, were necessary for testing using 70mL puff volumes. No product failures were attributed to any of the smoking regimes. Based on machine performance, 55mL puff volume appears to be more favorable than 70mL.

6.3 Impact of regime on overall yields The aerosol collected mass (ACM) is an indication of overall performance. Results were compared for each sample type between the test regimes. Results were not compared between samples, as there is no expectation that any of the samples were in common between the laboratories. Overall yields were similar for the four regimes under consideration (Tests 3-6 – Table 3); no practical or statistically significant differences were noted for any of the products. Precision for overall yields, as displayed in Appendix D, was similar for each of the regimes, as well.

Additionally, a comparison between e-cigarette mass loss and ACM indicated that results were similar between the regimes tested. Ideally, the mass loss of the e-cigarette and the weight gain of the particulate trap would be virtually the same. As displayed below, the ratio of mass loss to ACM values were near 1 in most cases.

3 No or slow activation


Table 5: Ratio of e-Cigarette Mass Loss to ACM

Lab1-Rechargeable

Lab2-Disposable

Lab2-Rechargeable

Lab3-Disposable

Lab3-Rechargeable

Lab4-Disposable

Lab4-Rechargeable

35/2/60/B 1.0 0.9 0.9 1.1 0.9 1.0 0.9 55/2/30/B 1.0 1.0 0.9 1.1 1.1 1.0 0.9 55/3/30/Sq 1.0 1.0 1.0 1.1 1.0 1.0 0.9 55/4/30/Sq 0.4 1.0 1.0 1.1 1.1 1.0 1.0 70/3/30/Sq 1.0 1.0 1.0 1.1 1.1 1.0 0.9 70/4/30/Sq 1.0 1.0 1.0 1.1 1.0 1.0 1.0

Sample Lab1-3 piece was excluded from this comparison due to experimental issues; raw data are shown in Appendix C

Thus, there is no advantage for any of the alternative regimes versus Test 3, 55/3/30/Sq, for overall (ACM) yields.


6.4 Impact on relative yields of analytes Another consideration is whether different regimes would give a different proportion of the analytes tested. Thus the percent of analyte in the ACM was calculated as Analyte (mg) / ACM (mg) x 100. As shown in the table below as the range and the percent difference in composition for each regime, in most cases the percent composition varied by no more than 10% among the regimes for a given sample except for water. For example, for sample Lab1-Rechargeable, the percent composition of nicotine was 1.22%, 1.24%, 1.21%, and 1.24% for Tests 3, 4, 5, and 6, respectively. This is a range of 0.03pt (as an absolute value) or 2% (calculated as percent difference). Thus, there appears to be no impact on the composition of the ACM based on regime choice for the regimes tested. Table 6: Range in Analyte Percent Composition across the Regimes for each Sample

As % Composition

Total PG Total Nicotine Total Glycerin Total Water Lab1-Rechargeable 47-48 1.2-1.2 26-27 11-13 Lab2-Disposable 56-58 1.8-1.9 28-29 8-11 Lab2-Rechargeable 57-59 1.8-1.9 28-29 8-12 Lab3-Disposable NA 1.6-1.6 71-76 20-20 Lab3-Rechargeable NA 1.3-1.4 72-76 15-16 Lab4-Disposable 42-47 1.0-1.2 33-39 15-18 Lab4-Rechargeable 34-41 1.4-1.5 41-44 11-13

As % Difference* in % Composition

Total PG Total Nicotine Total Glycerin Total Water Lab1-Rechargeable 3% 2% 4% 21% Lab2-Disposable 4% 4% 5% 33% Lab2-Rechargeable 3% 3% 4% 32% Lab3-Disposable NA 1% 6% 3% Lab3-Rechargeable NA 2% 7% 9% Lab4-Disposable 10% 22% 16% 21% Lab4-Rechargeable 19% 8% 6% 17%

*Calculated as (2(Max %Composition-Min %Composition))/(Max+Min)x100 Sample Lab1-3 piece was excluded from this comparison due to experimental issues; raw data are shown in Appendix C


6.5 Impact of regime on cumulative yield or puff trending The ACM was collected discretely rather than in total; 25 puffs were collected per pad up to 300 puffs. Thus delivery profile trends may be assessed. While the overall yields were similar among the regimes, the delivery profiles were impacted by puff duration (2s vs 3s), but not by puff volume. This trending is exemplified below for one of the samples. Trend lines for the regimes using 3s duration, 55/3/30/Sq and 70/3/30/Sq, are virtually identical. While trend lines for the 4s duration regimes, 55/4/30/Sq and 70/4/30/Sq, also group together. Note also that the 4s trends have higher yields and fewer puff sets than the 3s trends. All trend lines are displayed in Appendix E.

While there appears to be a pattern to the puff set profiling based on duration, there is no advantage for any of the alternative regimes versus Test 3, 55/3/30/Sq, for cumulative yield.

Figure 1: Puff Set Trending for Sample Lab 2 Rechargeable ACM (mg) Yield per pad.

6.6 Difference in yield variability The relative standard deviation (%RSD) was calculated for each pad set to determine if any of the regimes appeared to have improved precision. End-of-unit life puffs would be expected to be highly variable no matter the regime. Thus partial last puff sets were not considered in the evaluation of variability. Collection variability results calculated as the percent relative standard deviation (%RSD) of the ACM delivery for each pad set are shown in Appendix F. Puff set precision was relatively high and generally similar among and between the sets. For all products tested, 80% of the RSD values were less than 15% regardless of regime. There is no advantage for any of the alternative regimes versus Test 3, 55/3/30/Sq, for variability.

6.7 Trend with flow rate among the test parameters

One of the questions in the case of product failure for machine vaping relates to whether the flow rate is sufficient to activate the device. At the September 2013 meeting, TF participants discussed device failure issues for some products if the flow rate was not sufficient for device activation. A flowrate of 13.8 mL/s (55mL/4s) was specifically discussed as problematic. In this study, flow rates ranged from 13.8 mL/s to 23.3 mL/s and there were no apparent product failures due to regime (i.e. flow rate). There was no clear trending in yield when compared based on flow rate. Note that the number and range of products tested was limited. Thus, flow rate may still be a concern for less conventional products. Thus, the task force would be hesitant to recommend a regime using 55mL with 4s without additional testing.

0.00

20.00

40.00

60.00

80.00

100.00

120.00

140.00

AC

M (

mg/

pad

)

Puff Number

Test 3 - 55/3/30/Sq

Test 4 - 55/4/30/Sq

Test 5 - 70/3/30/Sq

Test 6 - 70/4/30/Sq


7. Recommendations

Based on discussions during TF meetings:

• A 70-mL puff volume may be problematic for smoking machine designs with 70mL as the maximum volume.

• Parameters which result in a low flow rate (i.e. 55mL with a 4s duration) may result in device failure depending on the product being tested.

• Puffing parameters using bell profile shapes may be problematic for some product types due to air flow issues.

Based on results from this study:

• Overall, yields were similar for the four test regimes.

• Delivery profile trends were dependent on puff duration and not on puff volume.

• Precision was acceptable and similar for all regimes.

• There were no technical advantages among the regimes tested.

Thus, based on TF discussion and on the results of this study, Test Regime 3 (a square 55mL puff, 3s in duration, taken twice a minute), was recommended for adoption as an interim standard vaping regime for e-cigarette testing. Choice of regime parameters may need to be refined as additional product types are tested.

8. Additional Considerations Limitations to the work that should be considered include:

• Only products of a conventional design were included in the study.

• Puff volume and combinations of volume and duration were limited by capabilities of conventional smoking machines in standard configuration.

• Reference products and standardized analytical methodology do not exist for e-cigarette aerosol collection at this time.

Reporting units that may be useful for fostering a collective understanding of the research include mg/pad for incremental collection, mg/ total puffs for total collection on a single pad. In addition to analytes of interest collection and reporting of ACM, puff counts, and e-cigarette weight change are useful quality measures and would aid collaborative understanding of results.

9. Acknowledgements The study team, Drs. Rob Stevens, Narendra Meruva, and Gene Gillman; the participating laboratories; and White Cloud and Red Kiwi that supplied some of the e-cigarettes for testing are greatly appreciated.


APPENDIX A: Study Protocol and Data Template

CORESTA E-CIGARETTE

ANALYTICAL TESTING SUB TEAM

(Team Leader – Dr. Rob Stevens, Lorillard

Tobacco)

Project Title: 2013 Major constituents in e-cigarette aerosol

Date: Nov 11, 2013

Written by: Gene Gillman, Ph.D. (Enthalpy Analytical)

Email: [email protected]

Phone: 1-919-949-2491

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 taskforce

members.

mailto:[email protected]


Study Protocol to Determine the Effect of Puff Profile on the Yield of the Major Constituents in E-Cigarette Aerosol

1. Objective The main objective of this study to determine the effect of puff profile on the yield of the major constituents in e-cigarette aerosol. This study will include six puff profiles or test conditions with various puff volumes, durations and puff shapes.

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. Analytes and Methods 3.1 Puff Count Puff count for each puffing increment (each pad) will be recorded. For most data points the puff count will be 25. For products which extinguish prior to 300 puffs there may be pads with fewer than 25 puffs. The actual puff count should be recorded. Record as count/pad in the data template.

3.2 Trapped Aerosol The total collected aerosol mass (ACM) for each sample will be determined 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 weight after collection – pad weight before collection). Record as mg/pad in the data template. This test measurement is akin to total particulate matter (TPM) for conventional cigarette testing.

3.3 Weight loss The amount of material lost from each e-cigarette will be determined by measuring the e-cigarette before and after each collection event. The total amount of weight loss will be determined by difference in mass (e-cigarette weight after collection – e- cigarette weight before collection). Record as mg in the data template.

3.4 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.

3.6 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.

3.7 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.



4. Samples 4.1 Required materials Each participating laboratory shall supply product for their own testing. Two models shall be tested. These should include both a rechargeable model and disposable model.

These two brands do not have to be products from the same manufacturer. A minimum of 30 e-cigarettes for each brand is required to fulfill the study design.

4.2 Sample Handling All samples should be stored at room temperature.

Rechargeable devices should be charged before use. A single battery charge will be used for each new cartomizer. Note: Only one battery charge will be used for each cartomizer.

5. Experimental plan Five replicates for each e-cigarette under each test condition is required. If possible, it is requested that all samples for a test condition be analyzed on a single day.

A series of discreet samples will be collected from each e-cigarette (disposable or cartomizer). For each e-cigarette, samples will be collected in 25 puffs increments (1-25, 26-50 and etc.) until the battery is depleted. Five e-cigarettes should be tested under each test condition.

For each aerosol sample, laboratories are asked to determine weight lost from the device, amount of ACM trapped, nicotine, propylene glycol, glycerin, and water. Data will be reported on a per mg basis.

Aerosol should be generated from each type of e-cigarette using the test conditions given in Table 1. Note that Tests 1 and 2 use puffing parameters specified in for ISO smoking (ISO 3308) and Canadian Intense smoking (HC-T-114) of conventional cigarettes. This protocol does not attempt to make any other specifications with regard to these two standard smoking regimes (i.e. room conditions).

Note: Five e-cigarettes should be tested under each test condition. Table 1: Test Conditions to be used for this study

Test Puff Volume Shape Frequency Duration Note 1 35 Bell* Every 60 Sec 2 Sec ISO 3308 Puffing

Parameters

2 55 Bell* Every 30 Sec 2 Sec HC-T-114 Puffing Parameters (without tape)

3 55 Square# Every 30 Sec 3 Sec 4 55 Square# Every 30 Sec 4 Sec 5 70 Square# Every 30 Sec 3 Sec 6 70 Square# Every 30 Sec 4 Sec

* Bell Shape is an ISO 3308 type puff profile # Square Shape is a constant flow rate profile

Note: Rechargeable devices must be tested using a new cartomizer and fully charged battery. Samples will be collected until the battery is discharged. Only one battery charge is to be used per cartomizer.


6. Data Submission The attached templates 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]) on or before Feb 14th, 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. Timescale First week of December 2013 All documents will be distributed to participating laboratories

o Protocol of the study o Report form

December 2013/January 2014 Laboratories will perform the study

Mid February The results must be sent to the data coordinator on or before February 14th 2014 in order to give to the statistician sufficient time to evaluate the data. Data received after February 14th will not be included in the draft report discussed at the May meeting.

March/April 2014 The statistician will perform the data analysis and the Task Force coordinators will format the data for presentation.

May 2014 The taskforce member will assess the results of the collaborative study during the next taskforce meeting.



Laboratory name

Company Representative (Title, Name)

Address

Tel

Fax

E-mail address

Data Sheet for 2013 Major Constituents in e-Cigarette AerosolParameters Study

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.

Note: Please return this completed spreadsheet to [email protected] by February 14, 2014.


Method Details (example) ACM Nicotine Water Glycerin PGSample HandlingStorage prior to testing unopened at 65% RH 72FAdditional Details

Type of Aerosol

Collection Machine

Style (Include a description of features if non-standard equipment was used) Linear Smoking Machine

Make Cerulean SM450Vaping was Concurent for Which analytes? All were concurrent

Room Conditions during aerosol collection 65 %RH, 72F

Additional Details for Aerosol Collection

Trapping SystemFilter 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, 30minAdditional Filtration PTFE: 0.45umAdditional 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 EquipmentDescription Agilent GC/MS, EI in SIM mode using detuerated 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 analysisReference --Quantitation

InformationLimit of Quantitation (mg/pad)Limit of Detection (mg/pad)Number of standardsConcentration of each StandardInternal Standard Ethanol (water), Anethole (others)Calibration Type linear, with ISr2

Additional Details

0

Method Synopsis: please type an overall summary of your method in this box and provide specific details below

*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.


Please paste in a picture of an example chromatogram for a calibration standard and for one or more samples for chromatographic methods

0

Please paste pictures relevant to any unusual observations noted during testing. Please include text explanation as necessary.


Condition Volume Shape Frequency Puff Duration NOTESTest 1 35 Bell Every 60 Sec 2 Sec ISO 3308 Puffing ParametersTest 2 55 Bell Every 30 Sec 2 Sec HC-T-114 Puffing Parameters (without tape)Test 3 55 Square Every 30 Sec 3 SecTest 4 55 Square Every 30 Sec 4 SecTest 5 70 Square Every 30 Sec 3 SecTest 6 70 Square Every 30 Sec 4 Sec

0


Sample 1 - Test 1

Sample Description

Test ConditionsPuff Volume

(mL) Shape Frequency Duration

Test 1 35 Bell Every 60 Sec 2 Sec

Testing DatesCollection Extraction Analyses

Test 1

Observations

Testing Summary Total PuffsTotal ACM

Total PG

Total Nicotine

Total Glycerin

Total Water

mg mg mg mg mg

0 0 0 0 0 0

Sample 1

Note: Please include under "observations" information about anything unusual in the behavior, etc of the samples. For example, unusual colors, smells, "spitting" (droplets inside pad holder and/or on pad).

0

Note: e-Cigarette brand names are not needed. At a minimum, indicate "rechargable" or "disposable" as a sample description.

Note: If photograph(s) would be helpful to demonstrate an unusual observation, please paste in on the chromatogram and photos tab with text to explain.


Sample 1 - Test 1

Test Conditions Puff Volume Shape Frequency DurationTest 1 35 Bell Every 60 Sec 2 Sec

Puff Count Puffs Replicate 1 Replicate 2 Replicate 3 Replicate 4 Replicate 50-2526-5051-75

76-100101-125126-150151-175176-200201-225226-250251-275276-300

Weight Loss Puffs Replicate 1 Replicate 2 Replicate 3 Replicate 4 Replicate 5(mg/device) 0-25

26-5051-75

76-100101-125126-150151-175176-200201-225226-250251-275276-300

0

Note: Later puff sets may not be a full 25 puffs. Record the actual puff counts for these pads.

Note: Puffing should be ceased after one battery discharged OR after 300 puffs, whichever comes first.


Sample 1 - Test 1




ACM Puffs Replicate 1 Replicate 2 Replicate 3 Replicate 4 Replicate 5(mg/pad) 0-25

26-5051-75

76-100101-125126-150151-175176-200201-225226-250251-275276-300

PG Puffs Replicate 1 Replicate 2 Replicate 3 Replicate 4 Replicate 5(mg/pad) 0-25

26-5051-75

76-100101-125126-150151-175176-200201-225226-250251-275276-300

0


Sample 1 - Test 1




Nicotine Puffs Replicate 1 Replicate 2 Replicate 3 Replicate 4 Replicate 5(mg/pad) 0-25

26-5051-75

76-100101-125126-150151-175176-200201-225226-250251-275276-300

Glycerin Puffs Replicate 1 Replicate 2 Replicate 3 Replicate 4 Replicate 5(mg/pad) 0-25

26-5051-75

76-100101-125126-150151-175176-200201-225226-250251-275276-300

Water Puffs Replicate 1 Replicate 2 Replicate 3 Replicate 4 Replicate 5(mg/pad) 0-25

26-5051-75

76-100101-125126-150151-175176-200201-225226-250251-275276-300

0


APPENDIX B: Laboratory Method Summaries and Example Chromatograms Laboratory 1 Method Summary

Nicotine Water Glycerin PG

Sample Handling

Storage prior to testing unopened at 65% RH 72F unopened at 65% RH 72F unopened at 65% RH 72F 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 Linear Smoking Machine Linear Smoking Machine Linear Smoking Machine

Make Cerulean SM450 Cerulean SM450 Cerulean SM450 Cerulean SM450

Vaping was Concurrent for Which analytes? All were concurrent All were concurrent All were concurrent All were concurrent

Room Conditions during aerosol collection 65 %RH, 72F 65 %RH, 72F 65 %RH, 72F 65 %RH, 72F



Laboratory 1 Method Summary (continued)

Trapping System Nicotine Water Glycerin PG

Filter Pad / Diameter CFP 44 mm CFP 44 mm CFP 44 mm CFP 44 mm

Were filter pads conditioned? Yes, 62+/-%RH, 75F Yes, 62+/-%RH, 75F Yes, 62+/-%RH, 75F Yes, 62+/-%RH, 75F

Trap Type + Number of Traps

Solvent 10 mL 2-Propanol 10 mL 2-Propanol 10 mL 2-Propanol 10 mL 2-Propanol

Extraction wrist-action shaker, 30min

wrist-action shaker, 30min



Additional Filtration

Additional sample processing prior to analysis

Additional Details extracts analyzed

same day for Nic/Water /Gly/PG

extracts analyzed same

day for Nic/Water /Gly/PG

extracts analyzed same day for Nic/Water

/Gly/PG

extracts analyzed same day for Nic/Water

/Gly/PG



Analytical Equipment Nicotine Water Glycerin PG

Description Agilent 58/90 GC Series II FID/TCD

Agilent 5890 GC Series II FID/TCD



Detection Systems + Conditions Column: Restek Stabilwax 30mX0.32mmX1.0Um, 1ul injection

Column: Supelco Porapak R 6ft. X 1/8 inch ID

Column: Restek Stabilwax 30mX0.32mmX1.0Um, 1ul injection

Column: Restek Stabilwax 30mX0.32mmX1.0Um, 1ul injection

Additional Details

Reference



Quantitation Information Nicotine Water Glycerin PG

Limit of Quantitation (mg/pad) 0.0514 0.4952 0.3312 0.2548

Limit of Detection (mg/pad) 0.0051 0.0495 0.0331 0.0255 Number of standards 7 6 10 10

Concentration of each Standard 0.0514, 0.103, 0.257, 0.514, 0.771, 1.03, 1.23 mg/mL

0.495, 1.24, 2.48, 3.71, 4.95, 5.94 mg/mL

0.331, 0.662, 1.66, 3.31, 4.97, 6.62, 7.95, 9.93, 13.2, 33.1 mg/mL

0.255, 0.510, 1.27, 2.55, 3.82, 5.10, 6.11, 7.64, 10.2, 25.5 mg/mL

Internal Standard Ethanol (water), Heptadecane (others)

Ethanol (water), Heptadecane (others)



Calibration Type linear, with IS linear, with IS linear, with IS linear, with IS r2 0.999179 0.999354 0.999452 0.999613 Additional Details


Figure 1: Laboratory 1 Example Chromatogram – Aerosol Sample



Figure 3: Laboratory 1 Example Chromatogram – Calibration Standard



Laboratory 2 Method Summary


Sample Handling

Storage prior to testing Unopened; room temp.

Unopened; room temp.



Additional Details N/A N/A N/A N/A

Type of Aerosol Collection Machine


Linear Smoking Machine







Additional Details for Aerosol Collection N/A N/A N/A N/A





Were filter pads conditioned? Yes, 60±2% RH; 22±2°C

Yes, 60±2% RH; 22±2°C

Yes, 60±2% RH; 22±2°C

Yes, 60±2% RH; 22±2°C

Trap Type + Number of Traps N/A N/A N/A N/A

Solvent 20 mL EtOAc 20 mL EtOAc 20 mL EtOAc 20 mL EtOAc

Extraction wrist-action shaker, 30min




Additional Filtration N/A N/A N/A N/A

Additional sample processing prior to analysis N/A N/A N/A N/A





Description Agilent 7890 GC-FID Agilent 6890 GC-TCD Agilent 7890 GC-FID Agilent 7890 GC-FID

Detection Systems + Conditions Column: RTXWax (30mx0.32mmx1µm); Split 20:1; 120 °C to 250 °C (11 °C/min ramp); 1

minute hold; 1 µL injection volume

Column: DBWax (30mx0.53mmx1µm); 50 °C to

240 °C (20 °C/min ramp); 1 minute hold; 0.5 µL injection

volume

Column: RTXWax (30mx0.32mmx1µm);

Split 20:1; 120 °C to 250 °C (11 °C/min ramp); 1


Column: RTXWax (30mx0.32mmx1µm);

Split 20:1; 120 °C to 250 °C (11 °C/min ramp); 1


Additional Details

Reference




Limit of Quantitation (mg/pad) 0.02 0.4 0.1 0.04

Limit of Detection (mg/pad) N/A N/A N/A N/A

Number of standards 12 8 12 12

Concentration of each Standard 1-1000 µg/mL 20 - 2000 µg/mL 5-15000 µg/mL 2 - 15000 µg/mL

Internal Standard 1,3-butanediol 1,3-butanediol 1,3-butanediol 1,3-butanediol

Calibration Type Linear; 1/x2 Linear; 1/x2 Linear; 1/x2 Linear; 1/x2

r2 ≥0.99950 ≥0.99950 ≥0.99950 ≥0.99950





Sample Handling

Storage prior to testing unopened at 65% RH 72F

unopened at 65% RH 72F



Additional Details










Additional Details for Aerosol Collection One vape run, nic water

concurrent, gly/pg concurrent

One vape run, nic water concurrent, gly/pg concurrent







Were filter pads conditioned? Yes, 62+/-%RH, 75F Yes, 62+/-%RH, 75F Yes, 62+/-%RH, 75F Yes, 62+/-%RH, 75F

Trap Type + Number of Traps NA NA NA NA

Solvent 10 ml IPA 10 ml IPA

Extraction 20min shake 20min shake 20min shake 20min shake

Additional Filtration NA NA NA NA

Additional sample processing prior to analysis Additional dilution for Gly based on ACM

Additional Details extracts analyzed same

day for Nic/Water next day for Gly/PG

extracts analyzed same day for Nic/Water next day

for Gly/PG

Samples were diluted if nec for gly

Samples were diluted if nec for gly



Description GC-FID GC-TCD (dual column with Nic analysis) GC-FID GC-FID


Agilent DB-Wax (10 m x 0.18 mm x 0.3 µm film)

Splitless (purge time 0.5 min, 50mL/min) 100

5.8 psi 40 mL/min

400 mL/min 160°C hold for 0.5 minutes

80°C/minute to 200 °C 50 °C/ minute to 225°C hold 2.0 min.

Stainless steel Packed column Haye Sep-Q 60/80

mesh; 3' x 1/4", or equivalent); on-column

injection; He pressure 9psi; initial temp 160C

DB-Wax Analytical GC column (15m X

0.25mm ID)(0.25 µm film thickness)

DB-Wax Analytical GC column (15m X 0.25mm

ID)(0.25 µm film thickness)

Additional Details

Reference




Limit of Quantitation (mg/pad) 0.2529 0.0065

Limit of Detection (mg/pad) 0.02529 0.00065 Number of standards 7 7 5 7

Concentration of each Standard (mg/mL) 0, 0.05, 1.15, 0.20, 0.25, 0.50, 1.0

(mg/mL) 0, 0.25, 0.75, 1.25, 2.5, 5.0, 1.0

(mg/mL) 0.025, 0.099, 0.25, 1.2, 2.5

(mg/mL) 0.00064, 0.0064, 0.04, 0.16, 0.40,

2.0, 4.0

Internal Standard Ethanol (water), Anethole (others)

Ethanol (water), Anethole (others)



Calibration Type linear, with IS linear, with IS linear, with IS linear, with IS r2 > 0.995 > 0.995 > 0.995 > 0.995 Additional Details




Sample Handling

Storage prior to testing Samples stored under ambient conditions

Samples stored under ambient conditions



Additional Details


Style (Include a description of features if non-standard equipment was used) Linear smoking machine Linear smoking machine Linear smoking machine Linear smoking machine

Make Cerulean Cerulean Cerulean Cerulean


Room Conditions during aerosol collection 60 ± 4 %RH, 72 ± 5 °F 60 ± 4 %RH, 72 ± 5 °F 60 ± 4 %RH, 72 ± 5 °F 60 ± 4 %RH, 72 ± 5 °F


Based on the collected aerosol mass, the

amount of extraction solution to be added is

adjusted



adjusted



adjusted



adjusted




Filter Pad / Diameter CFP 44mm CFP 44mm CFP 44mm CFP 44mm

Were filter pads conditioned? 60 ± 3 %RH, 72 ± 2 °F 60 ± 3 %RH, 72 ± 2 °F 60 ± 3 %RH, 72 ± 2 °F 60 ± 3 %RH, 72 ± 2 °F

Trap Type + Number of Traps N/A N/A N/A N/A

Solvent 20 mL of dry n-propanol extraction solution

20 mL of dry n-propanol extraction solution

20 mL of dry n-propanol extraction

solution

20 mL of dry n-propanol extraction

solution

Extraction 30 min mixing time on an orbital shaker

30 min mixing time on an orbital shaker



Additional Filtration N/A N/A N/A N/A

Additional sample processing prior to analysis

Samples were diluted 1:10 with extraction solution for PG and Glycerin




Additional Details

Care must be taken to ensure all glassware used for standard and sample preparation is free of residual water.







Description

Agilent GC equipped with dual hot split/splitless injection ports and dual detectors (FID and TCD).





Columns: Two DB-ALC1 capillary columns (front and back), 30m x 0.32 mm ID, 1.8 µm film thickness. Oven Programming: 90°C for 1min, 15°C/min to 120°c, 40°C to 280°C for 2min, Bake time 2 min, total run time 9 min, Injection port temperatures of 250°C, GC-FID - 1µL injection at 25:1 split and carrier gas flow of 3mL/min.

Columns: Two DB-ALC1 capillary columns (front and back), 30m x 0.32 mm ID, 1.8 µm film thickness. Oven Programming: 90°C for 1min, 15°C/min to 120°c, 40°C to 280°C for 2min, Bake time 2 min, total run time 9 min, Injection port temperatures of 225°C, GC-TCD - 2µL injection at 10:1 split and carrier gas flow of 1.5mL/min.



Additional Details

n-Propanol extraction solvent is stored dried with molecular sieves (5 g per liter of extraction solution) to remove any trace levels of water contamination.




Reference N/A N/A N/A N/A




Limit of Quantitation (mg/pad) 51.1 µg/mL 516 µg/mL 50.7 µg/mL 49.3 µg/mL

Limit of Detection (mg/pad) 16.9 µg/mL 170 µg/mL 16.7 µg/mL 16.3 µg/mL Number of standards 6 6 6 6

Concentration of each Standard 50, 100, 250, 500, 1000, 2000

500, 1000, 2500, 5000,

10000, 20000

50, 100, 250, 500, 1000, 2000

50, 100, 250, 500, 1000, 2000

Internal Standard Quinoline (FID) 1,4-Butanediol (TCD) 1,4-Butanediol (FID) 1,4-Butanediol (FID)

Calibration Type Linear, with IS Quadratic, with IS Quadratic, with IS Linear, with IS

r2 >0.990 >0.990 >0.990 >0.990 Additional Details N/A N/A N/A N/A


APPENDIX C: Raw Data Means Raw data are presented as means ± 1 standard deviation for puff sets and for total yields Results for puff sets with average ACM values <6mg are not reported. Lab1-3 piece Puff Set Data – Puff Count

35/2/60/B 55/2/30/B 55/3/30/Sq 55/4/30/Sq 70/3/30/Sq 70/4/30/Sq Puffs Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev 0-25 25 0 25 0 25 0 25 -- 25 0 25 0 26-50 25 0 25 0 25 0 25 -- 25 0 25 0 51-75 25 0 25 0 25 0 25 -- 25 0 25 0

76-100 25 0 25 0 25 0 25 -- 25 0 25 0 101-125 25 0 25 0 25 0 25 -- 25 0 20 7 126-150 25 0 25 0 25 0 25 -- 24 2 8 -- 151-175 25 0 25 0 18 8 -- -- 4 1 -- -- 176-200 25 0 25 0 -- -- -- -- -- -- -- -- 201-225 25 0 25 0 -- -- -- -- -- -- -- -- 226-250 25 0 24 2 -- -- -- -- -- -- -- -- 251-275 25 0 23 5 -- -- -- -- -- -- -- -- 276-300 25 0 19 5 -- -- -- -- -- -- -- --

Lab1-3 piece Puff Set Data – Weight Loss (mg)

35/2/60/B 55/2/30/B 55/3/30/Sq 55/4/30/Sq 70/3/30/Sq 70/4/30/Sq Puffs Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev 0-25 9.87 16.50 40.12 7.35 62.63 5.70 94.20 -- 84.30 10.56 108.13 15.88 26-50 26.13 19.63 37.98 6.56 54.03 8.30 83.30 -- 71.14 10.98 84.80 12.79 51-75 22.10 18.47 37.62 6.78 47.20 9.99 78.10 -- 66.68 8.61 64.05 19.24

76-100 28.27 7.10 35.58 4.65 47.07 5.62 67.80 -- 59.74 10.68 59.15 30.99 101-125 27.10 3.67 34.36 5.53 43.50 3.30 41.20 -- 53.68 8.10 39.95 27.53 126-150 26.63 2.96 31.70 4.36 34.05 2.90 -- -- 42.76 4.63 -- -- 151-175 27.73 4.86 29.08 2.75 10.75 2.47 -- -- -- -- -- -- 176-200 26.27 3.01 25.84 4.45 -- -- -- -- -- -- -- -- 201-225 24.63 2.57 26.14 1.80 -- -- -- -- -- -- -- -- 226-250 24.17 0.31 21.70 4.16 -- -- -- -- -- -- -- -- 251-275 25.87 0.93 19.30 8.75 -- -- -- -- -- -- -- -- 276-300 19.47 5.44 10.07 8.66 -- -- -- -- -- -- -- --


Lab1-3 piece Puff Set Data – ACM (mg)


76-100 25.97 4.31 35.08 4.60 45.23 6.00 65.50 -- 55.94 9.69 60.65 29.34 101-125 26.23 4.08 33.12 4.21 42.67 4.93 41.90 -- 52.72 8.43 37.68 24.45 126-150 26.57 2.93 28.24 6.47 33.15 3.61 -- -- 40.38 4.82 -- -- 151-175 24.90 3.17 28.84 2.60 9.35 1.63 -- -- -- -- -- -- 176-200 26.03 3.02 25.66 4.27 -- -- -- -- -- -- -- -- 201-225 23.70 2.14 24.94 2.12 -- -- -- -- -- -- -- -- 226-250 24.43 0.15 20.84 4.40 -- -- -- -- -- -- -- -- 251-275 23.53 0.67 18.35 8.21 -- -- -- -- -- -- -- -- 276-300 19.60 5.11 9.00 7.78 -- -- -- -- -- -- -- --

Lab1-3 piece Puff Set Data – Propylene Glycol (mg)


76-100 6.98 1.51 11.03 1.50 12.78 1.77 0.80 -- 19.85 6.45 21.99 10.88 101-125 7.03 1.35 10.34 1.17 12.40 1.42 0.90 -- 20.86 8.71 15.54 9.50 126-150 7.09 0.75 8.74 2.01 9.86 1.02 -- -- 17.73 9.22 -- -- 151-175 6.78 1.00 9.81 1.35 3.56 0.67 -- -- -- -- -- -- 176-200 6.96 1.00 8.01 1.18 -- -- -- -- -- -- -- -- 201-225 6.65 0.41 7.87 0.77 -- -- -- -- -- -- -- -- 226-250 6.52 0.34 7.12 1.19 -- -- -- -- -- -- -- -- 251-275 6.76 0.30 6.30 2.61 -- -- -- -- -- -- -- -- 276-300 5.63 1.24 3.61 2.43 -- -- -- -- -- -- -- --


Lab1-3 piece Puff Set Data – Glycerin (mg)


76-100 9.99 1.11 14.63 1.79 16.58 2.43 23.41 -- 19.85 6.45 14.43 10.97 101-125 10.23 1.06 13.78 1.41 16.12 1.49 0.00 -- 16.08 5.07 9.16 6.45 126-150 9.81 0.37 11.66 2.79 12.13 1.90 -- -- 12.18 2.93 -- -- 151-175 9.18 0.80 12.99 1.65 4.25 0.21 -- -- -- -- -- -- 176-200 9.04 0.31 10.50 1.34 -- -- -- -- -- -- -- -- 201-225 8.08 2.31 9.92 0.77 -- -- -- -- -- -- -- -- 226-250 8.05 2.06 8.44 1.49 -- -- -- -- -- -- -- -- 251-275 7.47 2.85 7.09 2.91 -- -- -- -- -- -- -- -- 276-300 8.74 0.23 4.01 2.43 -- -- -- -- -- -- -- --

Lab1-3 piece Puff Set Data – Nicotine (mg)


76-100 0.35 0.08 0.49 0.07 0.61 0.08 0.87 -- 0.80 0.12 0.82 0.44 101-125 0.34 0.05 0.47 0.06 0.58 0.06 0.00 -- 0.76 0.11 0.72 0.15 126-150 0.35 0.02 0.41 0.10 0.45 0.08 -- -- 0.61 0.07 -- -- 151-175 0.34 0.05 0.46 0.06 0.15 0.00 -- -- -- -- -- -- 176-200 0.33 0.02 0.38 0.05 -- -- -- -- -- -- -- -- 201-225 0.34 0.03 0.36 0.04 -- -- -- -- -- -- -- -- 226-250 0.34 0.03 0.32 0.06 -- -- -- -- -- -- -- -- 251-275 0.33 0.01 0.23 0.16 -- -- -- -- -- -- -- -- 276-300 0.31 0.01 0.09 0.15 -- -- -- -- -- -- -- --


Lab1-3 piece Puff Set Data – Water (mg)


76-100 4.28 0.90 7.01 1.20 6.80 1.60 10.94 -- 8.32 1.58 9.17 6.09 101-125 4.43 0.88 5.31 0.78 7.22 0.26 0.00 -- 7.90 1.75 6.05 2.76 126-150 3.50 1.37 4.37 1.35 3.85 0.42 -- -- 4.95 1.57 -- -- 151-175 3.93 0.15 14.11 8.19 -- -- -- -- -- -- -- -- 176-200 3.67 0.39 26.28 6.35 -- -- -- -- -- -- -- -- 201-225 2.32 1.19 5.44 3.65 -- -- -- -- -- -- -- -- 226-250 2.64 0.95 4.68 4.04 -- -- -- -- -- -- -- -- 251-275 2.90 2.21 1.06 0.85 -- -- -- -- -- -- -- -- 276-300 1.75 0.25 0.00 0.00 -- -- -- -- -- -- -- --

Lab1-Rechargeable Puff Set Data – Puff Count

35/2/60/B 55/2/30/B 55/3/30/Sq 55/4/30/Sq 70/3/30/Sq 70/4/30/Sq Puffs Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev 0-25 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 8.00 1.58 25.00 0.00 26-50 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 51-75 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00

76-100 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 101-125 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 126-150 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 151-175 25.00 0.00 25.00 0.00 25.00 0.00 21.00 0.00 25.00 0.00 9.80 4.82 176-200 25.00 0.00 25.00 0.00 25.00 0.00 -- -- 25.00 0.00 -- -- 201-225 25.00 0.00 25.00 0.00 10.40 8.91 -- -- 25.00 0.00 -- -- 226-250 25.00 0.00 25.00 0.00 -- -- -- -- -- -- -- -- 251-275 25.00 0.00 25.00 0.00 -- -- -- -- -- -- -- -- 276-300 25.00 0.00 25.00 0.00 -- -- -- -- -- -- -- --


Lab1-R Puff Set Data – Weight Loss (mg)


76-100 44.92 11.92 46.46 9.28 77.88 15.11 109.50 10.04 78.14 11.07 102.98 13.12 101-125 38.08 4.96 51.42 3.40 65.78 34.11 99.45 2.62 70.76 18.53 90.30 14.26 126-150 40.28 6.51 40.46 4.54 76.02 4.42 93.05 7.57 78.66 26.63 87.68 12.65 151-175 35.74 8.25 41.28 2.94 68.36 16.98 145.90 -- 78.58 10.03 25.66 15.70 176-200 36.48 4.43 36.72 4.44 72.00 9.61 -- -- 64.68 9.31 -- -- 201-225 35.32 7.09 37.82 6.30 3.68 15.54 -- -- 51.68 16.94 -- -- 226-250 33.84 6.14 38.40 4.33 -- -- -- -- -- -- -- -- 251-275 34.34 6.65 35.64 4.73 -- -- -- -- -- -- -- -- 276-300 30.60 4.19 39.02 6.71 -- -- -- -- -- -- -- --

Lab1-Rechargeable Puff Set Data – ACM (mg)


76-100 41.78 5.79 47.08 3.39 80.62 7.02 102.15 11.24 76.92 7.67 97.36 13.80 101-125 40.86 5.43 45.22 3.68 78.10 5.72 97.45 10.68 72.84 5.69 92.18 13.20 126-150 40.36 4.69 42.74 3.36 74.56 7.19 92.10 10.04 70.34 6.06 87.16 9.94 151-175 37.40 5.62 39.62 4.26 71.22 6.74 43.45 11.95 66.64 5.28 27.62 13.60 176-200 36.30 4.73 39.24 3.00 66.68 5.90 -- -- 63.18 4.73 -- -- 201-225 36.24 4.29 36.36 4.25 7.78 9.62 -- -- 19.12 10.91 -- -- 226-250 35.22 4.07 36.36 3.51 -- -- -- -- -- -- -- -- 251-275 33.64 3.47 36.36 3.14 -- -- -- -- -- -- -- -- 276-300 32.50 2.65 34.46 3.56 -- -- -- -- -- -- -- --


Lab1-Rechargeable Puff Set Data – Propylene Glycol (mg)


76-100 18.65 2.60 23.06 1.69 37.90 3.46 48.49 3.95 35.81 3.28 46.72 7.33 101-125 18.46 2.44 22.13 1.52 30.90 10.10 47.62 5.78 34.82 3.05 44.38 6.55 126-150 17.86 2.47 20.66 1.41 36.03 3.65 43.85 3.07 33.51 3.20 42.09 5.36 151-175 17.15 2.24 19.63 2.16 34.31 3.72 22.75 7.01 32.35 2.75 13.88 6.10 176-200 16.60 2.02 18.52 1.76 31.59 2.67 -- -- 28.24 8.10 -- -- 201-225 16.61 1.78 17.34 2.36 4.32 4.13 -- -- 8.77 5.53 -- -- 226-250 15.72 1.81 17.26 1.76 -- -- -- -- -- -- -- -- 251-275 15.64 1.44 17.43 1.28 -- -- -- -- -- -- -- -- 276-300 14.64 1.24 16.35 1.44 -- -- -- -- -- -- -- --

Lab1-Rechargeable Puff Set Data – Glycerin (mg)


76-100 10.46 1.30 12.76 0.94 20.83 1.63 27.34 2.84 19.51 1.61 24.66 3.39 101-125 10.35 1.16 12.18 0.86 18.06 2.65 25.42 2.19 18.71 2.13 23.88 3.09 126-150 10.01 1.15 11.29 0.75 18.87 1.73 23.72 1.85 18.05 1.97 22.56 2.73 151-175 9.53 1.20 10.85 1.06 18.62 1.88 12.01 3.30 17.61 1.70 7.64 3.24 176-200 9.24 1.12 10.43 0.88 17.26 1.52 -- -- 14.97 4.12 -- -- 201-225 8.69 1.44 9.74 1.29 3.21 2.28 -- -- 5.42 3.05 -- -- 226-250 8.76 1.09 9.66 0.88 -- -- -- -- -- -- -- -- 251-275 8.56 1.00 9.85 0.72 -- -- -- -- -- -- -- -- 276-300 8.41 0.71 9.19 0.81 -- -- -- -- -- -- -- --


Lab1-Rechargeable Puff Set Data – Nicotine (mg)


76-100 0.49 0.07 0.61 0.04 0.99 0.08 1.27 0.10 0.92 0.07 1.19 0.18 101-125 0.49 0.06 0.58 0.04 0.83 0.19 1.22 0.13 0.89 0.07 1.14 0.16 126-150 0.47 0.06 0.55 0.04 0.93 0.09 1.13 0.08 0.86 0.08 1.08 0.13 151-175 0.46 0.05 0.52 0.05 0.90 0.10 0.59 0.17 0.83 0.06 0.36 0.16 176-200 0.44 0.05 0.49 0.04 0.83 0.07 -- -- 0.72 0.20 -- -- 201-225 0.43 0.05 0.47 0.06 0.31 -- -- -- 0.25 0.15 -- -- 226-250 0.42 0.05 0.46 0.04 -- -- -- -- -- -- -- -- 251-275 0.41 0.03 0.46 0.04 -- -- -- -- -- -- -- -- 276-300 0.39 0.03 0.43 0.04 -- -- -- -- -- -- -- --

Lab1-Rechargeable Puff Set Data – Water (mg)


76-100 5.26 0.62 8.45 1.11 9.83 1.18 11.40 0.76 8.67 2.88 10.93 2.65 101-125 4.84 0.64 5.73 0.81 13.71 4.08 11.56 0.57 7.58 1.44 9.00 1.98 126-150 5.19 1.73 4.93 0.95 9.80 1.05 9.83 0.47 6.59 0.96 9.69 1.66 151-175 4.86 0.88 12.41 9.25 7.43 1.31 5.06 1.91 5.60 1.06 1.77 1.76 176-200 6.03 2.31 4.60 2.43 8.35 1.26 -- -- 6.22 1.99 -- -- 201-225 4.91 1.00 6.91 4.61 -- -- -- -- 2.72 0.17 -- -- 226-250 3.66 0.37 8.64 10.74 -- -- -- -- -- -- -- -- 251-275 3.37 0.84 4.36 1.35 -- -- -- -- -- -- -- -- 276-300 2.38 0.49 2.55 1.08 -- -- -- -- -- -- -- --


Lab2-Disposable Puff Set Data – Puff Count


76-100 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 101-125 25.00 0.00 25.00 0.00 25.00 0.00 -- -- 25.00 0.00 -- -- 126-150 25.00 0.00 25.00 0.00 24.00 1.73 -- -- -- -- -- -- 151-175 25.00 0.00 25.00 0.00 -- -- -- -- -- -- -- -- 176-200 25.00 0.00 25.00 0.00 -- -- -- -- -- -- -- -- 201-225 25.00 0.00 25.00 0.00 -- -- -- -- -- -- -- -- 226-250 25.00 0.00 -- -- -- -- -- -- -- -- -- -- 251-275 -- -- -- -- -- -- -- -- -- -- -- -- 276-300 -- -- -- -- -- -- -- -- -- -- -- --

Lab 2-D Puff Set Data – Weight Loss (mg)


76-100 22.92 3.92 28.18 3.40 40.94 12.24 43.30 3.21 35.24 5.17 36.30 2.18 101-125 19.64 4.51 23.60 3.19 27.60 9.54 -- -- 23.54 6.29 -- -- 126-150 15.40 6.59 18.24 2.92 4.88 3.55 -- -- -- -- -- -- 151-175 11.22 6.26 12.72 2.62 -- -- -- -- -- -- -- -- 176-200 10.05 2.09 7.10 3.20 -- -- -- -- -- -- -- -- 201-225 -- -- -- -- -- -- -- -- -- -- -- -- 226-250 -- -- -- -- -- -- -- -- -- -- -- -- 251-275 -- -- -- -- -- -- -- -- -- -- -- -- 276-300 -- -- -- -- -- -- -- -- -- -- -- --


Lab2-Disposable Puff Set Data – ACM (mg)


76-100 23.74 3.46 28.64 3.63 41.56 11.92 43.24 2.87 36.40 5.30 36.30 2.65 101-125 21.70 4.43 24.74 3.38 28.16 9.70 -- -- 24.04 6.36 -- -- 126-150 16.32 6.49 19.24 2.99 6.00 3.87 -- -- -- -- -- -- 151-175 12.22 6.50 13.98 2.67 -- -- -- -- -- -- -- -- 176-200 8.30 4.67 7.32 3.08 -- -- -- -- -- -- -- -- 201-225 -- -- -- -- -- -- -- -- -- -- -- -- 226-250 -- -- -- -- -- -- -- -- -- -- -- -- 251-275 -- -- -- -- -- -- -- -- -- -- -- -- 276-300 -- -- -- -- -- -- -- -- -- -- -- --

Lab2-Disposable Puff Set Data – Propylene Glycol (mg)


76-100 13.10 2.34 15.92 2.16 23.27 7.28 25.12 1.71 20.25 3.42 20.78 1.33 101-125 11.53 2.49 13.57 2.02 15.80 6.04 -- -- 13.52 3.77 -- -- 126-150 8.96 3.45 10.41 1.60 3.32 2.27 -- -- -- -- -- -- 151-175 6.66 3.59 7.50 1.39 -- -- -- -- -- -- -- -- 176-200 3.89 2.33 3.69 1.58 -- -- -- -- -- -- -- -- 201-225 -- -- -- -- -- -- -- -- -- -- -- -- 226-250 -- -- -- -- -- -- -- -- -- -- -- -- 251-275 -- -- -- -- -- -- -- -- -- -- -- -- 276-300 -- -- -- -- -- -- -- -- -- -- -- --


Lab2-Disposable Puff Set Data – Glycerin (mg)


76-100 6.26 0.98 7.77 1.06 11.08 3.00 12.27 0.75 9.89 1.52 10.14 1.19 101-125 5.68 1.12 6.75 0.98 7.73 2.83 -- -- 6.35 1.59 -- -- 126-150 4.37 1.64 5.19 0.83 1.39 0.93 -- -- -- -- -- -- 151-175 3.15 1.72 3.75 0.78 -- -- -- -- -- -- -- -- 176-200 1.78 1.05 1.78 0.82 -- -- -- -- -- -- -- -- 201-225 -- -- -- -- -- -- -- -- -- -- -- -- 226-250 -- -- -- -- -- -- -- -- -- -- -- -- 251-275 -- -- -- -- -- -- -- -- -- -- -- -- 276-300 -- -- -- -- -- -- -- -- -- -- -- --

Lab2-Disposable Puff Set Data – Nicotine (mg)


76-100 0.41 0.06 0.52 0.07 0.74 0.23 0.79 0.05 0.64 0.11 0.66 0.05 101-125 0.37 0.08 0.44 0.06 0.50 0.19 -- -- 0.42 0.12 -- -- 126-150 0.29 0.11 0.34 0.05 0.10 0.07 -- -- -- -- -- -- 151-175 0.21 0.11 0.26 0.05 -- -- -- -- -- -- -- -- 176-200 0.12 0.07 0.13 0.05 -- -- -- -- -- -- -- -- 201-225 -- -- -- -- -- -- -- -- -- -- -- -- 226-250 -- -- -- -- -- -- -- -- -- -- -- -- 251-275 -- -- -- -- -- -- -- -- -- -- -- -- 276-300 -- -- -- -- -- -- -- -- -- -- -- --


Lab2-Disposable Puff Set Data – Water (mg)


76-100 3.13 0.46 2.16 0.44 4.66 1.26 3.34 0.17 4.87 1.24 3.20 0.22 101-125 2.20 0.28 2.29 0.26 3.58 1.14 -- -- 3.21 0.63 -- -- 126-150 1.79 0.84 1.44 0.40 0.94 0.50 -- -- -- -- -- -- 151-175 1.37 0.76 0.93 0.26 -- -- -- -- -- -- -- -- 176-200 0.76 0.41 0.48 0.17 -- -- -- -- -- -- -- -- 201-225 -- -- -- -- -- -- -- -- -- -- -- -- 226-250 -- -- -- -- -- -- -- -- -- -- -- -- 251-275 -- -- -- -- -- -- -- -- -- -- -- -- 276-300 -- -- -- -- -- -- -- -- -- -- -- --



76-100 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 101-125 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 126-150 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 151-175 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 176-200 25.00 0.00 25.00 0.00 25.00 0.00 -- -- 25.00 0.00 -- -- 201-225 25.00 0.00 25.00 0.00 25.00 0.00 -- -- 25.00 0.00 -- -- 226-250 25.00 0.00 25.00 0.00 -- -- -- -- -- -- -- -- 251-275 25.00 0.00 25.00 0.00 -- -- -- -- -- -- -- -- 276-300 25.00 0.00 25.00 0.00 -- -- -- -- -- -- -- --


Lab 2-R Puff Set Data – Weight Loss (mg)


76-100 30.60 7.01 28.26 6.65 63.04 11.79 86.02 5.28 67.52 11.94 92.36 8.83 101-125 30.76 5.94 25.48 6.82 60.00 11.16 82.88 5.70 64.08 12.39 86.44 7.97 126-150 27.94 5.85 23.94 6.55 57.08 11.11 76.82 7.87 59.56 12.10 76.52 4.39 151-175 26.92 5.17 22.62 6.22 55.80 9.19 35.46 4.27 56.72 12.00 17.74 8.32 176-200 26.28 5.98 23.60 6.33 48.00 6.80 -- -- 39.30 10.36 -- -- 201-225 25.56 4.35 21.48 6.01 13.90 13.44 -- -- 28.80 1.70 -- -- 226-250 23.64 5.23 20.22 6.04 -- -- -- -- -- -- -- -- 251-275 23.48 5.20 19.40 6.40 -- -- -- -- -- -- -- -- 276-300 22.80 3.90 14.68 9.14 -- -- -- -- -- -- -- --



76-100 33.22 7.03 28.76 6.45 65.70 11.69 87.84 4.54 69.88 12.40 93.40 8.79 101-125 32.82 6.32 27.26 6.92 62.28 11.15 84.10 5.85 65.62 12.15 87.48 8.08 126-150 30.76 6.04 26.04 6.97 58.96 10.69 79.26 7.39 61.50 11.94 78.70 4.98 151-175 29.66 5.08 24.92 6.01 58.38 9.43 38.60 4.56 58.72 11.72 20.44 8.47 176-200 28.32 6.00 24.32 6.38 49.64 6.70 -- -- 41.78 10.12 -- -- 201-225 27.20 4.49 23.42 6.03 16.28 13.75 -- -- 31.05 1.91 -- -- 226-250 25.24 5.36 20.76 6.26 -- -- -- -- -- -- -- -- 251-275 25.34 5.24 20.46 7.04 -- -- -- -- -- -- -- -- 276-300 23.68 4.27 15.86 9.19 -- -- -- -- -- -- -- --




76-100 18.60 4.42 16.31 3.96 37.41 6.98 51.41 2.93 39.85 7.57 55.15 5.42 101-125 18.57 3.59 15.05 3.95 35.87 7.02 49.62 3.53 37.66 7.73 51.56 6.07 126-150 16.98 3.41 14.28 3.65 34.24 6.57 46.65 4.23 35.48 7.68 45.43 2.92 151-175 16.25 3.36 13.60 3.56 32.16 5.28 22.66 2.63 33.29 7.06 11.44 4.93 176-200 15.75 3.34 13.21 3.77 27.88 4.00 -- -- 23.62 5.94 -- -- 201-225 15.13 3.18 12.80 3.56 9.07 7.77 -- -- 17.24 1.44 -- -- 226-250 14.16 3.37 11.78 3.63 -- -- -- -- -- -- -- -- 251-275 14.17 2.83 11.03 3.71 -- -- -- -- -- -- -- -- 276-300 13.36 2.53 8.33 4.89 -- -- -- -- -- -- -- --



76-100 8.81 1.88 8.10 1.89 18.27 3.31 25.35 1.21 19.07 3.24 26.80 2.28 101-125 8.73 1.74 7.48 1.88 17.23 2.94 23.48 1.93 18.03 3.29 24.65 2.20 126-150 8.20 1.57 7.05 1.80 16.37 3.10 21.70 2.08 16.95 3.34 21.46 1.14 151-175 7.69 1.41 6.75 1.73 15.38 2.68 10.27 1.32 15.72 2.90 5.18 2.13 176-200 7.41 1.56 6.57 1.82 13.42 1.95 -- -- 11.29 3.09 -- -- 201-225 7.07 1.46 6.30 1.71 4.27 3.67 -- -- 8.36 0.66 -- -- 226-250 6.62 1.48 5.88 1.77 -- -- -- -- -- -- -- -- 251-275 6.54 1.21 5.50 1.75 -- -- -- -- -- -- -- -- 276-300 6.21 1.13 4.17 2.41 -- -- -- -- -- -- -- --




76-100 0.59 0.13 0.53 0.12 1.22 0.23 1.65 0.09 1.26 0.24 1.76 0.16 101-125 0.59 0.12 0.49 0.12 1.15 0.22 1.57 0.11 1.19 0.24 1.63 0.17 126-150 0.55 0.11 0.46 0.11 1.11 0.22 1.48 0.13 1.13 0.24 1.44 0.08 151-175 0.52 0.11 0.44 0.11 1.03 0.17 0.71 0.08 1.05 0.22 0.37 0.15 176-200 0.50 0.11 0.43 0.12 0.90 0.13 -- -- 0.74 0.19 -- -- 201-225 0.48 0.10 0.42 0.11 0.28 0.25 -- -- 0.54 0.05 -- -- 226-250 0.37 0.22 0.39 0.11 -- -- -- -- -- -- -- -- 251-275 0.45 0.09 0.36 0.11 -- -- -- -- -- -- -- -- 276-300 0.43 0.08 0.28 0.15 -- -- -- -- -- -- -- --



76-100 4.17 0.59 2.62 0.69 7.43 0.88 6.98 0.50 8.59 4.51 8.16 0.55 101-125 3.63 0.73 2.78 0.57 6.79 0.95 6.88 0.65 6.87 1.19 8.10 1.01 126-150 3.60 1.05 2.37 0.71 9.22 6.44 6.80 0.55 8.91 4.44 7.50 0.62 151-175 3.56 0.75 2.16 0.60 6.03 0.92 3.81 0.40 6.18 0.91 2.16 0.89 176-200 2.94 0.53 2.34 0.72 5.64 0.75 -- -- 5.07 1.02 -- -- 201-225 3.13 0.59 2.48 0.68 2.65 1.69 -- -- 4.36 0.16 -- -- 226-250 2.74 0.65 2.16 0.65 -- -- -- -- -- -- -- -- 251-275 2.93 0.54 1.58 0.68 -- -- -- -- -- -- -- -- 276-300 2.53 0.50 1.52 1.02 -- -- -- -- -- -- -- --




76-100 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 101-125 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 126-150 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 151-175 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 176-200 25.00 0.00 25.00 0.00 25.00 0.00 15.80 1.79 25.00 0.00 9.78 4.36 201-225 25.00 0.00 25.00 0.00 25.00 0.00 -- -- 25.00 0.00 -- -- 226-250 25.00 0.00 25.00 0.00 25.00 0.00 -- -- 15.20 7.09 -- -- 251-275 25.00 0.00 25.00 0.00 -- -- -- -- -- -- -- -- 276-300 25.00 0.00 25.00 0.00 -- -- -- -- -- -- -- --



76-100 26.30 2.31 24.60 2.89 44.53 4.41 59.26 7.07 45.28 6.74 52.84 7.79 101-125 24.60 2.44 22.82 2.91 41.00 4.29 51.18 6.77 41.34 6.43 48.88 8.33 126-150 24.44 2.05 21.66 2.58 38.35 4.24 53.98 7.00 39.08 8.77 45.08 8.39 151-175 21.76 2.23 20.24 2.42 35.15 4.33 44.52 6.32 35.08 5.41 39.08 7.42 176-200 24.96 2.11 20.48 2.40 33.78 3.73 16.04 4.46 34.08 6.02 8.20 5.47 201-225 21.00 2.35 18.98 2.30 29.30 5.84 -- -- 28.56 5.24 -- -- 226-250 20.44 2.79 18.36 2.36 14.60 9.75 -- -- 8.84 5.06 -- -- 251-275 20.20 2.29 17.46 2.30 -- -- -- -- -- -- -- -- 276-300 18.98 2.52 16.40 2.43 -- -- -- -- -- -- -- --




76-100 25.50 2.31 24.00 3.10 41.33 3.85 56.14 6.91 40.62 7.11 47.30 6.35 101-125 22.20 2.16 23.10 2.91 39.53 4.32 51.66 6.10 39.24 7.14 44.66 7.63 126-150 19.40 3.45 20.82 2.91 34.90 4.43 48.34 6.31 39.14 7.82 42.20 7.41 151-175 21.28 2.79 19.34 1.95 35.23 3.30 40.92 6.19 34.06 4.97 40.04 7.48 176-200 20.94 1.97 18.10 2.64 31.58 2.81 14.66 4.44 31.42 5.61 7.64 5.12 201-225 20.34 2.36 18.20 2.19 27.58 5.21 -- -- 26.26 4.68 -- -- 226-250 18.44 2.95 16.14 2.40 17.27 5.69 -- -- 6.04 3.91 -- -- 251-275 19.68 3.49 17.04 2.46 -- -- -- -- -- -- -- -- 276-300 18.77 3.59 16.24 2.57 -- -- -- -- -- -- -- --



76-100 0.03 0.00 0.03 0.00 0.05 0.00 0.07 0.01 0.05 0.01 0.06 0.01 101-125 0.03 0.00 0.03 0.00 0.04 0.00 0.06 0.01 0.05 0.01 0.06 0.01 126-150 0.03 0.00 0.03 0.00 0.04 0.00 0.06 0.01 0.05 0.01 0.05 0.01 151-175 0.03 0.00 0.03 0.00 0.04 0.00 0.06 0.01 0.04 0.01 0.04 0.01 176-200 0.03 0.00 0.02 0.00 0.04 0.00 0.02 0.01 0.04 0.01 0.01 0.00 201-225 0.03 0.00 0.03 0.00 0.03 0.01 -- -- 0.04 0.01 -- -- 226-250 0.03 0.00 0.02 0.00 0.02 0.01 -- -- 0.02 0.01 -- -- 251-275 0.02 0.00 0.02 0.00 -- -- -- -- -- -- -- -- 276-300 0.02 0.00 0.02 0.00 -- -- -- -- -- -- -- --




76-100 18.26 1.54 17.53 1.99 30.23 2.70 40.52 4.52 31.50 4.76 34.42 4.40 101-125 17.24 1.24 16.21 2.14 29.28 3.35 37.68 4.53 28.91 4.12 33.03 4.99 126-150 16.41 1.89 15.42 1.89 27.32 2.48 35.49 4.34 27.42 5.69 30.34 4.69 151-175 16.47 1.78 14.47 1.34 26.11 2.55 31.41 4.32 25.72 4.15 27.47 4.73 176-200 17.14 1.38 14.24 1.60 23.85 2.44 11.52 2.94 24.23 4.34 5.51 3.55 201-225 14.21 1.58 13.48 1.50 21.37 3.74 -- -- 20.60 3.76 -- -- 226-250 13.76 1.53 12.66 1.60 10.37 7.26 -- -- 6.40 3.33 -- -- 251-275 13.20 1.56 11.79 1.65 -- -- -- -- -- -- -- -- 276-300 12.58 1.61 11.38 1.61 -- -- -- -- -- -- -- --



76-100 0.40 0.03 0.38 0.06 0.67 0.06 0.88 0.11 0.68 0.10 0.80 0.12 101-125 0.39 0.03 0.45 0.05 0.63 0.07 0.82 0.12 0.62 0.10 0.72 0.13 126-150 0.38 0.03 0.40 0.05 0.59 0.06 0.76 0.12 0.62 0.13 0.70 0.13 151-175 0.36 0.03 0.31 0.05 0.53 0.08 0.66 0.12 0.52 0.08 0.62 0.12 176-200 0.39 0.03 0.32 0.04 0.49 0.05 0.25 0.07 0.49 0.09 0.13 0.08 201-225 0.33 0.03 0.31 0.04 0.51 0.07 -- -- 0.44 0.09 -- -- 226-250 0.34 0.03 0.30 0.03 0.35 0.09 -- -- 0.08 0.07 -- -- 251-275 0.31 0.04 0.29 0.04 -- -- -- -- -- -- -- -- 276-300 0.28 0.03 0.28 0.04 -- -- -- -- -- -- -- --




76-100 4.80 0.63 4.98 0.70 8.40 1.38 10.80 1.79 8.89 1.13 8.56 1.31 101-125 4.78 0.37 4.64 0.46 7.06 0.87 10.38 1.49 7.53 0.97 9.68 1.36 126-150 4.55 0.74 4.26 0.36 6.34 0.64 9.05 1.04 7.19 1.46 8.97 1.59 151-175 4.19 0.84 4.31 0.54 7.08 0.92 8.13 1.09 7.50 0.86 7.31 1.36 176-200 5.28 0.86 4.19 0.41 6.66 0.52 2.70 0.83 6.11 1.16 1.58 1.19 201-225 4.50 0.46 3.42 0.54 6.21 1.10 -- -- 5.29 0.69 -- -- 226-250 4.00 0.83 3.74 0.58 2.95 1.21 -- -- 1.60 0.94 -- -- 251-275 3.85 0.55 3.36 0.89 -- -- -- -- -- -- -- -- 276-300 3.73 0.71 2.83 1.30 -- -- -- -- -- -- -- --



76-100 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 101-125 25.00 0.00 25.00 0.00 25.00 0.00 -- -- 25.00 0.00 -- -- 126-150 25.00 0.00 25.00 0.00 -- -- -- -- -- -- -- -- 151-175 25.00 0.00 25.00 0.00 -- -- -- -- -- -- -- -- 176-200 -- -- -- -- -- -- -- -- -- -- -- -- 201-225 -- -- -- -- -- -- -- -- -- -- -- -- 226-250 -- -- -- -- -- -- -- -- -- -- -- -- 251-275 -- -- -- -- -- -- -- -- -- -- -- -- 276-300 -- -- -- -- -- -- -- -- -- -- -- --




76-100 20.14 5.89 20.76 3.65 44.20 9.21 44.43 21.26 53.04 8.84 51.16 9.57 101-125 16.58 4.65 14.50 2.91 34.30 11.46 42.50 10.79 126-150 13.16 5.05 11.96 3.12 151-175 176-200 201-225 226-250 251-275 276-300



76-100 22.64 3.67 15.44 4.91 44.28 11.47 43.65 20.49 50.98 8.51 51.30 9.36 101-125 18.02 5.30 14.06 2.45 35.44 14.22 -- -- 40.92 10.48 -- -- 126-150 16.76 3.83 11.62 1.82 -- -- -- -- -- -- -- -- 151-175 -- -- -- -- -- -- -- -- -- -- -- -- 176-200 -- -- -- -- -- -- -- -- -- -- -- -- 201-225 -- -- -- -- -- -- -- -- -- -- -- -- 226-250 -- -- -- -- -- -- -- -- -- -- -- -- 251-275 -- -- -- -- -- -- -- -- -- -- -- -- 276-300 -- -- -- -- -- -- -- -- -- -- -- --




76-100 0.02 0.01 0.02 0.00 0.04 0.01 -- -- -- -- 0.04 0.01 101-125 0.02 0.00 0.02 0.01 0.04 0.02 -- -- -- -- -- -- 126-150 0.02 0.00 0.02 0.00 -- -- -- -- -- -- -- -- 151-175 -- -- -- -- -- -- -- -- -- -- -- -- 176-200 -- -- -- -- -- -- -- -- -- -- -- -- 201-225 -- -- -- -- -- -- -- -- -- -- -- -- 226-250 -- -- -- -- -- -- -- -- -- -- -- -- 251-275 -- -- -- -- -- -- -- -- -- -- -- -- 276-300 -- -- -- -- -- -- -- -- -- -- -- --



76-100 14.57 4.46 10.59 2.45 28.85 7.35 31.68 16.10 36.82 6.06 38.10 7.05 101-125 11.52 3.31 9.15 2.07 35.23 7.18 -- -- 31.02 7.93 -- -- 126-150 8.56 3.59 7.97 2.25 -- -- -- -- -- -- -- -- 151-175 -- -- -- -- -- -- -- -- -- -- -- -- 176-200 -- -- -- -- -- -- -- -- -- -- -- -- 201-225 -- -- -- -- -- -- -- -- -- -- -- -- 226-250 -- -- -- -- -- -- -- -- -- -- -- -- 251-275 -- -- -- -- -- -- -- -- -- -- -- -- 276-300 -- -- -- -- -- -- -- -- -- -- -- --




76-100 0.32 0.07 0.23 0.05 0.58 0.16 0.58 0.29 0.65 0.12 0.70 0.14 101-125 0.22 0.07 0.22 0.04 0.46 0.19 -- -- 0.54 0.15 -- -- 126-150 0.20 0.05 0.19 0.02 -- -- -- -- -- -- -- -- 151-175 -- -- -- -- -- -- -- -- -- -- -- -- 176-200 -- -- -- -- -- -- -- -- -- -- -- -- 201-225 -- -- -- -- -- -- -- -- -- -- -- -- 226-250 -- -- -- -- -- -- -- -- -- -- -- -- 251-275 -- -- -- -- -- -- -- -- -- -- -- -- 276-300 -- -- -- -- -- -- -- -- -- -- -- --



76-100 4.04 0.75 2.06 0.72 7.76 1.52 6.39 2.95 9.34 1.25 7.79 0.82 101-125 3.53 1.08 2.88 0.66 5.64 1.88 -- -- 6.36 1.61 -- -- 126-150 3.09 0.73 2.11 0.34 -- -- -- -- -- -- -- -- 151-175 -- -- -- -- -- -- -- -- -- -- -- -- 176-200 -- -- -- -- -- -- -- -- -- -- -- -- 201-225 -- -- -- -- -- -- -- -- -- -- -- -- 226-250 -- -- -- -- -- -- -- -- -- -- -- -- 251-275 -- -- -- -- -- -- -- -- -- -- -- -- 276-300 -- -- -- -- -- -- -- -- -- -- -- --




76-100 25.00 0.00 25.00 0.00 25.00 0.00 19.40 3.78 25.00 0.00 20.80 2.68 101-125 25.00 0.00 25.00 0.00 23.20 4.02 -- -- 22.20 2.77 -- -- 126-150 25.00 0.00 25.00 0.00 -- -- -- -- 10.00 -- -- -- 151-175 25.00 0.00 25.00 0.00 -- -- -- -- -- -- -- -- 176-200 24.60 0.89 18.80 5.72 -- -- -- -- -- -- -- -- 201-225 5.75 4.79 -- -- -- -- -- -- -- -- -- -- 226-250 -- -- -- -- -- -- -- -- -- -- -- -- 251-275 -- -- -- -- -- -- -- -- -- -- -- -- 276-300 -- -- -- -- -- -- -- -- -- -- -- --



76-100 24.40 4.63 27.48 5.61 50.80 2.61 46.58 10.10 51.20 3.17 50.50 5.90 101-125 23.66 4.41 25.98 5.44 37.22 7.26 -- -- 37.78 4.91 -- -- 126-150 21.74 3.98 24.22 5.48 -- -- -- -- 15.90 -- -- -- 151-175 20.50 3.39 21.56 4.20 -- -- -- -- -- -- -- -- 176-200 16.90 3.71 12.12 2.58 -- -- -- -- -- -- -- -- 201-225 -- -- -- -- -- -- -- -- -- -- -- -- 226-250 -- -- -- -- -- -- -- -- -- -- -- -- 251-275 -- -- -- -- -- -- -- -- -- -- -- -- 276-300 -- -- -- -- -- -- -- -- -- -- -- --




76-100 24.80 4.43 27.12 5.94 49.16 2.99 57.15 2.56 52.52 2.82 53.26 6.17 101-125 23.40 4.25 25.50 5.27 35.88 6.60 -- -- 36.96 4.67 -- -- 126-150 21.24 3.86 22.76 5.40 -- -- -- -- 16.50 -- -- -- 151-175 19.86 3.81 21.64 4.59 -- -- -- -- -- -- -- -- 176-200 15.92 4.08 10.28 3.42 -- -- -- -- -- -- -- -- 201-225 -- -- -- -- -- -- -- -- -- -- -- -- 226-250 -- -- -- -- -- -- -- -- -- -- -- -- 251-275 -- -- -- -- -- -- -- -- -- -- -- -- 276-300 -- -- -- -- -- -- -- -- -- -- -- --



76-100 10.49 2.02 11.49 2.56 21.38 1.31 19.38 4.48 21.90 1.53 21.13 2.93 101-125 9.75 2.01 10.65 2.44 15.26 3.01 -- -- 16.19 1.95 -- -- 126-150 13.34 7.22 9.93 2.50 -- -- -- -- 14.53 -- -- -- 151-175 8.33 1.76 9.15 2.30 -- -- -- -- -- -- -- -- 176-200 6.79 1.80 5.74 2.98 -- -- -- -- -- -- -- -- 201-225 -- -- -- -- -- -- -- -- -- -- -- -- 226-250 -- -- -- -- -- -- -- -- -- -- -- -- 251-275 -- -- -- -- -- -- -- -- -- -- -- -- 276-300 -- -- -- -- -- -- -- -- -- -- -- --




76-100 7.84 1.40 8.65 1.86 16.17 1.04 14.86 3.46 16.74 0.96 15.75 2.24 101-125 7.14 1.39 8.06 1.75 11.47 2.31 -- -- 12.48 1.47 -- -- 126-150 10.24 5.50 7.60 1.76 -- -- -- -- 10.60 -- -- -- 151-175 6.47 1.23 7.05 1.59 -- -- -- -- -- -- -- -- 176-200 5.24 1.29 5.25 3.84 -- -- -- -- -- -- -- -- 201-225 -- -- -- -- -- -- -- -- -- -- -- -- 226-250 -- -- -- -- -- -- -- -- -- -- -- -- 251-275 -- -- -- -- -- -- -- -- -- -- -- -- 276-300 -- -- -- -- -- -- -- -- -- -- -- --


35/2/60/B 55/2/30/B 55/3/30/Sq 55/4/30/Sq 70/3/30/Sq 70/4/30/Sq

Puffs Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev 0-25 0.29 0.04 0.32 0.08 0.63 0.03 0.91 0.07 0.65 0.04 0.88 0.05 26-50 0.26 0.04 0.30 0.07 0.58 0.03 0.81 0.06 0.59 0.04 1.32 0.48 51-75 0.25 0.04 0.27 0.06 0.53 0.04 0.73 0.04 0.54 0.04 0.70 0.03

76-100 0.22 0.04 0.24 0.06 0.48 0.03 0.45 0.09 0.50 0.03 0.49 0.06 101-125 0.20 0.04 0.23 0.05 0.36 0.07 -- -- 0.38 0.05 -- -- 126-150 0.27 0.15 0.18 0.05 -- -- -- -- 0.35 -- -- -- 151-175 0.16 0.04 0.18 0.05 -- -- -- -- -- -- -- -- 176-200 0.13 0.02 0.14 0.12 -- -- -- -- -- -- -- -- 201-225 -- -- -- -- -- -- -- -- -- -- -- -- 226-250 -- -- -- -- -- -- -- -- -- -- -- -- 251-275 -- -- -- -- -- -- -- -- -- -- -- -- 276-300 -- -- -- -- -- -- -- -- -- -- -- --




76-100 2.99 0.76 2.28 0.61 8.59 1.58 7.49 1.45 8.87 0.94 7.12 1.12 101-125 2.76 0.80 2.43 0.91 6.47 0.57 -- -- 7.82 1.28 -- -- 126-150 8.33 4.10 5.89 0.83 -- -- -- -- 7.60 -- -- -- 151-175 5.16 0.72 5.38 0.72 -- -- -- -- -- -- -- -- 176-200 5.55 0.75 8.02 2.30 -- -- -- -- -- -- -- -- 201-225 -- -- -- -- -- -- -- -- -- -- -- -- 226-250 -- -- -- -- -- -- -- -- -- -- -- -- 251-275 -- -- -- -- -- -- -- -- -- -- -- -- 276-300 -- -- -- -- -- -- -- -- -- -- -- --


35/2/60/B 55/2/30/B 55/3/30/Sq 55/4/30/Sq 70/3/30/Sq 70/4/30/Sq Puffs Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev 0-25 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 26-50 25.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 51-75 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00

76-100 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 101-125 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 126-150 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 151-175 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 176-200 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 25.00 0.00 22.00 6.71 201-225 25.00 0.00 25.00 0.00 25.00 0.00 19.20 3.56 24.00 2.24 24.75 0.50 226-250 25.00 0.00 25.00 0.00 21.80 7.16 6.00 -- 25.00 0.00 3.00 1.41 251-275 25.00 0.00 25.00 0.00 25.00 0.00 -- -- 24.75 0.50 -- -- 276-300 25.00 0.00 25.00 0.00 13.50 10.15 -- -- 12.67 5.13 -- --




76-100 31.72 3.63 32.22 7.27 80.26 6.33 105.06 6.02 80.06 3.43 102.76 12.39 101-125 31.82 4.38 31.66 6.86 77.28 4.81 104.24 8.05 78.46 3.59 104.42 8.76 126-150 29.24 4.67 30.18 6.76 76.76 5.94 98.06 7.37 76.40 3.43 99.26 13.20 151-175 29.60 4.52 29.38 6.71 74.20 4.25 98.44 4.07 73.76 3.50 94.52 14.38 176-200 29.34 4.58 29.02 6.58 75.34 4.32 90.88 5.09 71.90 4.21 80.82 32.37 201-225 27.52 3.94 27.96 6.26 69.38 5.33 49.78 26.62 64.92 13.30 78.75 5.21 226-250 28.98 4.44 26.78 5.80 58.30 27.37 13.20 -- 68.45 5.54 17.45 1.91 251-275 26.80 5.87 28.10 7.25 66.75 8.47 -- -- 60.28 10.30 -- -- 276-300 26.62 4.12 27.66 7.21 29.23 26.87 -- -- 24.17 15.82 -- --



76-100 36.94 2.69 36.24 7.44 84.64 6.78 107.96 5.79 89.10 3.68 112.78 12.41 101-125 34.84 4.19 34.80 7.15 81.34 4.56 107.56 8.39 82.98 3.49 110.32 8.03 126-150 32.54 5.10 33.98 6.95 80.56 6.25 103.30 7.12 77.72 3.32 103.00 12.42 151-175 33.24 4.37 33.16 6.83 80.46 4.27 105.12 3.82 77.18 4.76 102.22 14.27 176-200 31.88 4.09 31.62 6.63 77.40 4.19 93.42 4.86 79.40 4.25 87.74 34.58 201-225 31.52 3.83 31.20 6.41 75.44 6.99 54.32 27.59 67.42 15.15 84.85 6.37 226-250 30.84 4.60 30.30 6.94 62.64 27.95 15.40 -- 75.05 6.26 17.50 1.70 251-275 30.14 5.87 30.34 6.33 68.95 5.20 -- -- 61.25 11.98 -- -- 276-300 29.62 4.77 30.38 7.26 32.47 28.73 -- -- 27.33 16.90 -- --




76-100 13.26 1.60 13.87 3.14 33.53 2.78 43.08 4.31 34.47 1.86 42.13 4.92 101-125 13.00 1.82 13.20 3.04 32.69 2.29 41.16 3.50 33.12 1.57 42.57 3.80 126-150 12.46 2.04 12.84 2.89 32.55 2.58 31.42 1.60 32.36 1.55 41.34 5.72 151-175 12.41 1.73 12.46 2.82 31.65 1.76 37.77 2.28 31.78 1.79 40.13 6.59 176-200 11.95 1.93 10.69 4.92 41.08 1.75 24.88 11.38 31.13 1.88 34.39 14.24 201-225 11.73 1.76 12.07 2.66 30.08 2.89 5.69 -- 28.39 6.07 34.57 3.07 226-250 11.94 1.68 11.81 2.72 21.38 11.33 -- -- 29.71 2.16 4.35 0.76 251-275 11.19 2.42 11.28 1.77 27.67 2.34 -- -- 26.24 4.48 -- -- 276-300 11.70 2.72 11.52 2.86 12.48 11.77 -- -- 10.21 6.72 -- --


35/2/60/B 55/2/30/B 55/3/30/Sq 55/4/30/Sq 70/3/30/Sq 70/4/30/Sq

Puffs Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev 0-25 18.35 2.81 17.88 3.37 41.69 3.87 56.64 2.72 41.86 1.16 57.09 8.36 26-50 16.81 2.03 16.54 3.25 39.44 2.40 52.85 3.42 38.96 2.11 38.05 16.54 51-75 15.77 1.81 15.78 3.20 38.40 2.10 49.62 3.12 37.56 1.68 49.11 6.31

76-100 15.22 1.71 15.33 3.14 36.07 2.05 47.41 2.78 36.18 1.54 47.10 5.05 101-125 14.77 1.89 14.49 3.05 35.05 2.06 47.36 3.44 34.94 1.30 45.73 4.96 126-150 14.68 2.28 14.64 2.95 34.24 1.88 44.61 2.51 34.12 1.08 43.77 5.32 151-175 14.45 2.06 14.18 2.84 33.39 1.81 32.61 1.74 33.06 1.53 42.14 5.56 176-200 13.58 2.09 11.70 5.78 44.01 2.15 40.05 1.65 32.32 1.86 35.38 14.39 201-225 13.18 1.91 13.36 2.68 31.19 2.88 25.77 11.85 29.04 6.08 34.75 2.36 226-250 13.29 1.84 13.11 2.62 21.95 11.45 5.63 -- 30.19 2.34 4.14 0.75 251-275 12.39 2.60 12.43 1.84 28.26 2.68 -- -- 26.63 4.63 -- -- 276-300 12.85 2.66 12.66 2.77 12.97 12.14 -- -- 10.44 6.86 -- --




76-100 0.48 0.05 0.50 0.11 1.23 0.09 1.60 0.10 1.27 0.07 1.53 0.20 101-125 0.48 0.07 0.47 0.10 1.20 0.07 1.62 0.14 1.22 0.06 1.57 0.16 126-150 0.43 0.07 0.43 0.09 1.19 0.09 1.53 0.12 1.20 0.05 1.51 0.21 151-175 0.40 0.05 0.42 0.09 1.15 0.06 1.14 0.05 1.17 0.07 1.47 0.24 176-200 0.38 0.06 0.37 0.20 1.53 0.07 1.40 0.09 1.15 0.08 1.24 0.51 201-225 0.38 0.05 0.39 0.09 1.10 0.10 0.93 0.40 1.05 0.22 1.23 0.10 226-250 0.38 0.05 0.38 0.09 0.78 0.39 0.26 -- 1.10 0.08 0.17 0.03 251-275 0.36 0.07 0.37 0.06 1.01 0.08 -- -- 0.97 0.16 -- -- 276-300 0.37 0.08 0.37 0.09 0.46 0.43 -- -- 0.39 0.26 -- --



76-100 1.32 0.91 1.81 1.25 10.79 2.28 11.11 0.88 11.82 1.76 11.34 1.46 101-125 1.13 1.05 2.22 0.89 8.93 0.86 12.05 1.43 9.84 0.52 12.07 1.30 126-150 7.27 1.04 7.36 1.14 8.81 0.52 11.68 0.88 9.78 0.55 10.23 1.25 151-175 6.65 0.65 7.72 1.11 9.47 0.29 9.04 0.27 9.99 0.34 10.88 1.32 176-200 6.81 0.82 6.69 1.97 12.46 0.26 11.03 0.44 9.60 1.15 10.50 2.50 201-225 6.58 0.46 6.99 0.78 9.33 1.22 7.25 2.74 9.26 0.98 10.47 0.58 226-250 6.63 0.50 6.50 0.75 7.63 1.87 2.46 -- 9.90 0.21 2.28 0.21 251-275 6.36 0.99 6.68 0.82 8.37 1.08 -- -- 8.42 0.81 -- -- 276-300 6.82 1.10 6.65 0.96 4.64 2.44 -- -- 3.99 1.29 -- --


Lab1-3 piece Total Yields

Puff Count Weight Loss (mg) ACM (mg) PG (mg) Glycerin (mg) Nicotine (mg) Water (mg) Test Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev

35/2/60/B 300 0 172.9 164.2 272.2 59.8 74.28 17.39 99.43 19.32 3.77 0.90 38.1 9.8 55/2/30/B 279 23 341.6 36.2 320.6 31.5 102.9 13.1 132.1 12.8 4.40 0.56 88.2 10.1 55/3/30/Sq 168 8 170.6 158.1 271.8 39.9 76.06 13.90 100.1 14.7 3.45 0.53 47.5 4.7 55/4/30/Sq 150 NA 73.8 165.1 358.9 NA 71.36 NA 111.4 NA 3.61 NA 64.5 NA 70/3/30/Sq 150 4 379.9 47.1 359.2 48.1 134.6 36.5 118.5 23.49 5.06 0.79 62.1 6.1 70/4/30/Sq 122 9 286.4 181.8 332.7 90.3 124.7 26.2 84.1 47.41 4.40 1.21 60.0 19.3

Lab1-Rechargeable Total Yields


35/2/60/B 300 0 453.9 58.0 464.5 58.4 208.3 23.7 116.2 13.1 5.50 0.61 54.7 6.3 55/2/30/B 300 0 513.8 37.0 503.3 45.2 241.6 21.4 134.4 11.5 6.42 0.52 83.0 15.0 55/3/30/Sq 210 9 641.9 47.4 647.2 46.3 302.5 25.6 167.5 11.5 7.89 0.58 83.8 7.5 55/4/30/Sq 171 0 290.3 75.5 676.5 60.5 321.4 33.3 180.3 18.8 8.39 0.86 76.3 7.6 70/3/30/Sq 208 2 606.2 60.1 621.0 45.3 293.0 28.5 159.4 17.2 7.53 0.72 65.3 9.4 70/4/30/Sq 160 5 646.4 75.8 629.3 74.0 302.1 32.2 166.9 13.5 7.78 0.82 70.6 6.2


Lab2-Disposable Total Yields Puff Count Weight Loss (mg) ACM (mg) PG (mg) Glycerin (mg) Nicotine (mg) Water (mg)

Test Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev 35/2/60/B 240 22 159.2 37.6 170.2 37.7 93.36 21.02 45.72 9.60 3.07 0.62 19.8 4.0 55/2/30/B 225 0 189.2 24.8 198.7 25.3 109.9 15.0 55.20 7.28 3.64 0.48 16.8 2.4 55/3/30/Sq 149 2 246.1 59.6 253.0 59.5 142.6 35.2 70.36 16.10 4.60 1.13 28.2 5.5 55/4/30/Sq 100 0 287.8 13.7 288.7 14.0 168.3 8.2 84.67 3.97 5.39 0.26 23.8 2.3 70/3/30/Sq 125 0 219.6 26.5 226.1 24.6 126.7 15.1 62.92 6.97 4.05 0.48 25.9 4.0 70/4/30/Sq 100 0 276.1 13.9 278.5 13.2 161.0 8.4 81.76 4.42 5.16 0.26 25.3 1.0

Lab2-Rechargeable Total Yields Puff Count Weight Loss (mg) ACM (mg) PG (mg) Glycerin (mg) Nicotine (mg) Water (mg)

Test Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev 35/2/60/B 300 0 333.8 70.6 358.3 71.9 203.3 44.7 95.29 19.37 6.39 1.43 41.8 7.8 55/2/30/B 300 0 290.8 83.3 308.6 84.7 170.7 48.7 85.01 23.62 5.55 1.51 29.2 8.6 55/3/30/Sq 225 0 515.2 79.2 537.3 79.3 305.3 46.3 148.7 22.3 9.87 1.53 61.9 8.7 55/4/30/Sq 175 0 572.0 29.5 590.0 30.3 345.4 19.4 168.8 8.8 11.0 0.6 49.5 2.7 70/3/30/Sq 210 14 522.9 77.1 542.5 78.8 311.6 50.1 149.5 21.6 9.87 1.59 62.1 7.0 70/4/30/Sq 175 0 600.0 49.3 611.4 48.4 359.1 32.3 174.3 13.9 11.5 0.9 56.5 2.5


Lab3-Disposable Total Yields Puff Count Weight Loss (mg) ACM (mg) PG (mg) Glycerin (mg) Nicotine (mg) Water (mg)

Test Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev 35/2/60/B 300 0 273.3 28.7 0.35 0.05 201.6 18.9 4.58 0.40 57.5 6.9 55/2/30/B 300 0 258.2 28.6 0.34 0.03 189.2 20.0 4.47 0.54 51.5 6.8 55/3/30/Sq 253 21 377.0 35.0 0.44 0.03 281.5 26.0 6.09 0.56 74.0 6.9 55/4/30/Sq 191 2 415.6 52.4 0.52 0.07 309.4 36.6 6.67 0.97 83.7 10.0 70/3/30/Sq 240 7 370.4 50.1 0.47 0.08 280.8 35.1 5.98 0.83 75.0 7.7 70/4/30/Sq 185 4 369.5 43.5 0.42 0.07 262.9 26.1 5.96 0.80 73.8 9.0


Test Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev 35/2/60/B 175 0 148.1 7.2 0.11 0.04 89.18 23.18 1.92 0.10 24.3 1.3 55/2/30/B 175 0 109.8 7.0 0.10 0.04 69.03 14.96 1.65 0.08 19.8 2.2 55/3/30/Sq 125 1 233.8 45.7 0.24 0.06 172.2 21.3 3.20 0.63 37.9 5.9 55/4/30/Sq 94 13 267.1 30.1 0.19 0.09 191.0 19.4 3.67 0.45 39.7 4.4 70/3/30/Sq 125 0 267.6 38.7 0.13 0.10 204.5 29.6 3.61 0.56 42.7 5.1 70/4/30/Sq 100 0 270.3 21.7 0.22 0.04 198.0 12.9 3.67 0.29 42.5 5.3


Lab4-Disposable Total Yields


35/2/60/B 204 5 198.3 31.6 196.9 31.8 86.91 19.23 65.92 13.83 1.75 0.41 40.2 7.7 55/2/30/B 194 6 210.2 40.7 205.0 40.5 87.95 19.98 67.99 15.58 1.87 0.48 32.9 3.4 55/3/30/Sq 123 4 268.2 8.6 257.7 9.2 113.2 3.9 86.80 3.69 2.57 0.10 44.2 3.4 55/4/30/Sq 94 4 305.7 21.5 302.8 17.4 128.6 9.7 101.3 7.4 2.90 0.22 49.7 4.2 70/3/30/Sq 124 6 273.5 16.0 265.2 16.9 119.5 9.6 91.26 6.65 2.73 0.21 49.0 3.7 70/4/30/Sq 96 3 296.0 13.0 283.5 10.7 133.1 7.4 111.0 12.7 3.40 0.47 42.6 4.2


Test Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev Average Stdev 35/2/60/B 300 0 364.0 49.1 406.0 48.3 152.8 20.9 175.3 22.7 5.19 0.64 55.4 5.0 55/2/30/B 300 0 369.4 80.4 411.6 80.1 154.3 34.0 172.1 34.3 5.32 1.12 58.6 8.1 55/3/30/Sq 278 26 839.9 109.5 890.6 118.4 362.6 43.8 388.4 44.9 13.4 1.6 111 11 55/4/30/Sq 220 6 887.8 71.0 923.7 70.2 310.3 31.2 398.0 31.5 13.5 1.2 102 8 70/3/30/Sq 271 30 823.0 102.8 870.4 111.0 352.7 45.5 369.7 46.1 13.1 1.7 110 13 70/4/30/Sq 218 19 896.0 157.0 941.6 162.2 364.7 66.7 387.8 75.0 13.1 2.7 101 16


APPENDIX D: Total Yield Graphs

Figure 1: Lab1-3 piece Total Yields

Figure 2: Lab1-Rechargeable Total Yields

Regime Code

Test 3 55/3/30/Sq

Test 4 55/4/30/Sq

Test 5 70/3/30/Sq

Test 6 70/4/30/Sq

0.0

50.0

100.0

150.0

200.0

250.0

300.0

350.0

400.0

450.0

Test 3 Test 4 Test 5 Test 6

Tota

l AC

M (

mg)

0.0

100.0

200.0

300.0

400.0

500.0

600.0

700.0

800.0


Tota

l AC

M (

mg)


Figure 3: Lab2-Disposable Total Yields


Regime Code

Test 3 55/3/30/Sq

Test 4 55/4/30/Sq

Test 5 70/3/30/Sq

Test 6 70/4/30/Sq

0.0

50.0

100.0

150.0

200.0

250.0

300.0

350.0


Tota

l AC

M (

mg)

0.0

100.0

200.0

300.0

400.0

500.0

600.0

700.0


Tota

l AC

M (

mg)




Regime Code

Test 3 55/3/30/Sq

Test 4 55/4/30/Sq

Test 5 70/3/30/Sq

Test 6 70/4/30/Sq

0.0

50.0

100.0

150.0

200.0

250.0

300.0

350.0

400.0

450.0

500.0


Tota

l AC

M (

mg)

0.0

50.0

100.0

150.0

200.0

250.0

300.0

350.0


Tota

l AC

M (

mg)




Regime Code

Test 3 55/3/30/Sq

Test 4 55/4/30/Sq

Test 5 70/3/30/Sq

Test 6 70/4/30/Sq

0.0

50.0

100.0

150.0

200.0

250.0

300.0

350.0


Tota

l AC

M (

mg)

0.0

200.0

400.0

600.0

800.0

1000.0

1200.0


Tota

l AC

M (

mg)


APPENDIX E: Puff Set Graphs

Figure 1: Lab1-3 piece Total Yields


Regime Code

Test 3 55/3/30/Sq

Test 4 55/4/30/Sq

Test 5 70/3/30/Sq

Test 6 70/4/30/Sq

0.00

10.00

20.00

30.00

40.00

50.00

60.00

70.00

80.00

90.00

100.00

AC

M (

mg/

pad

)

Puff Number

Test 3

Test 4

Test 5

Test 6

0.00

20.00

40.00

60.00

80.00

100.00

120.00

140.00

AC

M (

mg/

pad

)

Puff Number

Test 3

Test 4

Test 5

Test 6




Regime Code

Test 3 55/3/30/Sq

Test 4 55/4/30/Sq

Test 5 70/3/30/Sq

Test 6 70/4/30/Sq

0.00

20.00

40.00

60.00

80.00

100.00

120.00

AC

M (

mg/

pad

)

Puff Number

Test 3

Test 4

Test 5

Test 6

0.00

20.00

40.00

60.00

80.00

100.00

120.00

140.00

AC

M (

mg/

pad

)

Puff Number

Test 3

Test 4

Test 5

Test 6




Regime Code

Test 3 55/3/30/Sq

Test 4 55/4/30/Sq

Test 5 70/3/30/Sq

Test 6 70/4/30/Sq

0.00

10.00

20.00

30.00

40.00

50.00

60.00

70.00

80.00

90.00

AC

M (

mg/

pad

)

Puff Number

Test 3

Test 4

Test 5

Test 6

0.00

10.00

20.00

30.00

40.00

50.00

60.00

70.00

80.00

90.00

100.00

AC

M (

mg/

pad

)

Puff Number

Test 3

Test 4

Test 5

Test 6



Figure 8: Lab5-R Total Yields

Regime Code

Test 3 55/3/30/Sq

Test 4 55/4/30/Sq

Test 5 70/3/30/Sq

Test 6 70/4/30/Sq

0.00

10.00

20.00

30.00

40.00

50.00

60.00

70.00

80.00

90.00

100.00

AC

M (

mg/

pad

)

Puff Number

Test 3

Test 4

Test 5

Test 6

0.00

20.00

40.00

60.00

80.00

100.00

120.00

140.00

AC

M (

mg/

pad

)

Puff Number

Test 3

Test 4

Test 5

Test 6


APPENDIX F: ACM Variability - Percent Relative Standard Deviation for Puff Sets Rechargeable Products’ Results

n=5


Disposable Products’ Results

n=5

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