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Tobacco and Tobacco Products Analytes Sub-Group

Technical Report

Collaborative Study 2017 on TSNA, pH, and Moisture

(Oven Volatiles)

July 2017

Study Project Leaders:

David Ericson, Ph.D., Swedish Match, Sweden

Johan Lindholm, Ph.D., Swedish Match, Sweden

Anthony Brown, Altria Client Services LLC, U.S.A.

Author:

Anthony Brown, Altria Client Services LLC, U.S.A.

Co-Author and Statistical Analysis:

Michael Morton, Ph.D., Altria Client Services LLC, U.S.A.

Table of Contents

1. SUMMARY ...................................................................................................................... 3

2. INTRODUCTION ............................................................................................................ 3

2.1 Objective .................................................................................................................. 4

3. ORGANISATION ............................................................................................................ 4

3.1 Participants .............................................................................................................. 4

3.2 Protocol .................................................................................................................... 5

4. DATA – RAW .................................................................................................................. 6

5. DATA – STATISTICAL ANALYSIS ............................................................................. 6

5.1 Exclusion of Outliers ............................................................................................... 7

5.2 Calculation of Repeatability (r) and Reproducibility (R) ........................................ 8

6. DATA INTERPRETATIONS .......................................................................................... 9

7. RECOMMENDATIONS ................................................................................................ 10

8. APPENDICES ................................................................................................................ 10

TTPA-126-1-CTR 2017 Collaborative Study on TSNA, pH, and OV – July 2017 3/36

1. Summary

At the October 2016 CORESTA Smokeless Tobacco Sub-Group (STS) meeting (now named

Tobacco and Tobacco Products Analytes Sub-Group, TTPA) held in Berlin, the Sub-Group

initiated an interlaboratory collaborative study for the determination of TSNAs, pH, and

moisture (oven volatiles or OV) in ground tobacco, cigarette filler, and cigar filler. The intent

of this study was to update the scopes of the applicable CORESTA Recommended Methods

(CRMs) to include these additional matrices as the CRMs currently only include smokeless

tobacco products. CRM No. 72 (Determination of Tobacco Specific Nitrosamines in

Smokeless Tobacco Products by Liquid Chromatography - Tandem Mass Spectrometry) was

submitted to ISO/TC 126 for development into an ISO standard in June 2016. This work item

was approved as a Committee Draft on September 9, 2016 (ISO/CD 21766). The results of

this study will be used to update the scope of ISO/CD 21766 to include these additional

matrices. Tabulated data are presented along with repeatability (r) and reproducibility (R).

The results of the study demonstrate that the CRMs for TSNAs, pH, and moisture are suitable

for the analysis of ground tobacco, cigarette filler and cigar filler. The TTPA recommends

that the three CRMs and ISO draft be updated to include the additional tobacco matrices.

2. Introduction

In 2009, STS coordinated a collaborative study involving 23 laboratories to assess the

repeatability and reproducibility of a selection of methods used to determine TSNAs, pH, and

moisture in nine types of smokeless tobacco products1. The STS recommended that the

methods specified in the collaborative study for pH and TSNAs be the basis for two new

CRMs and CRM No. 69 (Determination of pH in Smokeless Tobacco Products) and CRM

No. 72 (Determination of Tobacco Specific Nitrosamines in Smokeless Tobacco Products by

LC-MS/MS) were published.

In the 2009 study report, the STS also recommended that a follow-up collaborative study be

conducted for moisture where standard conditions are specified. In 2010, the STS conducted

the follow-up study2. This study included the four CORESTA Reference Products (CRPs)

and five commercial smokeless tobacco products. Thirteen laboratories provided data using a

modified version of AOAC Official Method 966.02, Loss on Drying (Moisture) in Tobacco,

Gravimetric Method. The results of this collaborative study were the basis for CRM No. 76

(Determination of Moisture Content (Oven Volatiles) of Smokeless Tobacco Products). The

CRMs for TSNAs, pH, and OV have been used in robust annual collaborative studies and the

results of which are published at CORESTA.org.

In recent years, the prioritization of CRM development has been driven by tobacco product

regulation. Though the collaborative studies supporting the CRMs were focused on

smokeless tobacco products, it was anticipated that the methods would also be appropriate for

other tobacco products. At the STS meeting held in Berlin, Germany (October 2016), it was

decided to conduct a collaborative study to support the expansion of the scope of the CRMs

for TSNAs, pH, and moisture beyond smokeless tobacco to include ground tobacco, cigarette

filler and cigar filler.

1 STS Technical Report: 2009 Collaborative Study (Smokeless Tobacco r&R Study), July 2010 - updated Jan 2016.

2 STS Technical Report: Analysis of Moisture Content (Oven Volatiles) of Smokeless Tobacco Products, March

2014.


2.1 Objective

This study was conducted to support scope expansion of the TSNAs, pH, and moisture CRMs

beyond just smokeless tobacco to include ground tobacco, cigarette filler and cigar filler and

to provide an assessment of inter-laboratory variability. The participating laboratories were to

provide analytical results for the four TSNAs (N-nitrosonornicotine (NNN), N-

nitrosoanatabine (NAT), N-nitrosoanabasine (NAB) 4-(N-nitrosomethylamino)-1-(3-pyridyl)-

1-butanone (NNK), pH, and moisture (oven volatiles). This work was conducted using the

applicable CRMs referenced in Section 3. Data were collected from the participating

laboratories and statistically evaluated in basic conformance with the recommendations of

ISO 5725-2:1994 and ISO/TR 22971:2005.

3. Organisation

3.1 Participants

A list of the participating laboratories is provided in Table 1. Not all laboratories provided

data for all analyses nor did all laboratories analyze all samples. The laboratories are listed in

alphabetical order. Letter codes were assigned to each laboratory and do not correspond to

the order shown in the table below.

Table 1: List of Participating Laboratories in the 2017 WG4 Study

2017 WG4 Participants

Altria Client Services LLC, United States

American Snuff Company, LLC, United States

British American Tobacco, Germany

British American Tobacco Souza Cruz, Brazil

British American Tobacco, Sweden

China National Quality Supervision and Test Center, China

Enthalpy Analytical, Inc., United States

Essentra Scientific Services, United Kingdom

Global Laboratory Services, United States

Imperial Tobacco, Reemtsma, Germany

ITC Limited, India

ITG Brands, United States

Japan Tobacco Inc., Leaf Tobacco Research Center, Japan

KT&G Research Institute, South Korea

Labstat International ULC, Canada

Lauterbach & Associates, LLC, United States

C.I.T. Montepaz S.A., Uruguay

Philip Morris International, Switzerland

R.J. Reynolds Tobacco Company, United States

Shanghai Tobacco Group Co. Ltd., China

Swedish Match Northern Europe, Sweden

Swedish Match, Owensboro, United States

Swisher International, United States

University of Kentucky, United States


3.2 Protocol

Specific details from the protocol are described below:

3.2.1 Sample Shipment

Laboratories were responsible for procuring 1R6F, 1R5F, RTDAC, and RT2 from University

of Kentucky, NIST SRM 3222 from the United States National Institute of Standards and

Technology, and Cigar filler #1 and CigarM16 from Altria Client Services LLC. Laboratories

were requested to store the samples at approximately −20 °C upon receipt. Laboratories were

requested to conduct the study in December through March and report data by March 10,

2017. The samples are identified in Table 2.

Table 2: Sample Identification

Product Type

1R6F Ground Filler - American blended cigarette filler, ground

1R5F Ground Filler - American blended cigarette filler (high Burley), ground

RTDAC Ground Tobacco - Dark air-cured tobacco, ground

RT2 Ground Tobacco – Flue-cured tobacco, ground

NIST SRM 3222 - Cigarette tobacco filler, cut

Cigar Filler #1 - Flavored cigar filler, ground

CigarM16 - Traditional dark-air-cured cigar filler, ground

3.2.2 Within Laboratory Sample Preparation

The laboratories were directed to remove samples from the −20 °C freezer and place the

unopened samples in a refrigerator for a minimum of 24 hours to ensure water was fully

equilibrated. Samples could then be removed from the refrigerator for a minimum of 1 hour

prior to opening for analysis. Once samples were opened, the samples could be stored in a

tightly sealed container and stored at approximately 4 ºC for up to one week. Special

handling requirements, which differ from those specified in the CRMs, are described below:

- The 1R5F, RTDAC, Cigar Filler #1, and CigarM16 had high concentrations of

TSNAs. Participants were instructed to weigh out 0.4g for each TSNA replicate

instead of 1.0g, as is specified in the CRM for analysis.

- The NIST SRM 3222 sample was cut cigarette filler. Participants were instructed to

grind the contents of one bottle that contained 10g to ensure homogeneous aliquots

were removed for testing.

- The 1R6F, 1R5F, RTDAC, RT2, Cigar Filler #1, CigarM16, did not require sample

grinding and were to be analyzed as received.

3.2.3 Sample Analysis and Data Reporting

The participating laboratories were instructed to conduct triplicate replicate analyses

(individual tobacco weighing) for the following: TSNAs, pH, and moisture (oven volatiles)

using the current versions of the CRMs.

- TSNAs: CRM N° 72, Determination of Tobacco Specific Nitrosamines in Smokeless

Tobacco Products by Liquid Chromatography - Tandem Mass Spectrometry, February

2016.


- pH: CRM N° 69, Determination of pH in Smokeless Tobacco Products, June 2010

- Moisture (oven volatiles): CRM N° 76, Determination of Moisture Content (Oven

Volatiles) of Smokeless Tobacco Products, April 2014.

Participating laboratories were requested to document any deviations from the protocol and

the CRMs and submit the deviations with their results. As stated in the protocol, data

submitted with significant deviations from the applicable CRM would be excluded from the

study. Deviations reported by the laboratories are identified below. Since the reported

deviations were minor, no data sets were excluded from the study.

- Lab M: Minor deviations were reported for TSNAs where a different column than

that specified in the CRM was used. Specifically, a Gemini C18 3µm, (150mm x

3mm) was used instead of a C18 2.5µm, (50mm x 2.1mm).

- Lab N: Minor deviations were reported for TSNAs where two internal standards (d4-

NNN and d4-NNK) were used instead of four internal standards as is specified in the

CRM. Specifically, NNN-d4 was used as the internal standard for NNN and NNK-d4

was used as the internal standard for NNK, NAT, and NAB.

- Lab O: Minor deviations were reported for moisture where a fully automated

Brabender Moisture Tester was used instead conventional forced air oven. The

laboratory adhered to the recommended temperature of 100 °C and a drying time of 3

hours.

- Lab S: A deviation was reported where the laboratory removed the filler from 1R6F

and 1R5F cigarettes instead of acquiring ground cigarette fillers as was stated in the

study protocol.

- Lab Y: Minor deviations were reported for TSNAs where two internal standards (d4-

NNN and d4-NNK) were used instead of four internal standards as is specified in the

CRM. Specifically, NNN-d4 was used as the internal standard for NNN and NNK-d4

was used as the internal standard for NNK, NAT, and NAB.

All test results were to be reported on an as-is basis without correction for moisture content.

The results were not to be rounded and ideally reported to at least one more digit than

typically required. The study results and the comments were to be sent by e-mail to the study

coordinators.

4. Data – Raw

The full data set for the study is provided in Appendix A. The results are presented on an as-

is basis, without correction for moisture. Each analysis includes three replicates. Not all

laboratories provided data for all analyses or all samples. Data sets were removed from the

repeatability (r) and reproducibility (R) (r & R) portion of the study if the data were identified

as outlying data. Those data are included in Appendix A, but were eliminated prior to the r &

R analysis. Raw data plots that include all replicates, without removal of outliers, are given in

Appendix B.

5. Data – Statistical Analysis

The statistical analysis was conducted in basic conformance with ISO 5725-2:1994 and

ISO/TR 22971:2005. A summary of the results from outlier detection and the calculated

results for repeatability (r) and reproducibility (R) are given below in sections 5.1 and 5.2,

respectively. Raw data plots that include all replicates, without removal of outliers, are shown

in Appendix B.


5.1 Exclusion of Outliers

Procedures outlined in ISO 5725-2:1994 and ISO/TR 22971:2005 were generally used for the

exclusion of outliers. An adaptation of Levene’s Test was used for eliminating laboratories

with overly large repeatability standard deviations and Grubbs’ Test was used to eliminate

laboratories with outlying mean values.

ISO 5725(2) also recommends the use of Mandel’s h and k plots. Mandel’s h statistic is the

same as the statistic used in Grubbs’ Test. Similarly Mandel’s k statistic, associated with within

lab standard deviation, is statistically equivalent to the c-value calculated in Cochran’s Test

( cnk labs ). However, the critical values associated with Mandel’s h and k statistics do not

make allowance for multiple testing and can therefore, give a false impression of statistical

significance. Thus, Mandel’s h and k statistics do not add fundamentally new information and

may lead to incorrect conclusions. For those reasons, we do not include Mandel’s h and k plots.

The intent of ISO 5725-2:1994 is to eliminate outliers that exceed a 1% critical value. This

was accomplished by an adaptation of Levene’s Test. Levene’s Test is preferable to

Cochran’s Test, which is recommended in ISO 5725-2:1994, because of Cochran’s Test’s

extreme sensitivity to deviations from normality. Grubbs’ Test and an adaptation of Levene’s

Test were applied at the standard nominal 1% significance level to determine outliers and the

results are shown in Table 3. Levene’s Test is mentioned in ISO/TR 22971:2005 as an

alternative to Cochran’s Test. However, Levene’s Test does not directly apply without

adaptation. For more details, see the footnote below3.

Table 3: Outliers

Product Analyte Levene’s Outlier Lab Grubbs’ Outlier Lab

1R6F Moisture Q –

1R6F NAB – D

1R5F NAB – D

1R5F Moisture – L

1R5F pH – S

RTDAC NAB – D

RT2 NNN A –

NIST-SRM-3222 Moisture – H

Cigar filler #1 NAB – B

Cigar M16 NAB – D

The (–) symbol indicates an outlier was not detected.

3 Levene’s Test is commonly used to determine if each of several subpopulations have the same variance. Since

it was designed to test for overall differences, not to determine if the largest variance is significantly greater than

the others, some adaptation is necessary to use the approach to eliminate laboratories whose within lab variation

is too large. Levene’s Test was adapted to this purpose by Morton, who presented the approach utilized in this

report at the 2014 CORESTA Congress (Quebec, Canada, presentation ST28, October 14, 2014). Specifically,

the approach taken here is a two-step process with a lab being eliminated as an outlier if both steps are

statistically significant. First, Levene’s Test was run at a nominal -level of 0.02. Second a comparison of the

largest variance to the remaining variances is carried out at a one-sided nominal level of =0.01/number of labs.

Dividing by the number of labs is to account for multiple testing, since it is not known a priori which lab will

have the largest variance. Simulation studies were carried out by Morton and presented at the 2014 CORESTA

Congress and these results demonstrated that this process has an overall -level near 0.01 and is robust to

deviations from normality.


5.2 Calculation of Repeatability (r) and Reproducibility (R)

After removal of outlying data based on numerical data consistency methods (Grubbs’ Test

and Levene’s Test), the final repeatability and reproducibility (r & R) results were calculated.

The r & R results are shown in Table 4. The r & R results reflect both laboratory variability

and product consistency.

Table 4: Repeatability (r) and Reproducibility (R) Limits

Parameter Product N° of

Labs* Mean

Repeatability Reproducibility

r % r R % R

NNN (µg/g) 1R6F 18 2.29 0.24 10.3% 0.76 32.9%

NNN (µg/g) 1R5F 17 3.22 0.29 9.1% 1.14 35.4%

NNN (µg/g) RTDAC 17 3.95 0.37 9.3% 1.72 43.5%

NNN (µg/g) RT2 16 0.12 0.02 14.6% 0.05 45.8%

NNN (µg/g) NIST-SRM-3222 14 1.54 0.12 7.7% 0.52 33.9%

NNN (µg/g) Cigar filler #1 16 5.51 0.34 6.1% 1.76 32.0%

NNN (µg/g) CigarM16 15 3.53 0.28 7.8% 1.36 38.5%

NNK (µg/g) 1R6F 18 0.68 0.08 11.2% 0.18 27.0%

NNK (µg/g) 1R5F 17 0.78 0.08 9.7% 0.18 22.9%

NNK (µg/g) RTDAC 17 1.91 0.36 18.9% 0.62 32.7%

NNK (µg/g) RT2 17 0.11 0.02 17.1% 0.05 49.4%

NNK (µg/g) NIST-SRM-3222 14 0.032 0.010 31.3% 0.021 65.7%

NNK (µg/g) Cigar filler #1 15 1.78 0.15 8.4% 0.33 18.4%

NNK (µg/g) CigarM16 15 0.90 0.09 9.7% 0.22 24.4%

NAT (µg/g) 1R6F 18 2.09 0.22 10.4% 0.60 28.7%

NAT (µg/g) 1R5F 17 2.03 0.18 8.8% 0.50 24.5%

NAT (µg/g) RTDAC 17 4.35 0.42 9.6% 1.05 24.0%

NAT (µg/g) RT2 17 0.20 0.05 22.9% 0.08 41.2%

NAT (µg/g) NIST-SRM-3222 14 0.048 0.009 19.2% 0.030 62.5%

NAT (µg/g) Cigar filler #1 16 2.81 0.23 8.3% 0.61 21.8%

NAT (µg/g) CigarM16 15 1.74 0.25 14.6% 0.48 27.7%

NAB (µg/g) 1R6F 17 0.101 0.016 16.0% 0.039 38.1%

NAB (µg/g) 1R5F 16 0.111 0.022 19.8% 0.032 29.2%

NAB (µg/g) RTDAC 16 0.231 0.026 11.3% 0.045 19.5%

NAB (µg/g) RT2 16 0.014 0.004 26.6% 0.011 78.1%

NAB (µg/g) NIST-SRM-3222 13 0.007 0.004 49.9% 0.006 74.1%

NAB (µg/g) Cigar filler #1 15 0.188 0.021 10.9% 0.053 28.0%

NAB (µg/g) CigarM16 14 0.134 0.024 17.5% 0.042 31.5%


Parameter Product N° of

Labs* Mean

Repeatability Reproducibility

r % r R % R

Moisture % 1R6F 18 11.85 0.20 1.7% 0.92 7.7%

Moisture % 1R5F 17 12.68 0.20 1.6% 0.41 3.2%

Moisture % RTDAC 18 12.53 0.23 1.8% 0.76 6.0%

Moisture % RT2 18 12.65 0.24 1.9% 0.88 6.9%

Moisture % NIST-SRM-3222 15 11.52 0.34 2.9% 1.15 10.0%

Moisture % Cigar filler #1 17 18.54 0.42 2.3% 1.30 7.0%

Moisture % CigarM16 17 14.57 0.41 2.8% 0.77 5.3%

pH 1R6F 21 5.32 0.05 NA 0.24 NA

pH 1R5F 19 4.86 0.04 NA 0.18 NA

pH RTDAC 19 5.90 0.07 NA 0.23 NA

pH RT2 19 5.01 0.04 NA 0.22 NA

pH NIST-SRM-3222 16 8.71 0.08 NA 0.32 NA

pH Cigar filler #1 18 5.12 0.03 NA 0.18 NA

pH CigarM16 18 6.25 0.05 NA 0.27 NA

* This is the number of laboratory data sets reported as values and after removal of outliers.

NA = Since pH is not a proportional scale, it is not appropriate to calculate % r or % R.

6. Data Interpretations

Overall, the percent repeatability (%r) and percent reproducibility (%R) results from this

study compare well to the results presented in the CRMs. Notable differences include the

following:

- Overall, we noted greater variability for the TSNA results for RT2 and NIST SRM

3222 than seen for other sample types. The cause for the higher variability is likely

due to extremely low analyte concentrations that are at or below the limit of

quantitation for many laboratories.

- We also noted %R for moisture for NIST SRM 3222 was slightly greater than other

study samples. A plausible cause for this higher variability was that the protocol

stated this sample must be ground prior to analysis while all other samples were pre-

ground. Laboratories used their own grinding procedures and grinding may affect

moisture content due to the generation of heat and loss of moisture due to the physical

process of particle size reduction.

Table 5 and Table 6 provides a comparison of the average results for this study to the

certificates of analyses for 1R6F and NIST SRM 3222 where certified values are available4,5.

The values in this study are in good agreement with the certificates.

4 Certificate of Analysis for 1R6F Certified Reference Cigarette, Certificate Number 2016-002CTRP, University

of Kentucky Center for Tobacco Reference Products. 5 Certificate of Analysis for NIST Standard Reference Material

® 3222 Cigarette Tobacco Filler, National

Institute of Standards and Technology.


Table 5: Comparison of Study Results to Certified Values for 1R6F

Parameter Current Study

Mean Certified Mean

Values4

Certified Uncertainty

4

NNN (µg/g) 2.29 2.131 0.450

NNK (µg/g) 0.68 0.676 0.384

Moisture % 11.85 11.27 3.99

pH 5.32 5.45 0.29

Table 6: Comparison of Study Results to Certified Values for NIST SRM 32225

Parameter Current Study

Mean Certified Mean

Values5

Certified Uncertainty

5

NNN (µg/g) 1.54 1.440 0.090

NNK (µg/g) 0.032 0.0313 0.0025

Moisture % 11.52 12.1 0.6

7. Recommendations

The CRMs listed below were originally developed for the analysis of smokeless tobacco

products:

- TSNAs: CRM N° 72, Determination of Tobacco Specific Nitrosamines in Smokeless

Tobacco Products by Liquid Chromatography - Tandem Mass Spectrometry, February

2016. - pH: CRM N° 69, Determination of pH in Smokeless Tobacco Products, June 2010

- Moisture (oven volatiles): CRM N° 76, Determination of Moisture Content (Oven

Volatiles) of Smokeless Tobacco Products, April 2014.

The results of this study demonstrate that the CRMs are also fit for the analysis of ground

tobacco, cigarette filler, and cigar filler. The TTPA recommends the scope of the CRMs be

updated to include these additional matrices and that the r & R data from this study be added

to the CRMs. The TTPA also recommends that ISO/CD 21766 “Tobacco and tobacco

products- Determination of tobacco-specific nitrosamines in tobacco and tobacco products-

Method using LC-MS/MS” be updated to include the r & R data supporting the inclusion of

ground tobacco, cigarette filler and cigar filler.

8. Appendices

Appendix A: Full Data Set

Appendix B: Raw Data Plots


APPENDIX A: Full Data Set

Full Data Set (results are presented on an as-is basis)

NNK NNN NAT NAB

Oven volatiles

pH

Lab Code Product µg/g µg/g µg/g µg/g %

A 1R6F 0.636 2.189 2.047 0.093 12.33 5.30

A 1R6F 0.611 2.322 2.022 0.091 12.21 5.30

A 1R6F 0.592 2.311 2.018 0.090 12.20 5.25

B 1R6F – – – – 11.90 5.31

B 1R6F – – – – 12.08 5.31

B 1R6F – – – – 11.99 5.31

C 1R6F 0.614 1.820 1.892 0.082 11.91 5.27

C 1R6F 0.678 2.018 1.898 0.080 11.95 5.26

C 1R6F 0.680 1.922 1.832 0.082 11.90 5.27

D 1R6F 0.768 2.477 2.519 0.172 11.61 5.27

D 1R6F 0.808 2.530 2.502 0.176 11.70 5.28

D 1R6F 0.791 2.590 2.468 0.178 11.78 5.27

E 1R6F 0.624 2.102 2.169 0.079 11.85 5.38

E 1R6F 0.639 2.184 2.242 0.078 11.75 5.39

E 1R6F 0.612 2.174 2.151 0.077 11.75 5.38

F 1R6F 0.692 2.318 2.096 0.095 11.58 5.22

F 1R6F 0.677 2.332 2.178 0.097 11.76 5.18

F 1R6F 0.747 2.337 2.092 0.095 11.62 5.19

G 1R6F – – – – – 5.23

G 1R6F – – – – – 5.24

G 1R6F – – – – – 5.23

H 1R6F – – – – 12.60 5.33

H 1R6F – – – – 12.40 5.35

H 1R6F – – – – 12.30 5.32

I 1R6F – – – – 11.97 5.29

I 1R6F – – – – 12.13 5.30

I 1R6F – – – – 12.13 5.32

J 1R6F 0.651 2.150 1.906 0.082 11.71 5.33

J 1R6F 0.640 2.292 2.083 0.086 11.68 5.33

J 1R6F 0.665 2.589 2.032 0.088 11.71 5.29

K 1R6F 0.772 2.356 2.017 0.108 11.80 5.31

K 1R6F 0.767 2.385 2.034 0.114 11.80 5.31

K 1R6F 0.632 2.480 2.149 0.116 11.80 5.32


NNK NNN NAT NAB

Oven volatiles

pH


L 1R6F 0.820 2.200 2.240 0.105 11.00 5.29

L 1R6F 0.810 2.040 2.150 0.092 11.10 5.26

L 1R6F 0.760 1.980 2.105 0.095 11.00 5.25

M 1R6F 0.679 2.346 1.987 0.113 – –

M 1R6F 0.698 2.432 2.066 0.114 – –

M 1R6F 0.716 2.521 2.125 0.123 – –

N 1R6F 0.628 2.226 1.839 0.101 11.82 5.24

N 1R6F 0.625 2.168 1.841 0.101 11.79 5.24

N 1R6F 0.607 2.268 1.826 0.101 11.86 5.23

O 1R6F 0.623 2.212 1.979 0.120 12.15 5.52

O 1R6F 0.626 2.283 1.817 0.089 12.08 5.46

O 1R6F 0.628 2.308 1.957 0.128 12.19 5.43

P 1R6F 0.722 2.692 2.348 0.115 12.05 5.24

P 1R6F 0.737 2.727 2.361 0.112 11.99 5.26

P 1R6F 0.725 2.713 2.369 0.111 12.05 5.26

Q 1R6F – – – – 12.07 5.25

Q 1R6F – – – – 11.72 5.25

Q 1R6F – – – – 11.47 5.26

R 1R6F 0.688 2.652 2.198 0.109 12.15 5.32

R 1R6F 0.689 2.585 2.163 0.105 12.10 5.34

R 1R6F 0.685 2.584 2.152 0.105 12.11 5.33

S 1R6F – – – – – 5.55

S 1R6F – – – – – 5.57

S 1R6F – – – – – 5.58

T 1R6F 0.669 2.184 2.219 0.106 – –

T 1R6F 0.695 2.294 2.139 0.104 – –

T 1R6F 0.722 2.351 2.154 0.102 – –

U 1R6F 0.587 2.654 2.101 0.093 11.75 5.33

U 1R6F 0.585 2.662 1.928 0.091 11.77 5.33

U 1R6F 0.593 2.746 1.961 0.096 11.73 5.33

V 1R6F 0.571 1.761 2.244 0.122 – –

V 1R6F 0.585 1.654 2.691 0.128 – –

V 1R6F 0.596 1.647 2.543 0.123 – –

X 1R6F 0.689 2.130 1.750 0.114 11.60 5.34

X 1R6F 0.662 2.100 1.850 0.110 11.50 5.35

X 1R6F 0.681 1.950 1.680 0.110 11.50 5.36


NNK NNN NAT NAB

Oven volatiles

pH


Y 1R6F 0.692 2.376 1.989 0.101 11.36 5.35

Y 1R6F 0.704 2.306 1.987 0.100 11.53 5.40

Y 1R6F 0.680 2.265 1.912 0.098 11.59 5.33

A 1R5F 0.740 3.324 1.959 0.106 12.80 4.95

A 1R5F 0.763 3.455 2.153 0.121 12.83 4.92

A 1R5F 0.762 3.301 2.114 0.117 12.76 4.90

B 1R5F – – – – 12.68 4.79

B 1R5F – – – – 12.50 4.77

B 1R5F – – – – 12.47 4.78

C 1R5F 0.770 3.006 1.826 0.098 12.84 4.81

C 1R5F 0.770 3.034 1.798 0.098 12.82 4.82

C 1R5F 0.764 2.994 1.810 0.096 12.81 4.81

D 1R5F 0.911 3.674 2.387 0.179 12.62 4.84

D 1R5F 0.956 3.647 2.397 0.172 12.62 4.85

D 1R5F 0.916 3.801 2.354 0.187 12.61 4.86

E 1R5F – – – – – –

E 1R5F – – – – – –

E 1R5F – – – – – –

F 1R5F 0.764 3.025 1.919 0.096 12.55 4.84

F 1R5F 0.758 3.140 1.906 0.103 12.45 4.81

F 1R5F 0.753 3.169 1.919 0.105 12.50 4.80

G 1R5F – – – – – 4.75

G 1R5F – – – – – 4.75

G 1R5F – – – – – 4.74

H 1R5F – – – – 13.00 4.94

H 1R5F – – – – 12.80 4.95

H 1R5F – – – – 13.00 4.91

I 1R5F – – – – 12.66 4.93

I 1R5F – – – – 12.67 4.91

I 1R5F – – – – 12.73 4.90

J 1R5F 0.716 3.581 2.161 0.093 12.47 4.85

J 1R5F 0.699 3.328 2.020 0.097 12.52 4.87

J 1R5F 0.706 3.273 2.118 0.092 12.60 4.82

K 1R5F 0.728 3.197 2.058 0.121 12.50 4.85

K 1R5F 0.737 3.081 1.961 0.124 12.60 4.85

K 1R5F 0.804 3.216 1.983 0.127 12.60 4.86


NNK NNN NAT NAB

Oven volatiles

pH


L 1R5F 0.859 2.977 1.939 0.100 12.10 4.83

L 1R5F 0.921 3.302 2.102 0.107 12.00 4.80

L 1R5F 0.825 2.963 2.088 0.102 12.00 4.79

M 1R5F 0.807 3.460 2.186 0.118 – –

M 1R5F 0.763 3.508 2.087 0.119 – –

M 1R5F 0.801 3.536 2.113 0.120 – –

N 1R5F 0.692 3.017 1.811 0.117 12.45 4.80

N 1R5F 0.730 3.099 1.888 0.117 12.55 4.83

N 1R5F 0.699 3.131 1.883 0.114 12.54 4.81

O 1R5F 0.779 3.361 2.055 0.124 12.61 4.98

O 1R5F 0.746 3.090 1.925 0.075 12.58 4.99

O 1R5F 0.840 2.940 1.745 0.115 12.63 5.00

P 1R5F 0.786 3.620 2.169 0.112 12.87 4.78

P 1R5F 0.792 3.641 2.166 0.101 12.85 4.79

P 1R5F 0.794 3.646 2.146 0.113 12.81 4.80

Q 1R5F – – – – 12.50 4.81

Q 1R5F – – – – 12.69 4.83

Q 1R5F – – – – 12.76 4.84

R 1R5F 0.845 3.528 2.108 0.117 12.84 4.90

R 1R5F 0.839 3.629 2.105 0.115 12.86 4.92

R 1R5F 0.854 3.465 2.133 0.116 12.83 4.91

S 1R5F – – – – – 5.31

S 1R5F – – – – – 5.34

S 1R5F – – – – – 5.33

T 1R5F 0.832 3.108 2.113 0.116 – –

T 1R5F 0.747 3.305 2.071 0.114 – –

T 1R5F 0.755 3.029 2.033 0.115 – –

U 1R5F 0.785 3.931 2.004 0.107 12.63 4.89

U 1R5F 0.723 3.794 2.092 0.107 12.70 4.89

U 1R5F 0.713 3.912 2.074 0.101 12.64 4.90

V 1R5F 0.715 2.384 2.316 0.118 – –

V 1R5F 0.690 2.295 2.166 0.131 – –

V 1R5F 0.681 2.295 2.196 0.139 – –

X 1R5F 0.822 2.570 1.700 0.118 12.80 4.90

X 1R5F 0.816 2.380 1.670 0.114 12.70 4.89

X 1R5F 0.826 2.480 1.610 0.116 12.70 4.91


NNK NNN NAT NAB

Oven volatiles

pH


Y 1R5F 0.781 3.234 1.934 0.107 12.60 4.92

Y 1R5F 0.784 3.200 1.925 0.113 12.85 4.91

Y 1R5F 0.773 3.201 1.905 0.107 12.81 4.94

A RTDAC 1.544 3.899 3.925 0.221 12.72 5.96

A RTDAC 1.740 4.056 4.238 0.201 12.69 5.90

A RTDAC 1.811 3.873 4.279 0.220 12.73 5.87

B RTDAC – – – – 12.51 5.93

B RTDAC – – – – 12.46 5.94

B RTDAC – – – – 12.46 5.93

C RTDAC 1.948 3.080 3.862 0.228 12.88 5.81

C RTDAC 1.934 3.068 3.846 0.222 12.71 5.83

C RTDAC 1.930 3.062 3.896 0.224 12.60 5.81

D RTDAC 2.198 5.016 5.171 0.396 12.41 5.85

D RTDAC 2.222 4.958 5.091 0.382 12.43 5.86

D RTDAC 2.265 4.862 5.112 0.393 12.41 5.85

E RTDAC – – – – – –

E RTDAC – – – – – –

E RTDAC – – – – – –

F RTDAC 2.003 3.914 4.197 0.218 12.40 5.85

F RTDAC 2.141 3.977 4.284 0.220 12.48 5.71

F RTDAC 1.922 3.774 4.259 0.223 12.52 5.74

G RTDAC – – – – – 5.82

G RTDAC – – – – – 5.83

G RTDAC – – – – – 5.82

H RTDAC – – – – 13.10 5.90

H RTDAC – – – – 13.10 5.91

H RTDAC – – – – 13.10 5.91

I RTDAC – – – – 12.77 5.92

I RTDAC – – – – 12.62 5.95

I RTDAC – – – – 12.62 5.91

J RTDAC 1.748 4.736 4.460 0.220 12.36 5.93

J RTDAC 1.737 4.432 3.973 0.217 12.43 5.93

J RTDAC 1.801 4.339 4.262 0.201 12.40 5.92

K RTDAC 2.073 4.093 4.216 0.248 12.10 5.91

K RTDAC 2.088 3.904 4.225 0.242 12.30 5.92

K RTDAC 1.850 4.279 4.581 0.260 12.20 5.93


NNK NNN NAT NAB

Oven volatiles

pH


L RTDAC 1.901 3.214 4.815 0.213 11.90 5.86

L RTDAC 2.132 3.248 4.426 0.214 12.10 5.88

L RTDAC 1.928 3.334 4.703 0.215 11.70 5.86

M RTDAC 1.826 4.096 4.576 0.228 – –

M RTDAC 2.076 4.391 4.496 0.242 – –

M RTDAC 1.960 4.218 4.668 0.241 – –

N RTDAC 1.553 3.723 3.856 0.232 12.30 5.98

N RTDAC 1.675 3.636 4.038 0.242 12.21 5.97

N RTDAC 1.579 3.757 3.899 0.240 12.25 5.94

O RTDAC 1.890 3.754 4.242 0.256 12.75 6.12

O RTDAC 1.735 3.678 4.171 0.267 12.71 6.13

O RTDAC 1.771 3.572 3.857 0.247 12.60 6.12

P RTDAC 1.761 4.385 4.588 0.214 12.70 5.83

P RTDAC 1.850 4.598 4.847 0.229 12.71 5.84

P RTDAC 1.747 4.441 4.646 0.228 12.73 5.85

Q RTDAC – – – – 12.38 5.79

Q RTDAC – – – – 12.46 5.79

Q RTDAC – – – – 12.52 5.77

R RTDAC 2.286 4.976 4.678 0.249 12.54 5.87

R RTDAC 2.560 4.437 4.610 0.245 12.60 5.89

R RTDAC 2.031 4.413 4.496 0.233 12.55 5.86

S RTDAC – – – – – –

S RTDAC – – – – – –

S RTDAC – – – – – –

T RTDAC 2.100 4.002 4.476 0.234 – –

T RTDAC 1.985 3.855 4.549 0.222 – –

T RTDAC 1.732 3.744 4.217 0.214 – –

U RTDAC 2.284 4.806 4.340 0.230 12.42 5.93

U RTDAC 1.810 4.857 4.635 0.220 12.37 5.94

U RTDAC 1.965 4.684 4.467 0.213 12.39 5.92

V RTDAC 1.503 2.947 4.558 0.217 – –

V RTDAC 1.663 2.950 4.802 0.260 – –

V RTDAC 1.506 2.854 4.460 0.240 – –

X RTDAC 1.970 3.110 3.680 0.248 12.80 5.94

X RTDAC 1.940 3.210 3.660 0.248 12.80 5.94

X RTDAC 2.120 3.260 3.710 0.260 12.60 5.95


NNK NNN NAT NAB

Oven volatiles

pH


Y RTDAC 1.793 3.981 4.442 0.242 12.60 5.90

Y RTDAC 1.819 3.911 4.162 0.226 12.48 5.95

Y RTDAC 1.900 3.943 4.244 0.230 12.69 5.91

A RT2 0.154 0.255 0.299 0.017 12.93 5.07

A RT2 0.133 0.240 0.229 0.018 12.93 5.06

A RT2 0.131 0.216 0.237 0.017 12.88 5.07

B RT2 – – – – 12.73 5.04

B RT2 – – – – 12.83 5.03

B RT2 – – – – 12.89 5.03

C RT2 0.080 0.112 0.176 0.012 12.55 4.95

C RT2 0.080 0.112 0.172 0.012 12.54 4.95

C RT2 0.076 0.114 0.172 0.012 12.60 4.95

D RT2 0.133 0.132 0.231 0.018 12.48 5.01

D RT2 0.138 0.131 0.228 0.020 12.48 5.00

D RT2 0.137 0.140 0.228 0.018 12.50 5.00

E RT2 – – – – – –

E RT2 – – – – – –

E RT2 – – – – – –

F RT2 0.098 0.111 0.206 0.011 12.43 4.90

F RT2 0.096 0.110 0.197 0.011 12.42 4.92

F RT2 0.094 0.115 0.202 0.011 12.36 4.94

G RT2 – – – – – 4.90

G RT2 – – – – – 4.91

G RT2 – – – – – 4.89

H RT2 – – – – 13.40 5.09

H RT2 – – – – 13.40 5.11

H RT2 – – – – 13.10 5.09

I RT2 – – – – 12.69 5.10

I RT2 – – – – 12.95 5.11

I RT2 – – – – 12.76 5.14

J RT2 0.092 0.106 0.202 0.012 12.60 4.92

J RT2 0.104 0.124 0.213 0.012 12.55 4.92

J RT2 0.094 0.132 0.196 0.011 12.68 4.93

K RT2 0.101 0.127 0.178 0.012 12.80 5.04

K RT2 0.100 0.122 0.188 0.013 12.80 5.05

K RT2 0.085 0.120 0.184 0.013 12.80 5.03


NNK NNN NAT NAB

Oven volatiles

pH


L RT2 0.103 0.114 0.198 0.011 12.00 4.90

L RT2 0.122 0.108 0.199 0.011 11.70 4.95

L RT2 0.118 0.105 0.230 0.010 11.90 4.90

M RT2 0.116 0.117 0.175 0.021 – –

M RT2 0.104 0.127 0.180 0.022 – –

M RT2 0.109 0.128 0.173 0.025 – –

N RT2 0.102 0.120 0.176 0.013 12.25 4.96

N RT2 0.104 0.113 0.176 0.018 12.28 4.94

N RT2 0.104 0.109 0.173 0.015 12.39 4.93

O RT2 0.105 0.132 0.205 0.011 J 12.85 5.08

O RT2 0.124 0.144 0.233 0.010 J 12.98 5.08

O RT2 0.103 0.118 0.164 0.009 J 13.01 5.08

P RT2 0.109 0.145 0.188 0.019 12.75 4.94

P RT2 0.109 0.145 0.195 0.020 12.81 4.92

P RT2 0.108 0.144 0.194 0.020 12.85 4.93

Q RT2 – – – – 12.77 5.04

Q RT2 – – – – 12.73 5.07

Q RT2 – – – – 12.61 5.04

R RT2 0.107 0.110 0.204 0.012 12.72 5.11

R RT2 0.113 0.111 0.202 0.012 12.79 5.11

R RT2 0.116 0.104 0.202 0.011 12.79 5.11

S RT2 – – – – – –

S RT2 – – – – – –

S RT2 – – – – – –

T RT2 0.085 J 0.119 0.181 U – –

T RT2 0.085 J 0.119 0.199 U – –

T RT2 0.090 J 0.114 0.204 U – –

U RT2 0.135 0.152 0.203 0.011 12.74 5.02

U RT2 0.146 0.137 0.190 0.012 12.70 5.01

U RT2 0.138 0.141 0.187 0.016 12.73 5.00

V RT2 0.083 0.087 0.266 0.012 – –

V RT2 0.089 0.085 0.257 0.012 – –

V RT2 0.087 0.086 0.206 0.010 – –

X RT2 0.115 0.070 0.170 0.013 12.50 5.03

X RT2 0.102 0.080 0.170 0.014 12.50 5.03

X RT2 0.100 0.070 0.170 0.016 12.50 5.01


NNK NNN NAT NAB

Oven volatiles

pH


Y RT2 0.094 0.119 0.159 0.011 12.37 5.12

Y RT2 0.093 0.118 0.158 0.012 12.62 5.20

Y RT2 0.100 0.116 0.158 0.011 12.38 5.15

A SRM 3222 0.040 1.430 0.067 0.009 11.84 8.56

A SRM 3222 0.051 1.437 0.075 0.009 11.92 8.56

A SRM 3222 0.038 1.527 0.065 0.008 11.75 8.57

B SRM 3222 – – – – 11.60 8.76

B SRM 3222 – – – – 11.60 8.76

B SRM 3222 – – – – 11.60 8.72

C SRM 3222 0.032 1.302 0.036 0.006 11.62 8.95

C SRM 3222 0.030 1.384 0.048 0.004 11.84 8.94

C SRM 3222 0.032 1.310 0.040 0.006 12.12 8.98

D SRM 3222 0.035 1.826 0.058 0.010 11.59 8.62

D SRM 3222 0.038 1.812 0.060 0.011 11.49 8.64

D SRM 3222 0.038 1.849 0.058 0.010 11.68 8.66

E SRM 3222 – – – – – –

E SRM 3222 – – – – – –

E SRM 3222 – – – – – –

F SRM 3222 0.035 1.534 0.040 0.007 11.27 8.62

F SRM 3222 0.029 1.490 0.039 0.006 11.25 8.55

F SRM 3222 0.029 1.470 0.040 0.006 11.29 8.58

G SRM 3222 – – – – – –

G SRM 3222 – – – – – –

G SRM 3222 – – – – – –

H SRM 3222 – – – – 7.70 8.59

H SRM 3222 – – – – 7.50 8.55

H SRM 3222 – – – – 7.50 8.55

I SRM 3222 – – – – – –

I SRM 3222 – – – – – –

I SRM 3222 – – – – – –

J SRM 3222 0.033 1.502 0.046 0.006 11.69 8.71

J SRM 3222 0.028 1.512 0.038 0.006 11.72 8.74

J SRM 3222 0.028 1.518 0.046 0.006 11.69 8.74

K SRM 3222 0.028 1.453 0.045 0.007 11.30 8.65

K SRM 3222 0.027 1.374 0.044 0.008 11.50 8.67

K SRM 3222 0.028 1.432 0.046 0.007 11.20 8.66


NNK NNN NAT NAB

Oven volatiles

pH


L SRM 3222 0.032 1.465 0.040 0.006 10.80 8.68

L SRM 3222 0.043 1.630 0.042 0.007 10.80 8.72

L SRM 3222 0.039 1.510 0.034 0.008 10.50 8.77

M SRM 3222 – – – – – –

M SRM 3222 – – – – – –

M SRM 3222 – – – – – –

N SRM 3222 0.043 1.432 0.064 0.012 11.41 8.69

N SRM 3222 0.042 1.449 0.063 0.010 11.37 8.67

N SRM 3222 0.042 1.420 0.060 0.011 11.39 8.65

O SRM 3222 0.028 J 1.311 0.042 0.011 J 11.69 8.85

O SRM 3222 0.039 1.345 0.039 U 11.24 8.81

O SRM 3222 0.023 J 1.426 0.049 0.005 J 11.26 8.79

P SRM 3222 – – – – – –

P SRM 3222 – – – – – –

P SRM 3222 – – – – – –

Q SRM 3222 – – – – 11.09 8.78

Q SRM 3222 – – – – 11.12 8.87

Q SRM 3222 – – – – 10.96 8.84

R SRM 3222 0.032 1.843 0.047 0.007 11.08 8.87

R SRM 3222 0.032 1.859 0.049 0.007 11.10 8.85

R SRM 3222 0.031 1.813 0.048 0.007 11.05 8.87

S SRM 3222 – – – – – –

S SRM 3222 – – – – – –

S SRM 3222 – – – – – –

T SRM 3222 0.018 J 1.501 0.045 J U – –

T SRM 3222 0.015 J 1.439 0.043 J U – –

T SRM 3222 0.014 J 1.425 0.041 J U – –

U SRM 3222 0.028 1.853 0.062 0.008 12.30 8.63

U SRM 3222 0.027 1.934 0.060 0.008 12.21 8.58

U SRM 3222 0.028 1.961 0.065 0.008 12.18 8.68

V SRM 3222 – – – – – –

V SRM 3222 – – – – – –

V SRM 3222 – – – – – –

X SRM 3222 0.034 1.510 0.040 0.006 12.00 8.66

X SRM 3222 0.035 1.530 0.040 0.007 11.90 8.65

X SRM 3222 0.037 1.500 0.040 0.007 11.90 8.68


NNK NNN NAT NAB

Oven volatiles

pH


Y SRM 3222 0.030 1.479 0.039 0.008 11.74 8.68

Y SRM 3222 0.027 1.466 0.039 0.007 11.87 8.69

Y SRM 3222 0.028 1.444 0.037 0.007 11.81 8.63

A Cigar filler #1 1.649 5.629 2.637 0.185 19.35 5.14

A Cigar filler #1 1.620 5.557 2.816 0.190 19.34 5.14

A Cigar filler #1 1.668 5.721 2.731 0.184 19.36 5.13

B Cigar filler #1 – – – – 19.05 5.12

B Cigar filler #1 – – – – 18.99 5.13

B Cigar filler #1 – – – – 18.85 5.13

C Cigar filler #1 1.896 4.726 2.460 0.164 18.64 5.03

C Cigar filler #1 1.726 4.550 2.518 0.162 18.53 5.02

C Cigar filler #1 1.792 4.588 2.524 0.162 18.67 5.04

D Cigar filler #1 2.299 6.805 3.292 0.321 18.17 5.12

D Cigar filler #1 2.301 6.916 3.229 0.326 18.21 5.09

D Cigar filler #1 2.485 6.892 3.296 0.325 17.98 5.09

E Cigar filler #1 1.665 4.972 2.950 0.152 18.65 5.11

E Cigar filler #1 1.693 5.080 2.894 0.151 17.90 5.07

E Cigar filler #1 1.675 4.893 2.872 0.151 18.65 5.09

F Cigar filler #1 1.833 5.347 2.677 0.187 18.29 5.09

F Cigar filler #1 1.813 5.387 2.656 0.194 18.66 5.08

F Cigar filler #1 1.810 5.299 2.632 0.197 18.41 5.06

G Cigar filler #1 – – – – – 5.03

G Cigar filler #1 – – – – – 5.03

G Cigar filler #1 – – – – – 5.03

H Cigar filler #1 – – – – 18.90 5.13

H Cigar filler #1 – – – – 18.90 5.13

H Cigar filler #1 – – – – 18.90 5.13

I Cigar filler #1 – – – – 18.92 5.16

I Cigar filler #1 – – – – 18.82 5.18

I Cigar filler #1 – – – – 18.88 5.19

J Cigar filler #1 1.642 5.890 2.816 0.181 18.01 –

J Cigar filler #1 1.644 5.873 3.026 0.172 18.30 –

J Cigar filler #1 1.665 5.679 3.150 0.185 18.20 –

K Cigar filler #1 1.788 5.452 2.953 0.216 18.90 5.12

K Cigar filler #1 1.852 5.568 2.914 0.231 18.70 5.11

K Cigar filler #1 1.924 5.467 2.890 0.218 18.80 5.12


NNK NNN NAT NAB

Oven volatiles

pH


L Cigar filler #1 1.573 5.155 2.896 0.171 17.40 5.05

L Cigar filler #1 1.783 5.597 3.154 0.199 17.20 5.05

L Cigar filler #1 1.663 5.089 2.863 0.174 17.40 5.01

M Cigar filler #1 1.870 5.724 2.903 0.198 – –

M Cigar filler #1 1.840 5.820 2.948 0.190 – –

M Cigar filler #1 1.887 6.085 3.065 0.199 – –

N Cigar filler #1 1.792 5.323 2.549 0.184 18.42 5.11

N Cigar filler #1 1.698 5.393 2.597 0.170 18.49 5.10

N Cigar filler #1 1.635 5.258 2.564 0.164 18.45 5.13

O Cigar filler #1 1.821 5.354 2.745 0.197 18.66 5.22

O Cigar filler #1 1.767 5.537 2.444 0.217 18.83 5.23

O Cigar filler #1 1.741 5.356 2.689 0.204 18.83 5.23

P Cigar filler #1 – – – – – –



Q Cigar filler #1 – – – – 18.62 5.06

Q Cigar filler #1 – – – – 18.61 5.07

Q Cigar filler #1 – – – – 18.55 5.06

R Cigar filler #1 1.958 5.949 2.794 0.188 18.81 5.17

R Cigar filler #1 1.942 5.981 2.761 0.183 18.81 5.17

R Cigar filler #1 1.941 6.003 2.795 0.186 18.80 5.18

S Cigar filler #1 – – – – – 5.23

S Cigar filler #1 – – – – – 5.24

S Cigar filler #1 – – – – – 5.25

T Cigar filler #1 1.863 5.495 2.873 0.193 – –

T Cigar filler #1 1.743 5.510 2.861 0.178 – –

T Cigar filler #1 1.755 5.294 2.849 0.179 – –

U Cigar filler #1 1.666 6.227 2.836 0.186 18.45 5.11

U Cigar filler #1 1.716 6.465 2.940 0.182 18.47 5.11

U Cigar filler #1 1.630 6.321 2.874 0.193 18.39 5.11

V Cigar filler #1 – – – – – –



X Cigar filler #1 2.040 4.190 2.460 0.213 – –

X Cigar filler #1 1.970 4.130 2.440 0.213 – –

X Cigar filler #1 1.930 4.420 2.580 0.200 – –


NNK NNN NAT NAB

Oven volatiles

pH


Y Cigar filler #1 1.841 5.415 2.840 0.197 18.27 5.18

Y Cigar filler #1 1.871 5.480 2.883 0.205 18.38 5.18

Y Cigar filler #1 1.900 5.578 2.880 0.197 17.86 5.17

A Cigar M16 0.808 3.363 1.652 0.130 14.97 6.07

A Cigar M16 0.825 3.212 1.767 0.133 14.67 6.05

A Cigar M16 0.871 3.413 1.985 0.126 14.79 6.06

B Cigar M16 – – – – 14.65 6.24

B Cigar M16 – – – – 14.68 6.25

B Cigar M16 – – – – 14.54 6.26

C Cigar M16 0.872 2.396 1.514 0.108 14.68 6.18

C Cigar M16 0.916 2.400 1.568 0.108 14.68 6.19

C Cigar M16 0.888 2.478 1.514 0.120 14.82 6.18

D Cigar M16 1.057 4.599 2.006 0.236 14.23 6.21

D Cigar M16 1.151 4.424 2.064 0.227 14.36 6.26

D Cigar M16 1.109 4.550 1.989 0.223 14.48 6.28

E Cigar M16 0.798 3.182 1.729 0.112 14.50 6.35

E Cigar M16 0.812 3.135 1.706 0.111 14.40 6.28

E Cigar M16 0.819 3.011 1.721 0.110 14.35 6.30

F Cigar M16 0.920 3.365 1.692 0.135 14.54 6.21

F Cigar M16 0.905 3.517 1.704 0.132 14.46 6.15

F Cigar M16 0.927 3.410 1.741 0.129 14.45 6.14

G Cigar M16 – – – – – 6.14

G Cigar M16 – – – – – 6.13

G Cigar M16 – – – – – 6.12

H Cigar M16 – – – – 14.50 6.25

H Cigar M16 – – – – 14.60 6.26

H Cigar M16 – – – – 14.60 6.26

I Cigar M16 – – – – 14.91 6.28

I Cigar M16 – – – – 14.79 6.29

I Cigar M16 – – – – 14.71 6.26

J Cigar M16 0.878 3.769 1.930 0.125 14.52 –

J Cigar M16 0.858 3.731 1.656 0.118 13.95 –

J Cigar M16 0.785 3.973 1.846 0.117 14.69 –

K Cigar M16 0.935 3.519 1.788 0.156 14.70 6.26

K Cigar M16 0.902 3.676 1.717 0.171 15.20 6.27

K Cigar M16 0.945 3.556 1.638 0.155 14.70 6.28


NNK NNN NAT NAB

Oven volatiles

pH


L Cigar M16 0.818 3.631 1.977 0.154 13.90 6.18

L Cigar M16 0.801 3.433 1.810 0.127 14.00 6.22

L Cigar M16 0.820 3.546 1.956 0.146 13.80 6.20

M Cigar M16 0.963 3.773 1.875 0.148 – –

M Cigar M16 0.906 3.759 1.850 0.146 – –

M Cigar M16 0.926 4.078 1.859 0.143 – –

N Cigar M16 0.848 3.341 1.621 0.140 14.58 6.28

N Cigar M16 0.854 3.369 1.621 0.144 14.40 6.28

N Cigar M16 0.832 3.586 1.595 0.147 14.33 6.26

O Cigar M16 0.970 3.160 1.111 0.105 14.69 6.46

O Cigar M16 0.891 3.069 1.492 0.143 14.83 6.46

O Cigar M16 0.919 3.120 1.521 0.150 14.80 6.46

P Cigar M16 – – – – – –

P Cigar M16 – – – – – –

P Cigar M16 – – – – – –

Q Cigar M16 – – – – 14.54 6.15

Q Cigar M16 – – – – 14.43 6.18

Q Cigar M16 – – – – 14.69 6.17

R Cigar M16 0.954 3.851 1.783 0.138 14.92 6.32

R Cigar M16 0.973 3.841 1.771 0.137 14.95 6.28

R Cigar M16 0.973 3.770 1.763 0.138 14.91 6.29

S Cigar M16 – – – – – 6.43

S Cigar M16 – – – – – 6.42

S Cigar M16 – – – – – 6.43

T Cigar M16 0.859 3.416 1.835 0.141 – –

T Cigar M16 0.947 3.400 1.860 0.143 – –

T Cigar M16 0.890 3.510 1.771 0.140 – –

U Cigar M16 0.836 4.195 1.764 0.130 14.57 6.25

U Cigar M16 0.928 4.084 1.687 0.131 14.51 6.25

U Cigar M16 0.867 3.934 1.653 0.132 14.53 6.26

V Cigar M16 – – – – – –

V Cigar M16 – – – – – –

V Cigar M16 – – – – – –

X Cigar M16 – – – – – –

X Cigar M16 – – – – – –

X Cigar M16 – – – – – –


NNK NNN NAT NAB

Oven volatiles

pH


Y Cigar M16 0.947 3.527 1.730 0.137 14.53 6.30

Y Cigar M16 0.928 3.494 1.756 0.140 14.35 6.26

Y Cigar M16 0.901 3.460 1.717 0.142 14.51 6.25

The (–) symbol indicates the laboratory did not submit a value for that sample analysis.

The (J) symbol indicates the result was below the limit of quantitation.

The (U) symbol indicates the result was below the limit of detection.


APPENDIX B: Raw Data Plots

tobacco and tobacco products analytes sub-group · tobacco and tobacco products analytes sub-group...

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