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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.
TTPA-126-1-CTR 2017 Collaborative Study on TSNA, pH, and OV – July 2017 4/36
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
TTPA-126-1-CTR 2017 Collaborative Study on TSNA, pH, and OV – July 2017 5/36
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.
TTPA-126-1-CTR 2017 Collaborative Study on TSNA, pH, and OV – July 2017 6/36
- 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.
TTPA-126-1-CTR 2017 Collaborative Study on TSNA, pH, and OV – July 2017 7/36
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.
TTPA-126-1-CTR 2017 Collaborative Study on TSNA, pH, and OV – July 2017 8/36
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%
TTPA-126-1-CTR 2017 Collaborative Study on TSNA, pH, and OV – July 2017 9/36
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.
TTPA-126-1-CTR 2017 Collaborative Study on TSNA, pH, and OV – July 2017 10/36
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
TTPA-126-1-CTR 2017 Collaborative Study on TSNA, pH, and OV – July 2017 11/36
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
TTPA-126-1-CTR 2017 Collaborative Study on TSNA, pH, and OV – July 2017 12/36
NNK NNN NAT NAB
Oven volatiles
pH
Lab Code Product µg/g µg/g µg/g µg/g %
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
TTPA-126-1-CTR 2017 Collaborative Study on TSNA, pH, and OV – July 2017 13/36
NNK NNN NAT NAB
Oven volatiles
pH
Lab Code Product µg/g µg/g µg/g µg/g %
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
TTPA-126-1-CTR 2017 Collaborative Study on TSNA, pH, and OV – July 2017 14/36
NNK NNN NAT NAB
Oven volatiles
pH
Lab Code Product µg/g µg/g µg/g µg/g %
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
TTPA-126-1-CTR 2017 Collaborative Study on TSNA, pH, and OV – July 2017 15/36
NNK NNN NAT NAB
Oven volatiles
pH
Lab Code Product µg/g µg/g µg/g µg/g %
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
TTPA-126-1-CTR 2017 Collaborative Study on TSNA, pH, and OV – July 2017 16/36
NNK NNN NAT NAB
Oven volatiles
pH
Lab Code Product µg/g µg/g µg/g µg/g %
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
TTPA-126-1-CTR 2017 Collaborative Study on TSNA, pH, and OV – July 2017 17/36
NNK NNN NAT NAB
Oven volatiles
pH
Lab Code Product µg/g µg/g µg/g µg/g %
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
TTPA-126-1-CTR 2017 Collaborative Study on TSNA, pH, and OV – July 2017 18/36
NNK NNN NAT NAB
Oven volatiles
pH
Lab Code Product µg/g µg/g µg/g µg/g %
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
TTPA-126-1-CTR 2017 Collaborative Study on TSNA, pH, and OV – July 2017 19/36
NNK NNN NAT NAB
Oven volatiles
pH
Lab Code Product µg/g µg/g µg/g µg/g %
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
TTPA-126-1-CTR 2017 Collaborative Study on TSNA, pH, and OV – July 2017 20/36
NNK NNN NAT NAB
Oven volatiles
pH
Lab Code Product µg/g µg/g µg/g µg/g %
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
TTPA-126-1-CTR 2017 Collaborative Study on TSNA, pH, and OV – July 2017 21/36
NNK NNN NAT NAB
Oven volatiles
pH
Lab Code Product µg/g µg/g µg/g µg/g %
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
TTPA-126-1-CTR 2017 Collaborative Study on TSNA, pH, and OV – July 2017 22/36
NNK NNN NAT NAB
Oven volatiles
pH
Lab Code Product µg/g µg/g µg/g µg/g %
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 – – – – – –
P Cigar filler #1 – – – – – –
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 – – – – – –
V Cigar filler #1 – – – – – –
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 – –
TTPA-126-1-CTR 2017 Collaborative Study on TSNA, pH, and OV – July 2017 23/36
NNK NNN NAT NAB
Oven volatiles
pH
Lab Code Product µg/g µg/g µg/g µg/g %
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
TTPA-126-1-CTR 2017 Collaborative Study on TSNA, pH, and OV – July 2017 24/36
NNK NNN NAT NAB
Oven volatiles
pH
Lab Code Product µg/g µg/g µg/g µg/g %
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 – – – – – –
TTPA-126-1-CTR 2017 Collaborative Study on TSNA, pH, and OV – July 2017 25/36
NNK NNN NAT NAB
Oven volatiles
pH
Lab Code Product µg/g µg/g µg/g µg/g %
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.
TTPA-126-1-CTR 2017 Collaborative Study on TSNA, pH, and OV – July 2017 26/36
APPENDIX B: Raw Data Plots