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Routine Analytical Chemistry Sub-Group Technical Report 2017 Collaborative Study of CORESTA Monitor 8 (CM8) for the Determination of Test Piece Weight, TPM, Water, Nicotine, NFDPM, Carbon Monoxide and Puff Count Obtained under Mainstream ‘ISO’ and ‘Intense’ Smoking Regimes November 2017 Coordinator: Linda A. Crumpler, Cerulean, USA Authors: Guy Jaccard and Donatien Tafin Djoko Philip Morris International, Switzerland

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Page 1: Routine Analytical Chemistry Sub-Group · RAC-134-CTR CM8 Coll. Study 2017 – November 2017 6/103 Table 5: WEIGHT mean and standard deviation per laboratory code Lab Code Machine

Routine Analytical Chemistry Sub-Group

Technical Report

2017 Collaborative Study of

CORESTA Monitor 8 (CM8)

for the Determination of Test Piece

Weight, TPM, Water, Nicotine,

NFDPM, Carbon Monoxide and Puff Count Obtained under Mainstream

‘ISO’ and ‘Intense’ Smoking

Regimes

November 2017

Coordinator:

Linda A. Crumpler, Cerulean, USA

Authors:

Guy Jaccard and Donatien Tafin Djoko

Philip Morris International, Switzerland

Page 2: Routine Analytical Chemistry Sub-Group · RAC-134-CTR CM8 Coll. Study 2017 – November 2017 6/103 Table 5: WEIGHT mean and standard deviation per laboratory code Lab Code Machine

Table of Contents

1. Introduction ......................................................................................................................... 3

2. Organisation ........................................................................................................................ 3

2.1 Participants .............................................................................................................. 3

2.2 Protocol ................................................................................................................... 4

3. Raw Data ............................................................................................................................. 5

4. Statistical Analysis ............................................................................................................ 26

4.1 Exclusion of outliers .............................................................................................. 26

4.1.1 Numerical outlier technique: Cochran & Grubbs test ............................... 26

4.2 Repeatability and Reproducibility estimation ....................................................... 26

5. Data Representation .......................................................................................................... 28

5.1 ISO smoking regime .............................................................................................. 29

5.2 Intense smoking regime ......................................................................................... 32

6. Comparison ....................................................................................................................... 35

Comparisons of Linear with Rotary smoking machines for test piece CM8 ........ 35

Comparison with previous studies ........................................................................ 35

7. Conclusion......................................................................................................................... 38

APPENDIX A – List of Participating Laboratories ................................................................. 39

APPENDIX B – Experimental Protocol .................................................................................. 40

APPENDIX C – Departures from Experimental Protocol ....................................................... 54

APPENDIX D – Raw Data Set ................................................................................................ 55

APPENDIX E – IUPAC 1994 Harmonized Statistical Procedure ........................................... 67

APPENDIX F – Linear – Rotary Comparisons ....................................................................... 68

APPENDIX G – Rotary Smoking Machines ........................................................................... 74

APPENDIX H – Linear Smoking Machines ............................................................................ 80

APPENDIX I – Equipment Survey .......................................................................................... 86

Page 3: Routine Analytical Chemistry Sub-Group · RAC-134-CTR CM8 Coll. Study 2017 – November 2017 6/103 Table 5: WEIGHT mean and standard deviation per laboratory code Lab Code Machine

RAC-134-CTR CM8 Coll. Study 2017 – November 2017 3/103

1. Introduction

The CORESTA Routine Analytical Chemistry Sub-Group has been given the responsibility to

organize the annual testing of the CORESTA Monitor test piece.

The 2017 study was designed:

• to measure mainstream ISO and Intense smoke yields of nicotine-free dry particulate

matter (NFDPM), nicotine (NIC) and carbon monoxide (CO) to verify the current

monitor test piece CM8

• to determine intra- and inter-laboratory variability for the measured ISO and Intense

smoke yields for the CM8

• to verify the conditioned weight for the CM8

2. Organisation

2.1 Participants

In total 32 laboratories participated in the 2017 study. Appendix A lists the participating

laboratories in alphabetical order. Note: the mix of labs between ISO and Intense differed.

32 laboratories delivered data for ISO mainstream smoke for the CM8 test piece using 45

smoking machines (24 rotary smoking machines and 21 linear smoking machines).

26 laboratories delivered data for Intense mainstream smoke for the CM8 test piece using 34

smoking machines (16 rotary smoking machines and 18 linear smoking machines).

One laboratory provided an incomplete data set (conditioned weight data missing).

Table 1 summarises the number and type of smoking machines used.

Table 1: Number of smoking machines

Machine Class ISO Intense

Linear smoking machines 21 18

LX-20 type 2 2

SM450 type

LM20X type

Hawktech 2000 type

18

1

-

14

1

1

Rotary smoking machines 24 16

RM20 A type 1 1

RM20D type 2 2

RM20H type

RM 20M type

RM 20 type

6

1

1

3

1

1

RM200 A type 13 9

Total 45 34

Page 4: Routine Analytical Chemistry Sub-Group · RAC-134-CTR CM8 Coll. Study 2017 – November 2017 6/103 Table 5: WEIGHT mean and standard deviation per laboratory code Lab Code Machine

RAC-134-CTR CM8 Coll. Study 2017 – November 2017 4/103

Table 2 summarises the number of datasets provided for the reported parameters.

Table 2: Number of datasets obtained

Physical Parameter

WEIGHT 220

Smoking Parameter ISO Intense

TPM 225 170

WATER 225 170

NIC 225 170

NFDPM 225 170

CO 225 170

PUFF 225 170

Total individual data obtained 1350 1020

Total individual data expected 1350 1020

A code number has been assigned in confidence by the study co-ordinator to each of the

individual smoking machines used in the study.

2.2 Protocol

Participants were requested to follow the protocol “Annual Study of the CORESTA Monitor

Test Piece CM 8 - 2017 Experimental Protocol” (provided in Appendix B) to analyse the

product CM8 and to report the seven parameters listed in Table 3.

Table 3: Parameters to be reported

Parameter Number of replicates

Unit Code

Conditioned Weight 5 mg/test piece (t.p.) WEIGHT

Total Particulate Matter 5 mg/test piece (t.p.) TPM

Water content (smoke) 5 mg/test piece (t.p.) WATER

Smoke Nicotine 5 mg/test piece (t.p.) NIC

Nicotine Free Dry

Particulate Matter 5 mg/test piece (t.p.) NFDPM

Carbon Monoxide 5 mg/test piece (t.p.) CO

Puff count 5 puff/test piece (t.p.) PUFF

CM8 test pieces should have been smoked under two different mainstream smoking regimes

with a fixed butt length of 33 mm as defined in the following table:

Table 4: Mainstream ISO and Intense smoking regime parameters

Smoking

Regime

Puff Volume

(mL)

Puff Frequency

(s)

Puff Duration

(s)

Vent. Blocking

(%)

ISO 35 60 2 0

Intense 55 30 2 100

Page 5: Routine Analytical Chemistry Sub-Group · RAC-134-CTR CM8 Coll. Study 2017 – November 2017 6/103 Table 5: WEIGHT mean and standard deviation per laboratory code Lab Code Machine

RAC-134-CTR CM8 Coll. Study 2017 – November 2017 5/103

The CM8 test piece was purchased by the participants individually via Borgwaldt KC or

Cerulean.

3. Raw Data

Table 5 provides the results for conditioned weight, while Tables 6 to 11 list the results for the

reported parameters for ISO smoking regime. Tables 12 to 17 list the results for intense

smoking regime. Basic statistics (mean and standard deviation) were applied to summarize the

raw data for each smoking machine used and parameters reported for CM8 test piece. At this

stage no outlier statistics were applied. Appendix D contains the raw data (single values) for

every measured parameter reported by smoking machine included in the study.

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RAC-134-CTR CM8 Coll. Study 2017 – November 2017 6/103

Table 5: WEIGHT mean and standard deviation per laboratory code

Lab Code Machine Mean SD CV [%] Sample size

1B L 959.35 0.713 0.074 5

2B L 959.00 4.848 0.505 5

9A L 961.30 7.538 0.784 5

10 L 957.30 2.771 0.289 5

11 L 957.88 4.212 0.440 5

16A L 957.88 4.290 0.448 5

16B L 959.04 4.248 0.443 5

16C L 956.80 3.546 0.371 5

17 L 957.58 5.988 0.625 5

18 L 955.20 3.834 0.401 5

19 L 949.79 4.611 0.485 5

20 L 946.92 7.334 0.775 5

21 L 961.77 1.671 0.174 5

24 L 953.35 3.135 0.329 5

25 L 965.87 5.026 0.520 5

27 L 962.02 1.228 0.128 5

28 L 964.00 6.519 0.676 5

29 L 958.26 4.879 0.509 5

32 L 965.00 20.406 2.115 5

33 L 956.29 1.534 0.160 5

34 L 953.72 5.914 0.620 5

1A R 966.59 5.346 0.553 5

2A R 963.00 6.595 0.685 5

4A R 962.20 5.263 0.545 5

4B R 963.20 7.396 0.768 5

5A R 961.90 2.987 0.311 5

5B R 964.57 2.089 0.217 5

5C R 961.80 2.706 0.281 5

6A R 967.54 3.673 0.380 5

6B R 966.24 3.927 0.406 5

7 R 957.60 1.673 0.175 5

8 R 961.92 2.478 0.258 5

9B R 963.25 2.530 0.263 5

12 R 958.40 4.930 0.514 5

13A R 956.90 3.170 0.331 5

13B R 953.97 2.642 0.277 5

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RAC-134-CTR CM8 Coll. Study 2017 – November 2017 7/103

Lab Code Machine Mean SD CV [%] Sample size

14 R 965.42 2.873 0.298 5

15 R 961.20 4.396 0.457 5

16D R 954.44 3.942 0.413 5

22A R 960.20 1.095 0.114 5

22B R 961.00 1.581 0.165 5

26 R 968.29 6.119 0.632 5

30 R 956.74 2.596 0.271 5

31 R 955.82 6.732 0.704 5

35 R 961.51 3.861 0.402 5

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RAC-134-CTR CM8 Coll. Study 2017 – November 2017 8/103

Table 6: ISO smoking regime. TPM mean and standard deviation per laboratory code

Lab Code Machine

Type Mean

(mg/t.p.) SD CV [%] Sample size

1B L 17.54 0.34 1.92 5

2B L 17.71 0.07 0.38 5

9A L 17.41 0.48 2.78 5

10 L 18.12 0.52 2.85 5

11 L 17.75 0.61 3.41 5

16A L 17.35 0.29 1.67 5

16B L 17.56 0.25 1.43 5

16C L 16.99 0.25 1.47 5

17 L 16.45 0.42 2.55 5

18 L 18.60 0.56 3.00 5

19 L 18.14 0.35 1.92 5

20 L 17.96 1.47 8.16 5

21 L 18.04 0.44 2.46 5

24 L 16.46 0.66 4.00 5

25 L 17.28 0.81 4.69 5

27 L 16.65 0.27 1.64 5

28 L 17.42 0.35 2.03 5

29 L 17.32 0.20 1.14 5

32 L 15.96 0.70 4.37 5

33 L 18.15 0.46 2.51 5

34 L 17.10 0.30 1.76 5

1A R 16.53 0.32 1.95 5

2A R 17.58 0.32 1.81 5

4A R 17.53 0.13 0.77 5

4B R 18.12 0.61 3.34 5

5A R 17.13 0.22 1.26 5

5B R 17.07 0.21 1.25 5

5C R 17.08 0.29 1.69 5

6A R 18.11 0.22 1.21 5

6B R 17.65 0.37 2.08 5

7 R 17.95 0.56 3.11 5

8 R 17.62 0.26 1.50 5

9B R 16.86 0.31 1.81 5

12 R 17.58 0.40 2.27 5

13A R 16.41 0.35 2.15 5

13B R 16.29 0.21 1.26 5

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RAC-134-CTR CM8 Coll. Study 2017 – November 2017 9/103

Lab Code Machine

Type Mean

(mg/t.p.) SD CV [%] Sample size

14 R 17.58 0.18 1.02 5

15 R 17.99 0.30 1.64 5

16D R 17.25 0.22 1.27 5

22A R 17.30 0.18 1.02 5

22B R 17.30 0.20 1.14 5

26 R 17.97 0.24 1.33 5

30 R 16.88 0.08 0.47 5

31 R 17.83 0.21 1.19 5

35 R 16.67 0.22 1.33 5

Page 10: Routine Analytical Chemistry Sub-Group · RAC-134-CTR CM8 Coll. Study 2017 – November 2017 6/103 Table 5: WEIGHT mean and standard deviation per laboratory code Lab Code Machine

RAC-134-CTR CM8 Coll. Study 2017 – November 2017 10/103

Table 7: ISO smoking regime. WATER mean and standard deviation per laboratory code

Lab Code Machine

Type Mean

(mg/t.p.) SD CV [%] Sample size

1B L 1.53 0.08 5.42 5

2B L 1.54 0.15 9.59 5

9A L 1.53 0.09 5.99 5

10 L 1.61 0.11 6.73 5

11 L 1.59 0.19 11.81 5

16A L 1.21 0.12 10.32 5

16B L 1.17 0.09 7.95 5

16C L 1.20 0.08 6.42 5

17 L 1.24 0.09 6.91 5

18 L 1.67 0.16 9.63 5

19 L 1.68 0.17 9.98 5

20 L 1.18 0.34 28.95 5

21 L 1.32 0.02 1.58 5

24 L 1.43 0.08 5.82 5

25 L 1.30 0.13 9.62 5

27 L 1.30 0.14 10.91 5

28 L 1.64 0.11 6.89 5

29 L 1.54 0.15 9.99 5

32 L 1.75 0.30 16.88 5

33 L 1.65 0.12 7.20 5

34 L 1.79 0.23 13.11 5

1A R 1.80 0.08 4.29 5

2A R 1.98 0.22 11.17 5

4A R 2.02 0.08 3.87 5

4B R 2.37 0.20 8.32 5

5A R 2.10 0.10 4.84 5

5B R 2.08 0.11 5.25 5

5C R 2.02 0.16 8.01 5

6A R 2.53 0.09 3.44 5

6B R 2.38 0.06 2.56 5

7 R 2.17 0.14 6.67 5

8 R 2.20 0.18 8.20 5

9B R 2.04 0.12 6.11 5

12 R 2.50 0.12 4.64 5

13A R 2.07 0.14 6.56 5

13B R 2.02 0.10 4.98 5

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RAC-134-CTR CM8 Coll. Study 2017 – November 2017 11/103

Lab Code Machine

Type Mean

(mg/t.p.) SD CV [%] Sample size

14 R 1.96 0.11 5.82 5

15 R 2.43 0.25 10.50 5

16D R 1.32 0.05 3.96 5

22A R 2.11 0.10 4.68 5

22B R 2.08 0.05 2.60 5

26 R 2.34 0.08 3.21 5

30 R 1.85 0.14 7.79 5

31 R 2.03 0.23 11.34 5

35 R 1.98 0.13 6.68 5

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RAC-134-CTR CM8 Coll. Study 2017 – November 2017 12/103

Table 8: ISO smoking regime. NICOTINE mean and standard deviation per laboratory code

Lab Code Machine

Type Mean

(mg/t.p.) SD CV [%] Sample size

1B L 1.721 0.048 2.79 5

2B L 1.635 0.033 2.03 5

9A L 1.623 0.049 2.99 5

10 L 1.747 0.106 6.09 5

11 L 1.718 0.041 2.38 5

16A L 1.764 0.039 2.20 5

16B L 1.804 0.029 1.63 5

16C L 1.783 0.037 2.07 5

17 L 1.596 0.031 1.91 5

18 L 1.718 0.028 1.65 5

19 L 1.753 0.026 1.46 5

20 L 1.700 0.125 7.35 5

21 L 1.698 0.035 2.06 5

24 L 1.541 0.053 3.43 5

25 L 1.708 0.045 2.64 5

27 L 1.693 0.013 0.77 5

28 L 1.685 0.034 2.04 5

29 L 1.848 0.025 1.37 5

32 L 1.823 0.026 1.42 5

33 L 1.763 0.029 1.64 5

34 L 1.582 0.017 1.09 5

1A R 1.610 0.035 2.16 5

2A R 1.629 0.026 1.58 5

4A R 1.656 0.017 1.02 5

4B R 1.639 0.059 3.61 5

5A R 1.620 0.021 1.33 5

5B R 1.582 0.026 1.63 5

5C R 1.599 0.046 2.89 5

6A R 1.725 0.027 1.56 5

6B R 1.688 0.033 1.93 5

7 R 1.679 0.043 2.54 5

8 R 1.688 0.038 2.23 5

9B R 1.560 0.049 3.16 5

12 R 1.719 0.024 1.42 5

13A R 1.504 0.021 1.40 5

13B R 1.485 0.066 4.43 5

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RAC-134-CTR CM8 Coll. Study 2017 – November 2017 13/103

Lab Code Machine

Type Mean

(mg/t.p.) SD CV [%] Sample size

14 R 1.650 0.019 1.13 5

15 R 1.649 0.022 1.34 5

16D R 1.715 0.005 0.28 5

22A R 1.606 0.022 1.36 5

22B R 1.614 0.026 1.62 5

26 R 1.647 0.026 1.59 5

30 R 1.658 0.008 0.46 5

31 R 1.854 0.031 1.69 5

35 R 1.649 0.027 1.63 5

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RAC-134-CTR CM8 Coll. Study 2017 – November 2017 14/103

Table 9: ISO smoking regime. NFDPM mean and standard deviation per laboratory code

Lab Code Machine

Type Mean

(mg/t.p.) SD CV [%] Sample size

1B L 14.29 0.25 1.72 5

2B L 14.55 0.15 1.01 5

9A L 14.21 0.36 2.54 5

10 L 14.75 0.36 2.46 5

11 L 14.45 0.43 2.99 5

16A L 14.37 0.25 1.74 5

16B L 14.59 0.30 2.06 5

16C L 14.01 0.24 1.74 5

17 L 13.61 0.34 2.50 5

18 L 15.21 0.44 2.88 5

19 L 14.70 0.18 1.20 5

20 L 15.08 1.13 7.51 5

21 L 15.03 0.45 2.98 5

24 L 13.49 0.53 3.92 5

25 L 14.27 0.66 4.59 5

27 L 13.66 0.16 1.21 5

28 L 14.10 0.27 1.90 5

29 L 14.09 0.68 4.83 5

32 L 11.79 1.66 14.12 5

33 L 14.74 0.38 2.55 5

34 L 13.74 0.36 2.59 5

1A R 13.11 0.22 1.64 5

2A R 13.97 0.14 1.00 5

4A R 13.85 0.09 0.65 5

4B R 14.11 0.39 2.76 5

5A R 13.41 0.14 1.05 5

5B R 13.41 0.17 1.29 5

5C R 13.46 0.34 2.53 5

6A R 13.86 0.18 1.32 5

6B R 13.58 0.31 2.25 5

7 R 14.10 0.41 2.91 5

8 R 13.73 0.16 1.13 5

9B R 13.26 0.22 1.63 5

12 R 13.37 0.37 2.78 5

13A R 12.83 0.24 1.89 5

13B R 12.78 0.27 2.13 5

Page 15: Routine Analytical Chemistry Sub-Group · RAC-134-CTR CM8 Coll. Study 2017 – November 2017 6/103 Table 5: WEIGHT mean and standard deviation per laboratory code Lab Code Machine

RAC-134-CTR CM8 Coll. Study 2017 – November 2017 15/103

Lab Code Machine

Type Mean

(mg/t.p.) SD CV [%] Sample size

14 R 13.97 0.09 0.67 5

15 R 13.92 0.16 1.17 5

16D R 14.22 0.26 1.86 5

22A R 13.59 0.10 0.71 5

22B R 13.60 0.20 1.47 5

26 R 13.99 0.20 1.44 5

30 R 13.37 0.08 0.59 5

31 R 13.95 0.28 2.03 5

35 R 13.04 0.13 1.02 5

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RAC-134-CTR CM8 Coll. Study 2017 – November 2017 16/103

Table 10: ISO smoking regime. CO mean and standard deviation per laboratory code

Lab Code Machine

Type Mean

(mg/t.p.) SD CV [%] Sample size

1B L 12.79 0.24 1.90 5

2B L 13.84 0.15 1.12 5

9A L 12.62 0.23 1.83 5

10 L 12.80 0.50 3.93 5

11 L 12.28 0.42 3.44 5

16A L 12.82 0.41 3.21 5

16B L 12.78 0.17 1.35 5

16C L 13.49 0.08 0.56 5

17 L 12.34 0.50 4.03 5

18 L 14.50 0.89 6.15 5

19 L 13.92 0.18 1.31 5

20 L 12.87 1.00 7.76 5

21 L 13.39 0.26 1.96 5

24 L 11.81 0.48 4.08 5

25 L 12.69 0.36 2.82 5

27 L 12.89 0.74 5.74 5

28 L 12.72 0.47 3.70 5

29 L 12.04 0.30 2.46 5

32 L 12.06 0.45 3.76 5

33 L 13.57 0.22 1.65 5

34 L 12.79 0.56 4.40 5

1A R 12.89 0.30 2.35 5

2A R 13.74 0.12 0.90 5

4A R 13.50 0.12 0.93 5

4B R 13.40 0.26 1.96 5

5A R 13.72 0.22 1.58 5

5B R 13.48 0.26 1.94 5

5C R 13.54 0.14 1.05 5

6A R 14.52 0.22 1.48 5

6B R 14.35 0.40 2.80 5

7 R 14.22 0.46 3.21 5

8 R 13.84 0.48 3.49 5

9B R 12.73 0.27 2.11 5

12 R 13.17 0.34 2.56 5

13A R 13.03 0.37 2.86 5

13B R 12.87 0.23 1.79 5

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RAC-134-CTR CM8 Coll. Study 2017 – November 2017 17/103

Lab Code Machine

Type Mean

(mg/t.p.) SD CV [%] Sample size

14 R 13.46 0.09 0.67 5

15 R 14.15 0.42 2.94 5

16D R 13.45 0.46 3.39 5

22A R 13.47 0.30 2.24 5

22B R 13.67 0.06 0.45 5

26 R 13.42 0.34 2.55 5

30 R 13.12 0.13 1.01 5

31 R 13.56 0.26 1.92 5

35 R 13.00 0.24 1.87 5

Page 18: Routine Analytical Chemistry Sub-Group · RAC-134-CTR CM8 Coll. Study 2017 – November 2017 6/103 Table 5: WEIGHT mean and standard deviation per laboratory code Lab Code Machine

RAC-134-CTR CM8 Coll. Study 2017 – November 2017 18/103

Table 11: ISO smoking regime. PUFF COUNT mean and standard deviation per laboratory code

Lab Code Machine

Type Mean

(puff/t.p.) SD CV [%] Sample size

1B L 8.05 0.08 0.98 5

2B L 8.08 0.08 1.02 5

9A L 7.73 0.17 2.16 5

10 L 7.95 0.17 2.13 5

11 L 8.01 0.22 2.72 5

16A L 8.33 0.06 0.67 5

16B L 8.58 0.16 1.83 5

16C L 8.51 0.17 2.05 5

17 L 7.83 0.09 1.19 5

18 L 7.87 0.12 1.53 5

19 L 7.92 0.14 1.71 5

20 L 7.42 0.21 2.85 5

21 L 7.95 0.11 1.38 5

24 L 7.40 0.24 3.23 5

25 L 7.99 0.20 2.51 5

27 L 7.80 0.10 1.25 5

28 L 8.13 0.11 1.37 5

29 L 7.46 0.08 1.02 5

32 L 8.70 0.17 1.91 5

33 L 8.05 0.10 1.18 5

34 L 7.98 0.02 0.26 5

1A R 7.54 0.06 0.83 5

2A R 7.56 0.14 1.82 5

4A R 7.54 0.05 0.73 5

4B R 7.50 0.12 1.63 5

5A R 7.83 0.23 2.99 5

5B R 7.41 0.12 1.66 5

5C R 7.48 0.06 0.79 5

6A R 7.85 0.11 1.38 5

6B R 7.73 0.06 0.78 5

7 R 7.61 0.10 1.38 5

8 R 7.74 0.11 1.41 5

9B R 7.40 0.08 1.07 5

12 R 7.55 0.06 0.78 5

13A R 7.28 0.17 2.38 5

13B R 7.16 0.12 1.66 5

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RAC-134-CTR CM8 Coll. Study 2017 – November 2017 19/103

Lab Code Machine

Type Mean

(puff/t.p.) SD CV [%] Sample size

14 R 7.64 0.08 1.02 5

15 R 7.75 0.11 1.45 5

16D R 7.87 0.08 1.05 5

22A R 7.63 0.12 1.52 5

22B R 7.43 0.06 0.84 5

26 R 8.02 0.13 1.68 5

30 R 7.49 0.06 0.75 5

31 R 7.65 0.12 1.50 5

35 R 7.63 0.11 1.41 5

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Table 12: Intense smoking regime. TPM mean and standard deviation per laboratory code

Lab Code Machine

Type Mean

(mg/t.p.) SD CV [%] Sample size

1B L 45.09 0.40 0.89 5

2B L 45.19 0.76 1.68 5

10 L 46.31 1.46 3.15 5

11 L 45.85 0.83 1.80 5

16A L 44.12 1.16 2.62 5

16B L 44.77 0.46 1.04 5

16C L 41.59 0.70 1.68 5

17 L 43.74 1.49 3.40 5

18 L 48.01 0.61 1.28 5

19 L 48.16 0.55 1.14 5

20 L 46.54 0.29 0.63 5

21 L 50.52 0.83 1.63 5

24 L 43.20 1.38 3.20 5

25 L 44.67 0.88 1.97 5

27 L 44.30 0.84 1.90 5

29 L 44.85 0.85 1.90 5

33 L 44.86 1.24 2.77 5

34 L 44.72 0.93 2.08 5

1A R 38.55 0.24 0.63 5

2A R 41.21 0.66 1.60 5

4A R 42.34 0.25 0.60 5

4B R 42.12 0.75 1.77 5

6A R 42.67 0.50 1.18 5

6B R 42.14 0.38 0.91 5

7 R 41.58 0.61 1.48 5

8 R 41.36 0.31 0.75 5

12 R 41.25 0.46 1.12 5

16D R 39.91 0.27 0.68 5

22A R 40.17 0.50 1.25 5

22B R 40.58 0.67 1.65 5

26 R 40.38 0.57 1.41 5

30 R 40.70 0.32 0.78 5

31 R 40.86 0.44 1.07 5

35 R 42.09 0.78 1.85 5

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Table 13: Intense smoking regime. WATER mean and standard deviation per laboratory code

Lab Code Machine

Type Mean

(mg/t.p.) SD CV [%] Sample size

1B L 12.23 0.19 1.52 5

2B L 10.65 0.29 2.74 5

10 L 10.77 0.78 7.27 5

11 L 11.58 0.51 4.43 5

16A L 9.48 0.42 4.39 5

16B L 10.34 0.43 4.13 5

16C L 9.18 0.30 3.30 5

17 L 10.62 0.52 4.94 5

18 L 13.19 0.71 5.36 5

19 L 13.02 0.33 2.51 5

20 L 11.46 0.72 6.25 5

21 L 13.33 0.68 5.12 5

24 L 10.58 0.56 5.29 5

25 L 9.67 0.82 8.45 5

27 L 11.36 0.51 4.51 5

29 L 11.71 0.44 3.76 5

33 L 10.67 0.85 8.01 5

34 L 12.22 0.44 3.64 5

1A R 8.61 0.10 1.16 5

2A R 8.74 0.34 3.84 5

4A R 9.32 0.20 2.19 5

4B R 9.67 0.21 2.13 5

6A R 9.68 0.22 2.31 5

6B R 9.41 0.24 2.54 5

7 R 9.23 0.18 1.96 5

8 R 9.61 0.38 3.95 5

12 R 10.04 0.51 5.08 5

16D R 7.79 0.15 1.89 5

22A R 9.36 0.25 2.70 5

22B R 9.82 0.45 4.58 5

26 R 9.18 0.30 3.28 5

30 R 9.36 0.17 1.79 5

31 R 7.92 0.51 6.41 5

35 R 9.91 0.67 6.81 5

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Table 14: Intense smoking regime. NICOTINE mean and standard deviation per laboratory code

Lab Code Machine

Type Mean

(mg/t.p.) SD CV [%] Sample size

1B L 3.466 0.075 2.16 5

2B L 3.384 0.043 1.28 5

10 L 3.546 0.277 7.83 5

11 L 3.522 0.070 1.98 5

16A L 3.514 0.069 1.96 5

16B L 3.558 0.057 1.61 5

16C L 3.486 0.077 2.21 5

17 L 3.359 0.140 4.17 5

18 L 3.424 0.035 1.02 5

19 L 3.500 0.016 0.45 5

20 L 3.476 0.059 1.68 5

21 L 3.566 0.024 0.68 5

24 L 3.256 0.073 2.25 5

25 L 3.282 0.033 1.00 5

27 L 3.394 0.049 1.44 5

29 L 3.580 0.032 0.88 5

33 L 3.516 0.050 1.43 5

34 L 3.462 0.058 1.69 5

1A R 3.219 0.019 0.59 5

2A R 3.316 0.028 0.84 5

4A R 3.487 0.032 0.92 5

4B R 3.277 0.060 1.83 5

6A R 3.433 0.036 1.04 5

6B R 3.443 0.057 1.65 5

7 R 3.266 0.115 3.52 5

8 R 3.481 0.104 2.98 5

12 R 3.452 0.030 0.85 5

16D R 3.346 0.084 2.50 5

22A R 3.216 0.046 1.44 5

22B R 3.214 0.052 1.60 5

26 R 3.148 0.033 1.04 5

30 R 3.631 0.028 0.78 5

31 R 3.733 0.018 0.48 5

35 R 3.558 0.085 2.39 5

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Table 15: Intense smoking regime. NFDPM mean and standard deviation per laboratory code

Lab Code Machine

Type Mean

(mg/t.p.) SD CV [%] Sample size

1B L 29.40 0.23 0.77 5

2B L 31.16 0.63 2.01 5

10 L 32.01 0.88 2.75 5

11 L 30.76 0.44 1.44 5

16A L 31.13 0.75 2.41 5

16B L 30.87 0.49 1.59 5

16C L 28.91 0.42 1.45 5

17 L 29.77 1.26 4.22 5

18 L 31.40 0.36 1.13 5

19 L 31.64 0.44 1.38 5

20 L 31.60 0.53 1.69 5

21 L 33.62 0.26 0.77 5

24 L 29.37 0.77 2.62 5

25 L 31.74 0.34 1.08 5

27 L 29.54 0.40 1.34 5

29 L 29.66 0.35 1.19 5

33 L 30.68 0.43 1.39 5

34 L 29.03 0.63 2.18 5

1A R 26.72 0.17 0.65 5

2A R 29.15 0.35 1.20 5

4A R 29.53 0.44 1.48 5

4B R 29.18 0.52 1.79 5

6A R 29.56 0.28 0.93 5

6B R 29.29 0.28 0.96 5

7 R 29.09 0.48 1.64 5

8 R 28.26 0.27 0.96 5

12 R 27.76 0.48 1.71 5

16D R 28.78 0.37 1.29 5

22A R 27.59 0.21 0.78 5

22B R 27.55 0.40 1.47 5

26 R 28.06 0.41 1.46 5

30 R 27.71 0.22 0.78 5

31 R 29.20 0.18 0.63 5

35 R 28.62 0.66 2.29 5

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Table 16: Intense smoking regime. CO mean and standard deviation per laboratory code

Lab Code Machine

Type Mean

(mg/t.p.) SD CV [%] Sample size

1B L 24.39 0.32 1.33 5

2B L 25.87 0.46 1.76 5

10 L 23.51 0.75 3.20 5

11 L 23.44 0.23 0.96 5

16A L 24.18 0.58 2.39 5

16B L 23.81 0.30 1.28 5

16C L 24.76 0.41 1.66 5

17 L 23.44 0.62 2.66 5

18 L 25.70 0.57 2.21 5

19 L 26.10 0.16 0.61 5

20 L 24.46 0.91 3.71 5

21 L 25.65 0.18 0.69 5

24 L 23.67 0.79 3.33 5

25 L 24.12 0.30 1.23 5

27 L 27.20 1.27 4.68 5

29 L 23.08 0.40 1.74 5

33 L 24.72 0.30 1.22 5

34 L 24.94 0.41 1.63 5

1A R 24.21 0.39 1.61 5

2A R 25.82 0.41 1.59 5

4A R 25.39 0.15 0.60 5

4B R 24.90 0.38 1.51 5

6A R 26.22 0.54 2.06 5

6B R 26.10 0.19 0.73 5

7 R 25.70 0.50 1.96 5

8 R 25.78 0.06 0.22 5

12 R 25.06 0.23 0.93 5

16D R 24.73 0.39 1.60 5

22A R 24.80 0.31 1.25 5

22B R 25.22 0.22 0.87 5

26 R 24.69 0.38 1.55 5

30 R 25.19 0.29 1.15 5

31 R 25.82 0.53 2.06 5

35 R 24.86 0.40 1.60 5

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Table 17: Intense smoking regime. PUFF COUNT mean and standard deviation per laboratory code

Lab Code Machine

Type Mean

(puff/t.p.) SD CV [%] Sample size

1B L 11.35 0.12 1.05 5

2B L 11.51 0.08 0.66 5

10 L 11.23 0.22 2.00 5

11 L 11.14 0.21 1.87 5

16A L 11.79 0.22 1.84 5

16B L 12.16 0.19 1.58 5

16C L 11.90 0.25 2.13 5

17 L 11.40 0.13 1.18 5

18 L 11.13 0.07 0.62 5

19 L 10.82 0.11 0.98 5

20 L 10.52 0.17 1.59 5

21 L 11.32 0.13 1.11 5

24 L 10.75 0.25 2.30 5

25 L 11.47 0.18 1.53 5

27 L 11.04 0.17 1.57 5

29 L 10.74 0.16 1.52 5

33 L 11.32 0.16 1.41 5

34 L 11.46 0.10 0.89 5

1A R 10.80 0.20 1.85 5

2A R 10.92 0.12 1.05 5

4A R 10.82 0.08 0.70 5

4B R 10.70 0.11 0.99 5

6A R 10.85 0.10 0.94 5

6B R 11.07 0.09 0.85 5

7 R 11.03 0.10 0.94 5

8 R 10.97 0.15 1.34 5

12 R 11.02 0.20 1.86 5

16D R 11.34 0.13 1.13 5

22A R 10.97 0.10 0.95 5

22B R 10.39 0.14 1.39 5

26 R 11.25 0.14 1.23 5

30 R 10.44 0.06 0.56 5

31 R 11.22 0.10 0.85 5

35 R 11.12 0.18 1.59 5

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4. Statistical Analysis

4.1 Exclusion of outliers

4.1.1 Numerical outlier technique: Cochran & Grubbs test

The statistical evaluation of data for this collaborative study followed the methods provided

by ISO 5725-21. For outlier testing, the Grubbs and Cochran methods were used.

ISO 5725-2 Tests Consistency

Cochran’s – test Within-laboratory variability: Suitable for detecting whether the highest value in a set of laboratory standard deviations is an outlier or not.

Grubbs’ – test Between-laboratory variability: Suitable for detecting whether the highest (or lowest) laboratories averages are outliers or not.

The protocol “Harmonized statistical procedure” defined by IUPAC (International Union of

Pure and Applied Chemistry) has been applied as well. It consists of sequential applications

of the Cochran and Grubbs tests until no further outliers are detected or until a drop of more

than 22.2% in the original number of laboratories would occur (see flowchart in Appendix F).

First apply the Cochran outlier test, and if an outlying laboratory is identified, then a single

value Grubbs test is performed on the individual values of this outlying laboratory (Individual

Grubbs). If no individual value is identified as outlier, the outlying laboratory is removed.

When an individual value is identified as an outlier, only this value is removed.

Afterwards single-value Grubbs test is applied and outlying laboratories are removed. If no

laboratory is identified as outlier, the pair-value test is applied (two values at the same end).

Remove any laboratory(ies) flagged by these tests, but stop removal if more than 22.2%

would be removed.

The test was performed with both linear and rotary smoking machines together, but also with

rotary, respectively linear smoking machines separately. The results provided in the report for

all smoking machines, respectively with linear or rotary only smoking machines are obtained

after exclusion of the outliers for those respective categories.

Note:

The paired value Grubbs’ test is an extension of the single value Grubbs' test for pairs of

outliers. The use is advised in ISO 5725 to detect pairs of outlier undetectable sequentially by

using single value Grubbs' test.

The outlying laboratories are provided in the Tables 18 to 23.

4.2 Repeatability and Reproducibility estimation

Repeatability and reproducibility limits are calculated for both smoking regimes, each

parameter and for both smoking machine types. The results are summarized in tables 18 to 23,

with all machines grouped, respectively with linear or rotary machines only, both with ISO

and intense smoking regimes. Outlying laboratories are provided in the same tables. The

corresponding graphs named “individual values” are given in Part 5 of this report.

1 “ISO 5725-2:1994 : Accuracy (trueness and precision) of measurement methods and results – Part 2: Basic

method for the determination of repeatability and reproducibility of a standard measurement method

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Table 18: r&R estimations for CM8 under ISO smoking regime (all machines)

p n Global Mean

Sr CVr [%]

r SR CVR [%]

R C G/G2 Stragglers Parameter

All

44 5 959.705 4.358 0.454 12.328 6.031 0.628 17.057 32 NA 32 Conditioned.Weight

45 5 17.370 0.377 2.171 1.067 0.684 3.937 1.934 20 NA 25 TPM

45 5 1.820 0.141 7.734 0.398 0.405 22.236 1.145 20 NA 32 Water

45 5 1.672 0.034 2.031 0.096 0.090 5.376 0.254 20-10 NA NA Nicotine

45 5 13.952 0.314 2.247 0.887 0.656 4.700 1.855 32-20 NA 32-29 NFDPM

45 5 13.208 0.341 2.585 0.966 0.697 5.276 1.971 20-18 NA NA CO

45 5 7.780 0.128 1.638 0.360 0.355 4.564 1.004 NA NA NA Puff.count

Table 19: r&R estimations for CM8 under ISO smoking regime (rotary machines)

p n Global Mean

Sr CVr [%]

r SR CVR [%]

R C G/G2 Stragglers Parameter

Rotary

24 5 17.345 0.299 1.724 0.846 0.604 3.483 1.709 NA NA 4B TPM

24 5 2.099 0.139 6.601 0.392 0.284 13.539 0.804 NA NA 16D Water

24 5 1.643 0.033 2.011 0.093 0.081 4.906 0.228 NA NA 31 Nicotine

24 5 13.603 0.235 1.729 0.665 0.458 3.366 1.295 NA NA NA NFDPM

24 5 13.512 0.296 2.189 0.837 0.538 3.985 1.523 NA NA NA CO

24 5 7.595 0.111 1.461 0.314 0.219 2.887 0.620 NA NA 5A Puff.count

Table 20: r&R estimations for CM8 under ISO smoking regime (linear machines)

p n Global Mean

Sr CVr [%]

r SR CVR [%]

R C G/G2 Stragglers Parameter

Linear

21 5 17.401 0.453 2.606 1.283 0.780 4.483 2.207 20 NA NA TPM

21 5 1.485 0.143 9.654 0.405 0.235 15.853 0.666 20 NA 32 Water

21 5 1.708 0.035 2.054 0.099 0.089 5.224 0.252 20-10 NA NA Nicotine

21 5 14.393 0.391 2.714 1.105 0.602 4.181 1.702 32-20 NA 32 NFDPM

21 5 12.906 0.473 3.667 1.338 0.795 6.163 2.250 NA NA NA CO

21 5 7.991 0.144 1.802 0.407 0.368 4.604 1.040 NA NA NA Puff.count

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Table 21: r&R estimations for CM8 under Intense smoking regime (all machines)

p n Global Mean

Sr CVr[%] r SR CVR [%]

R C G/G2 Stragglers Parameter

All

34 5 43.365 0.766 1.767 2.167 2.780 6.411 7.863 NA NA NA TPM

34 5 10.285 0.471 4.578 1.332 1.479 14.378 4.183 NA NA NA Water

34 5 3.425 0.057 1.663 0.161 0.147 4.294 0.416 10-17 NA 17 Nicotine

34 5 29.654 0.459 1.549 1.299 1.613 5.439 4.562 17.janv NA NA NFDPM

34 5 24.858 0.438 1.764 1.240 0.961 3.867 2.719 27 NA 20 CO

34 5 11.116 0.153 1.379 0.433 0.417 3.754 1.180 NA NA NA Puff.count

Table 22: r&R estimations for CM8 under Intense smoking regime (rotary machines)

p n Global Mean

Sr CVr [%]

r SR CVR [%]

R C G/G2 Stragglers Parameter

Rotary

16 5 41.120 0.512 1.245 1.448 1.165 2.833 3.295 NA NA NA TPM

16 5 9.228 0.342 3.705 0.967 0.726 7.863 2.052 NA NA 35 Water

16 5 3.389 0.059 1.750 0.168 0.175 5.153 0.494 NA NA 7 Nicotine

16 5 28.503 0.381 1.337 1.078 0.919 3.226 2.600 NA NA NA NFDPM

16 5 25.280 0.362 1.431 1.023 0.661 2.613 1.869 NA NA NA CO

16 5 10.931 0.131 1.199 0.371 0.289 2.647 0.818 NA NA NA Puff.count

Table 23: r&R estimations for CM8 under Intense smoking regime (linear machines)

p n Global Mean

Sr CVr [%]

r SR CVR [ %]

R C G/G2 Stragglers Parameter

Linear

18 5 45.360 0.936 2.063 2.647 2.195 4.840 6.209 NA NA NA TPM

18 5 11.225 0.561 4.999 1.587 1.335 11.896 3.777 NA NA NA Water

18 5 3.462 0.055 1.575 0.154 0.106 3.058 0.299 '10-17 NA 7 Nicotine

18 5 30.737 0.522 1.699 1.477 1.353 4.400 3.825 17 NA NA NFDPM

18 5 24.461 0.500 2.044 1.414 1.041 4.256 2.944 27 NA NA CO

18 5 11.281 0.171 1.512 0.482 0.449 3.984 1.271 NA NA NA Puff.count

5. Data Representation

The following figures show the raw data for CM8 and for all parameters. The plots indicate

mean values with 95% confidence interval (CI) highlighted in green (for valid participants) or

in red (for participants detected as outlier) for each smoking machine. Laboratories excluded

by outlier statistics are denoted by the name of the test rejecting the laboratory (G for Grubbs,

G2 for double Grubbs and C for Cochran). The confidence limits at 95% and 99% for the

difference between the reference value (average of all laboratories) and the average of one

laboratory are plotted in orange and red respectively.

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5.1 ISO smoking regime

Figure 1: CM8 Individual observations of conditioned test piece WEIGHT

Outlier value in red

Figure 2: CM8 Individual observations of mainstream “ISO” TPM

Outlier value in red, straggler value in orange

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Figure 3: CM8 Individual observations of mainstream “ISO” WATER

Outlier value in red, straggler value in orange

Figure 4: CM8 Individual observations of mainstream “ISO” Nicotine

Outlier values in red

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Figure 5: CM8 Individual observations of mainstream “ISO” NFDPM

Outlier values in red, straggler value in orange

Figure 6: CM8 Individual observations of mainstream “ISO” CO

Outlier values in red

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Figure 7: CM8 Individual observations of mainstream “ISO” PUFF Count

5.2 Intense smoking regime

Figure 8: CM8 Individual observations of mainstream “Intense” TPM

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Figure 9: CM8 Individual observations of mainstream “Intense” WATER

Figure 10: CM8 Individual observations of mainstream “Intense” Nicotine

Outlier values in red

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Figure 11: CM8 Individual observations of mainstream “Intense” NFDPM

Outlier value in red

Figure 12: CM8 Individual observations of mainstream “Intense” CO

Outlier value in red, straggler value in orange

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Figure 13: CM8 Individual observations of mainstream “Intense” PUFF Count

6. Comparison

Comparisons of Linear with Rotary smoking machines for test piece CM8

It should be noted that a statistical evaluation of differences in linear and rotary smoking

machine results on the basis of just one product (CM8) could be misleading. Furthermore, a

simplistic differentiation between linear and rotary smoking machines could also be

misleading as both machine types used in this study comprise different models produced by

different manufacturers. Furthermore it has to be noted that each measurement from a rotary

machine represents a single result from a single pad onto which the smoke of twenty (or ten in

intense smoking regime) test pieces is trapped. Linear smoking machines require 4 pads to

collect mainstream TPM from the same number of test pieces and hence each measurement

on a linear machine is the average of 4 results. This has to be taken into account when

interpreting statistical differences in repeatability between machine classes.

Due to the aforementioned reasons a pure statistical comparison is considered to have limited

value.

Graphical comparison of smoke data separated for linear and rotary smoking machines are

available in Appendix F.

Comparison with previous studies

This section compares the results of this study with previous collaborative studies of different

test pieces conducted by the Routine Analytical Subgroup under the ISO smoking regime. It

has to be noted that the number of smoking machines, smoking machine types and

participants varies throughout the studies.

Table 24 lists the averages, reproducibility and repeatability limits for the test pieces CM6,

CM7 and CM8 under ISO smoking regime.

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Table 24: Averages, repeatability, reproducibility of CORESTA collaborative studies from 2008

to 2017 for different test pieces under ISO smoking conditions

ISO smoking regime

Year 2008 2010 2011 2011 2012 2013 2014 2014 2016 2017

Test piece CM6 CM6 CM6 CM7 CM7 CM7 CM7 CM8 CM8 CM8

Average

TPM (mg/t.p.)

17.54 17.37 17.43 16.37 16.28 16.16 16.15 17.57 17.33 17.37

WATER (mg/t.p.)

1.87 1.81 1.84 1.78 1.75 1.71 1.71 1.84 1.81 1.82

NICOTINE (mg/t.p.)

1.390 1.366 1.362 1.236 1.221 1.221 1.204 1.650 1.657 1.672

NFDPM (mg/t.p.)

14.28 14.18 14.21 13.34 13.29 13.23 13.25 14.06 13.86 13.95

CO (mg/t.p.)

14.83 14.56 14.42 12.93 12.84 12.76 12.83 13.42 13.24 13.21

PUFF (/t.p.)

9.15 9.09 9.00 8.36 8.36 8.32 8.23 7.70 7.72 7.78

Repeatability (r)

TPM (mg/t.p.)

0.83 0.81 0.94 0.93 0.80 0.85 0.87 1.06 1.05 1.07

WATER (mg/t.p.)

0.43 0.40 0.47 0.41 0.41 0.39 0.36 0.39 0.35 0.40

NICOTINE (mg/t.p.)

0.080 0.074 0.084 0.075 0.066 0.076 0.075 0.119 0.093 0.096

NFDPM (mg/t.p.)

0.71 0.63 0.80 0.77 0.78 0.72 0.72 0.82 0.89 0.89

CO (mg/t.p.)

0.82 0.92 0.95 0.95 0.78 0.75 0.79 1.05 0.79 0.97

PUFF (/t.p.)

0.37 0.39 0.33 0.38 0.34 0.31 0.36 0.30 0.39 0.36

Reproducibility (R)

TPM (mg/t.p.)

1.77 1.54 1.72 1.77 1.67 1.61 1.93 1.89 1.95 1.93

WATER (mg/t.p.)

1.11 1.09 0.98 0.97 1.03 0.98 1.01 1.12 1.08 1.15

NICOTINE (mg/t.p.)

0.131 0.150 0.173 0.150 0.143 0.146 0.155 0.197 0.202 0.254

NFDPM (mg/t.p.)

1.80 1.53 1.92 1.88 1.73 1.85 2.16 1.97 1.91 1.86

CO (mg/t.p.)

1.64 1.96 1.83 1.94 1.75 1.61 1.97 2.02 1.52 1.97

PUFF (/t.p.)

0.88 0.82 0.69 0.86 0.93 0.91 0.82 0.75 0.83 1.00

There is no systematic tendency for the mean values of CM 8 between 2014 and 2017: some

parameters decrease slightly, but nicotine increases slightly. Repeatability and reproducibility

figures are quite stable and comparable to those obtained with the other test pieces, taking into

account the slightly higher mean values of TPM and nicotine for CM 8 than for the previous

test pieces.

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Table 25 lists the averages, reproducibility and repeatability limits for the test pieces CM7 and

CM8 under intense smoking regime.

Table 25: Averages, repeatability, reproducibility of CORESTA collaborative studies from 2013

to 2017 for different test pieces under intense smoking conditions

Intense smoking regime Year 2013 2016 2017

Test piece CM7 CM8 CM8

Average

TPM (mg/t.p.) 41.56 43.08 43.36

WATER (mg/t.p.) 10.33 10.01 10.29

NICOTINE (mg/t.p.) 2.493 3.400 3.425

NFDPM (mg/t.p.) 28.39 29.65 29.65

CO (mg/t.p.) 24.72 24.88 24.86

PUFF (/t.p.) 11.79 11.08 11.12

Repeatability (r)

TPM (mg/t.p.) 2.38 1.96 2.167

WATER (mg/t.p.) 1.23 0.98 1.332

NICOTINE (mg/t.p.) 0.152 0.152 0.161

NFDPM (mg/t.p.) 1.57 1.39 1.299

CO (mg/t.p.) 1.30 1.04 1.240

PUFF (/t.p.) 0.52 0.47 0.433

Reproducibility (R)

TPM (mg/t.p.) 10.53 9.47 7.863

WATER (mg/t.p.) 4.77 3.79 4.183

NICOTINE (mg/t.p.) 0.313 0.508 0.416

NFDPM (mg/t.p.) 5.66 5.03 4.562

CO (mg/t.p.) 3.01 2.00 2.719

PUFF (/t.p.) 1.27 0.92 1.180

The mean values obtained for CM 8 are very stable between 2016 and 2017. The values for

repeatability and reproducibility are also generally well aligned.

Table 26 lists the averages, reproducibility and repeatability limits of conditioned weight

Table 26: Average weight data, repeatability and reproducibility for test pieces CM8

Study CM8 2014 CM8 2016 CM8 2017

Weight (mg/t.p.) 961.0 959.0 959.7

Repeatability (r) 14.1 11.4 12.3

Reproducibility (R) 17.3 17.5 17.1

The data obtained in the three collaborative tests for the test piece conditioned weight are

quite stable in terms of average, repeatability and reproducibility.

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7. Conclusion

In summary the analytical results for the CM8 test piece lead to the conclusion that it can be

used as a monitor test piece in smoke analysis.

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APPENDIX A – List of Participating Laboratories

Altria JTI Oekolab

ASL Karelia Tobacco Co.

BAT Brazil - Souza Cruz KT&G

BAT Germany (GmbH) Landewyck Group sarl.

Borgwaldt KC Liggett Group

C.I.T. Monte Paz S.A. LNE

China National Tobacco Quality Supervision and Test Center

Miaoli Tobacco Industry Corp.,LTD

Enthalpy Analytical Richmond MST/Vectis

Essentra Scientific Services Papierfabrik Wattens

Global Laboratory Service PMI AL CC's

Imperial JOURE PMI R&D

Imperial Tobacco Polaska S.A. PT HM Sampoerna Tbk.

Imperial Tobacco Production Ukraine (ITPU) R. J. Reynolds Tobacco Co.

INCIENSA-CNRBRO Reemstma/Imperial Tobacco

ITC Limited Seita

ITG Brands SWM-LTR

Japan Tobacco Inc. Tabacalera del Este S.A.

JTI Germany GmbH

Out of the 35 participating laboratories, 8 labs did not perform the intense smoking regime.

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APPENDIX B – Experimental Protocol

Routine Analytical Chemistry

Sub-Group

Collaborative Study

ANNUAL STUDY OF THE CORESTA

MONITOR TEST PIECE CM8 - 2017

EXPERIMENTAL PROTOCOL

Linda A. Crumpler, Cerulean, USA 10 January 2017

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Table of Contents

Foreword .................................................................................................................................. 41

1. Introduction .................................................................................................................. 43

2. Objectives ..................................................................................................................... 43

3. Study Coordinator(s) .................................................................................................... 43

4. Normative References .................................................................................................. 43

5. Methods ....................................................................................................................... 44

6. Target Variables and Data Reporting ........................................................................... 47

7. Study Time Table ......................................................................................................... 50

8. Data Submission ........................................................................................................... 50

9. Explanation of Minimum Statistics to be Applied for a Collaborative Study ............... 50

Bibliography ............................................................................................................................ 51

Appendix A – Système International (SI) Units and their Symbols ......................................... 52

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Foreword

This CORESTA protocol describes the elements that the Standards Task Force has identified

as important for describing elements of an experimental protocol for a collaborative study or

a proficiency study as defined below (Horwitz 862):

• Collaborative study

“A collaborative study is an interlaboratory study in which each laboratory uses the

defined method of analysis to analyse identical portions of homogeneous materials

to assess the performance characteristics obtained for that method of analysis.”

CORESTA recognizes that collaborative studies require considerable effort and

should be conducted only on methods that have received adequate prior testing.

• Proficiency Study

“A proficiency study is an interlaboratory study consisting of one or more assays-

conducted by a group of laboratories on one or more identical materials, by whatever

method is in use in each laboratory, for the purpose of comparing the results of each

laboratory with those of other laboratories, with the objective of evaluating or

improving performance.”

Proficiency studies often serve as pre-work for selecting a method for a

full collaborative study.

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1. Introduction

The CORESTA Routine Analytical Chemistry Sub Group has been given the

responsibility to organize the annual testing of the CORESTA Monitor test piece. This

year the study will include CM8.

2. Objectives

This year’s study will have expanded objectives that include smoking the monitor test

piece under both ISO and a specified intense smoking regime. The study objectives are:

• To measure mainstream smoke yields of nicotine-free dry particulate matter

(NFDPM), nicotine and carbon monoxide (CO) when smoked under ISO and a

specified intense smoking regime

• To establish the conditioned weight of CM8 prior to smoking

• To determine intra- and inter-laboratory variability for the measured smoke yields

and to continue this comparison over time

• To obtain statistical information about possible differences in smoke yields from

different smoking machines

3. Study Coordinator(s)

Linda A. Crumpler

Linda.crumpler(at)cerulean.com

Phone: +1 336-778-9282 Mobile: +1 804-274-0085

4. Normative References

The relevant Standards for ISO, Intense smoking and statistical analyses are:

Definitions and standard conditions ISO 3308

Conditioning ISO 3402

TPM / NFDPM ISO 4387

Carbon monoxide ISO 8454

Nicotine ISO 10315

Water (GC) ISO 10362-1

Statistical Analysis ISO 5725-2

Ventilation zone blocking, puffing parameters, and number of test pieces smoked

*Health Canada Method T-115 paragraph 16.1

*Note: T-115 has been removed from the Health Canada website and therefore is

embedded here.

Tar and Nicotine and

CO T-115e4.pdf

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5. Methods

5.1. General Guidance

As a general guide, experiments conducted under each puffing regime should be conducted

according to ISO standard requirements. Exceptions to this guiding principle include the

puffing parameters applied for intense smoking regime, the vent blocking applied, the

number of cigarettes smoked per sample and the butt length for smoking. The study (the

smoking results) and the daily use of the monitor are based on a fixed butt length of 33 mm.

Please note that any operating conditions (a) not specified in the above ISO standards, or

regarded as optional, (b) not specified in the intense method documents provided as

guidelines and (c) any circumstances that may have influenced test results should be noted in

the test report.

Puffing parameter and vent blocking specifications for each puffing regime are summarized

in Table 1. Note: Although the CORESTA Monitor Test Pieces are unventilated it is advised

to follow the Health Canada procedures exactly and tape the filter ventilation zone.

Table 1: Smoking Regime Specifications

Smoking Regime

Puff Volume (mL)

Puff Frequency*

(s)

Puff Duration

(s)

Vent Blocking

(%) Description

1 35 ± 0.3 60 ± 0.5 2 ± 0.02 0 ISO

2 55 ±0.5 30 ± 1.0 2 ± 0.02 100 Intense

5.2. Test Specimen(s)

CM8 test piece.

5.3. Sampling

The smoking plans will use 200 test pieces for each rotary smoking machine or 220 test

pieces for each linear smoking machine included in the study. A composite of all packs

should be prepared for conditioning according to ISO 8243:2006. If a substantial period of

time is expected to occur between the times when the test pieces are smoked with the

different smoking regimes, then two separate composite samples should be prepared, one for

each smoking regime.

5.4. Ventilation Zone Blocking for Intense Smoking

The blocking of the filter ventilation zone will be achieved by wrapping a single layer of

invisible tape, 19.0 mm wide or equivalent, around the complete circumference of the filter

and tipping paper of the test articles.

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5.5. Butt Marking

For the purpose of this study the CM8 test pieces will be butt marked to a fixed butt length of

33 mm.

5.6. Conditioning

The composite samples shall be conditioned for at least 48 hours but no more than 10 days

under the following conditions:

Temperature: 22 ± 1°C Relative humidity: 60 ± 3%

Temperature and relative humidity of the conditioning enclosure (chamber or room) shall be

checked and recorded for every smoking run.

Test cigarettes to be smoked for the determination of NFDPM, nicotine and CO should be

selected at random from the conditioned cigarettes.

Any test pieces with visible defects shall be discarded.

5.7. Test Piece Weight

The test articles will be weighed for ISO smoking only since the ventilation zone blocking

tape applied for intense smoking may vary between laboratories. The weight of the test piece

after conditioning is to be determined by weighing all test pieces to be smoked just before

they are placed at the smoking machine. The result is reported as the mean weight of the 20

test pieces for linear or rotary smoking machine at ISO puffing parameters.

5.8. Smoking Machine

Where smoking laboratories have more than one type of smoking machine (i.e. linear and

rotary variants) they are encouraged to include as many types in the study as possible.

5.9. Smoking Plans

The smoking plans will incorporate one product (CM8), shown as M in the smoking plans.

These plans are designed to smoke the CM8 in all ports for each puffing regime, spread over

a number of days. If possible, each participating laboratory should use only one operator (for

each smoking machine type) throughout the course of the study.

For ISO smoking, one test result is defined as the mean yield obtained from smoking 20 test

pieces in a single smoking machine run, therefore from a rotary machine it is the result from

one run smoking 20 test pieces and from a linear machine it is the average of four ports,

smoking five test pieces per port. This is repeated on five separate days resulting in 100 test

pieces being smoked (Tables 2-3).

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For Intense smoking, the number of test pieces smoked per filter pad is reduced to avoid

overloading the pad. As a consequence, the number of smoking runs/ports has to be

increased so that the same nominal numbers of test pieces are smoked. Thus, a test result

from a rotary machine is the mean of two runs, each of 10 test pieces, and from a linear

machine it is the average of eight ports, smoking three test pieces per port (Tables 4-5).

Note that the side seam of the test pieces should be positioned at random and not in a fixed

position since it has been observed that some laboratory staff habitually place cigarettes in a

particular orientation. Ports not occupied by the test pieces are left blank, which may be

assigned to any other cigarette that is to be smoked by the laboratory, or the ports may be left

empty.

Table 2: Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per pad)

Port Number

Day 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20

1 M M M M

2 M M M M

3 M M M M

4 M M M M

5 M M M M

Table 3: Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per pad)

Day Run Test Piece

1 1 M

2 2 M

3 3 M

4 4 M

5 5 M

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Table 4: Smoking Plan for 20-port Linear Machines for Intense smoking (3 test pieces per

pad)

Port Number

Day

Run

1 2 3 4 5 6 7 8 9 10

11

12

13

14

15

16

17

18

19

20

1 6 M M M M

7 M M M M

2 8 M M M M

9 M M M M

3 10 M M M M

11 M M M M

4 12 M M M M

13 M M M M

5 14 M M M M

15 M M M M

Table 5: Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces per

pad)

Day Run Test Piece

1 6 M

7 M

2 8 M

9 M

3 10 M

11 M

4 12 M

13 M

5 14 M

15 M

6. Target Variables and Data Reporting

The variables to be reported fall into two categories: those which will form the basis of the

statistical evaluation of the data and those that are ancillary to the test.

The variables to be reported for statistical analysis are:

• Mean weight of the Monitor after conditioning (just prior to smoking)

• Mean puff number per test piece

• Mean TPM per test piece

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• Mean nicotine delivery per test piece

• Mean water delivery per test piece

• Mean NFDPM delivery per test piece

• Mean CO delivery per test piece

The ancillary variables are:

• Date of testType of smoking machine used

• Temperature (C°) and relative humidity (RH%) of conditioning enclosure

• Temperature (C°) and relative humidity (RH%) of smoking environment

• Atmospheric pressure in the laboratory during smoking

• Ambient air flow in the smoking machine before smoking (mm/sec)

Dimensions and rounding of test results

Analytical variables:

Weight of Monitor mg per test piece ####.#

Puff number number ##.##

TPM mg per test piece ##.##

Nicotine mg per test piece #.###

Water mg per test piece ##.##

NFDPM mg per test piece ##.##

Carbon Monoxide mg per test piece ##.##

Ancillary variables:

Date of test DD/MM/YY

Conditioning temperature degrees Celsius ##.#

Conditioning humidity percent RH ##.#

Air velocity mm/s ###

Laboratory temperature degrees Celsius ##.#

Laboratory humidity percent RH ##.#

Laboratory

barometric

pressure

kPa ###.#

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Please note that the rounding of the data to the formats specified above must take place

after any calculations that may be involved. All calculations will use the laboratory data as

recorded using the maximum number of digits available.

All data arising from this study will be made available to the laboratories participating in the

study. The distribution of data will be done after collation and statistical evaluation.

To facilitate the statistical evaluation, all data must be reported using the attached

spreadsheets and must be submitted via e-mail. Please use the attached spreadsheets as

provided without changing the format.

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7. Study Time Table

The smoking should be performed during January and February, 2017. Strict adherence to

the timeline is very important for the data to be compiled for an initial assessment at the

next Sub-Group meeting on April, 2016. Data not received by March 1, 2017 will be

excluded from the formal statistical analysis. Please review your data carefully before

submitting as the statistical analysis is very labor intensive.

The statistical analysis of the results will follow as closely as possible the recommendations

of ISO 5725.

Should any questions arise please contact the study coordinator, Linda Crumpler. All results

must be sent via e-mail to:

Linda A. Crumpler linda.crumpler(at)cerulean.com

8. Data Submission

All results must be sent via e-mail to:

Linda A. Crumpler linda.crumpler(at)cerulean.com

9. Explanation of Minimum Statistics to be Applied for a Collaborative

Study

At a minimum Repeatability and Reproducibility estimation will be applied.

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Bibliography

• Chem. Pure Appl. QUALITY ASSURANCE SCHEMES THE INTERNATIONAL

HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF

ANALYTICAL CHEMISTRY LABORATORIES (n.d.): n. pag. Web.

• Council of Science Editors. 8th ed. N.p.: Council of Science Editors, n.d. Print.

• Form and Style for ASTM Standards. West Conshohocken, PA: ASTM

INTERNATIONAL, 2015. Print.

• Horwitz, William. "Protocol for the Design, Conduct and Interpretation of

Collaborative Studies." Pure and Applied Chemistry 60.6 (1988): 855-64. ShareGate.

International Union of Pure and Applied Chemistry, De Gruyter, Jan. 1988. Web. 30

July 2015.

• ISO 5725 Standard And Reference Laboratories Error.pdf. "ISO 5252." ISO 5725

Standard And Reference Laboratories Error (n.d.): n. pag. Web.

• "IUPAC 2006 IUPAC, Pure and Applied Chemistry 78, 145–196"" N.p., n.d. Web. 25

Aug. 2015.

• "Numbers, Units, Mathematicial Expressions, and Statistics." Scientific Style and

Format; The CSE Manual for Authors Editors, and Publishers. 8th ed. Chicago: The

University of Chicago, 2014. 157-91. Print.

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Appendix A – Système International (SI) Units and their Symbols

SI base units

Base Quantity Name Symbol

Length meter m

Mass kilogram Kg

Time second s

Electric current ampere A

Temperature kelvin K

Amount of substance mole mol

Luminous intensity Candela cd

SI derived units

Derived Quantity Name Symbol Equivalent SI Units

Frequency hertz Hz s-1

Force newton N m·kg·s-2

Pressure pascal Pa N/m2

Energy joule J N·m

Power watt W J/s

Electric charge coulomb C s·A

Electric potential volt V W/A

Electric resistance ohm Ω V/A

Celsius temperature Degrees Celsius °C K*

*Unit degree Celsius is equal in magnitude to unit kelvin

SI prefixes

Factor Name Symbol Numerical value

1012 tera T 1 000 000 000 000

109 giga G 1 000 000 000

106 mega M 1 000 000

103 kilo k 1 000

102 hecto h 100

101 deka da 10

10-1 deci d 0.1

10-2 centi c 0.01

10-3 milli m 0.001

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Factor Name Symbol Numerical value

10-4 micro µ 0.000 001

10-6 nano n 0.000 000 001

10-7 pico p 0.000 000 000 001

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APPENDIX C – Departures from Experimental Protocol

In determining the conditioned weight Lab 32 did not weigh all 20 test pieces as a single

group but rather as 4 groups of 5 test pieces.

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APPENDIX D – Raw Data Set

Table 1: Raw data for CM8 – ISO Smoking regime

Lab count

Machine Count

Lab Code

Machine Class

Machine Type

Run No.

Cond. Weight

(mg/t.p)

TPM (mg/t.p.)

Water

(mg/t.p)

Nicotine

(mg/t.p)

NFDPM

(mg/t.p)

CO

(mg/t.p)

Puff Count

1 1 1A R RM200A

1 975.0 17.06 1.94 1.660 13.46 13.33 7.58

2 965.4 16.43 1.78 1.606 13.04 12.54 7.58

3 960.4 16.56 1.79 1.610 13.16 12.99 7.47

4 967.5 16.21 1.75 1.562 12.90 12.69 7.47

5 964.8 16.38 1.76 1.612 13.01 12.91 7.59

1 2 1B L SM450

1 959.3 17.57 1.53 1.793 14.25 12.73 8.17

2 958.9 17.24 1.47 1.696 14.07 12.69 8.07

3 958.9 17.24 1.46 1.668 14.10 12.53 8.04

4 960.6 18.06 1.64 1.741 14.68 13.18 7.97

5 959.2 17.59 1.54 1.706 14.35 12.84 7.99

2 3 2A R RM200A

1 969.0 17.90 2.25 1.618 14.03 13.83 7.57

2 967.0 17.63 1.98 1.617 14.03 13.82 7.64

3 952.0 17.24 1.90 1.607 13.74 13.60 7.35

4 964.0 17.26 1.66 1.633 13.97 13.61 7.51

5 963.0 17.87 2.10 1.672 14.10 13.84 7.71

2 4 2B L SM450

1 954.0 17.67 1.58 1.582 14.50 13.86 8.18

2 959.0 17.79 1.49 1.632 14.67 13.93 8.09

3 966.0 17.63 1.34 1.647 14.64 13.57 8.02

4 955.0 17.77 1.49 1.672 14.61 13.89 7.98

5 961.0 17.70 1.74 1.644 14.31 13.95 8.14

3

5 4A R RM200A

1 955.0 17.57 1.97 1.650 13.95 13.60 7.50

2 965.0 17.34 2.00 1.635 13.71 13.35 7.60

3 960.0 17.71 2.16 1.681 13.87 13.43 7.50

4 969.9 17.49 1.98 1.653 13.88 13.45 7.50

5 962.0 17.55 2.00 1.662 13.89 13.65 7.60

6 4B R RM20D

1 954.0 17.41 2.19 1.570 13.64 13.6 7.30

2 973.0 18.84 2.60 1.711 14.53 13.09 7.60

3 966.0 17.72 2.33 1.621 13.76 13.41 7.50

4 965.0 18.64 2.55 1.688 14.39 13.71 7.60

5 958.0 18.00 2.18 1.603 14.21 13.19 7.50

4

7 5A R RM20A

1 964.5 16.94 1.94 1.584 13.42 14.00 7.63

2 960.0 17.26 2.19 1.622 13.45 13.70 7.59

3 965.5 17.44 2.19 1.640 13.62 13.80 8.05

4 961.0 17.01 2.07 1.621 13.32 13.40 7.8

5 958.5 16.98 2.11 1.632 13.24 13.70 8.1

8 5B R RM200A

1 965.4 17.32 2.17 1.558 13.59 13.63 7.31

2 965.0 16.81 2.02 1.585 13.20 13.09 7.28

3 966.5 17.00 1.92 1.589 13.49 13.36 7.4

4 965.0 16.97 2.17 1.558 13.24 13.59 7.53

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Lab count

Machine Count

Lab Code

Machine Class

Machine Type

Run No.

Cond. Weight

(mg/t.p)

TPM (mg/t.p.)

Water

(mg/t.p)

Nicotine

(mg/t.p)

NFDPM

(mg/t.p)

CO

(mg/t.p)

Puff Count

5 961.0 17.26 2.13 1.620 13.51 13.75 7.55

9 5C R RM200A

1 966.0 17.32 2.18 1.623 13.52 13.40 7.46

2 960.0 17.46 1.77 1.668 14.03 13.74 7.49

3 959.0 16.85 2.02 1.563 13.27 13.49 7.58

4 961.5 16.84 2.02 1.557 13.27 13.43 7.47

5 962.5 16.93 2.14 1.586 13.20 13.62 7.42

5

10 6A R RM200A

1 967.4 17.76 2.43 1.680 13.65 14.35 7.77

2 966.8 18.04 2.62 1.722 13.69 14.48 7.94

3 967.6 18.27 2.61 1.745 13.91 14.89 7.93

4 962.8 18.21 2.48 1.736 13.99 14.42 7.7

5 973.1 18.29 2.49 1.743 14.06 14.46 7.91

11 6B R RM200A

1 966.6 18.10 2.45 1.720 13.93 14.88 7.81

2 963.7 17.55 2.33 1.701 13.52 14.19 7.68

3 971.2 17.25 2.31 1.660 13.28 13.79 7.73

4 961.2 17.38 2.43 1.647 13.30 14.50 7.66

5 968.5 17.96 2.39 1.712 13.86 14.38 7.76

6 12 7 R RM20H

1 955.0 18.55 2.27 1.697 14.58 14.86 7.67

2 958.0 17.77 2.22 1.676 13.88 13.93 7.55

3 959.0 18.17 2.30 1.691 14.18 14.29 7.77

4 957.0 17.08 1.95 1.609 13.53 13.66 7.54

5 959.0 18.17 2.11 1.722 14.34 14.36 7.53

7 13 8 R RM20H

1 962.5 18.00 2.39 1.673 13.93 14.18 7.68

2 964.9 17.79 2.39 1.673 13.73 14.07 7.75

3 963.4 17.43 2.18 1.748 13.50 13.96 7.63

4 959.1 17.40 2.01 1.700 13.69 14.00 7.74

5 959.7 17.48 2.06 1.649 13.77 12.99 7.92

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RAC-134-CTR CM8 Coll. Study 2017 – November 2017 57/103

Lab count

Machine Count

Lab Code

Machine Class

Machine Type

Run No.

Cond. Weight

(mg/t.p)

TPM (mg/t.p.)

Water

(mg/t.p)

Nicotine

(mg/t.p)

NFDPM

(mg/t.p)

CO

(mg/t.p)

Puff Count

8

14 9A L SM450

1 957.5 16.61 1.41 1.567 13.63 12.39 7.53

2 970.5 17.60 1.58 1.696 14.32 12.86 7.95

3 953.0 17.88 1.65 1.641 14.58 12.76 7.68

4 968.0 17.60 1.60 1.612 14.39 12.75 7.85

5 957.5 17.36 1.62 1.600 14.14 12.36 7.65

15 9B R RM200A

1 965.0 16.99 1.93 1.535 13.53 13.02 7.33

2 959.5 17.27 2.20 1.624 13.45 13.02 7.42

3 964.0 16.83 2.12 1.600 13.12 12.54 7.42

4 - 16.44 1.91 1.511 13.02 12.45 7.33

5 964.5 16.75 2.04 1.528 13.18 12.61 7.52

9 16 10 L SM450

1 955.3 18.10 1.58 1.840 14.68 12.83 8.00

2 954.4 17.30 1.48 1.645 14.18 12.15 7.65

3 960.0 18.48 1.60 1.725 15.13 13.45 8.00

4 960.5 18.08 1.63 1.650 14.78 12.50 8.00

5 956.2 18.63 1.78 1.875 14.98 13.08 8.08

10 17 11 L SM450

1 964.1 18.42 1.60 1.765 15.05 12.00 8.38

2 960.0 17.61 1.66 1.683 14.26 12.40 7.83

3 953.9 17.96 1.71 1.735 14.52 12.69 7.88

4 956.8 16.80 1.26 1.668 13.87 11.70 7.95

5 954.6 17.97 1.70 1.740 14.53 12.62 8.00

11 18 12 R RM200A

1 956.0 17.78 2.60 1.711 13.47 13.44 7.47

2 962.0 18.11 2.56 1.738 13.81 13.40 7.63

3 956.0 17.25 2.55 1.715 12.99 12.90 7.53

4 953.0 17.65 2.31 1.747 13.59 13.40 7.53

5 965.0 17.13 2.46 1.685 12.99 12.72 7.57

12

19 13A R RM20H

1 962.5 16.44 2.20 1.502 12.74 12.91 7.15

2 955.0 16.50 2.02 1.494 12.98 13.44 7.48

3 956.0 15.93 1.86 1.490 12.58 12.47 7.05

4 956.0 16.27 2.08 1.494 12.70 13.07 7.35

5 955.0 16.90 2.18 1.541 13.18 13.27 7.35

20 13B R RM20H

1 952.8 16.12 2.14 1.474 12.51 12.95 7.17

2 952.8 16.39 1.88 1.375 13.14 12.90 7.03

3 952.1 16.15 2.05 1.518 12.58 12.49 7.11

4 953.6 16.17 1.98 1.510 12.68 12.92 7.13

5 958.6 16.60 2.07 1.544 12.99 13.11 7.35

13 21 14 R RM200A

1 964.1 17.40 1.90 1.620 13.88 13.30 7.51

2 969.8 17.60 2.00 1.660 13.94 13.50 7.71

3 966.8 17.70 2.10 1.650 13.95 13.50 7.68

4 963.6 17.80 2.00 1.670 14.13 13.50 7.67

5 962.8 17.40 1.80 1.650 13.95 13.50 7.63

14 22 15 R RM20D 1 954.0 17.64 1.99 1.650 14.00 13.78 7.57

2 962.5 17.75 2.50 1.615 13.64 13.74 7.76

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RAC-134-CTR CM8 Coll. Study 2017 – November 2017 58/103

Lab count

Machine Count

Lab Code

Machine Class

Machine Type

Run No.

Cond. Weight

(mg/t.p)

TPM (mg/t.p.)

Water

(mg/t.p)

Nicotine

(mg/t.p)

NFDPM

(mg/t.p)

CO

(mg/t.p)

Puff Count

3 961.5 18.02 2.43 1.650 13.94 14.07 7.75

4 962.0 18.29 2.60 1.653 14.04 14.54 7.78

5 966.0 18.27 2.61 1.677 13.98 14.63 7.88

15

23 16A L SM450

1 950.9 16.98 1.26 1.735 13.99 12.67 8.30

2 960.2 17.46 1.32 1.745 14.39 12.80 8.38

3 956.6 17.22 1.02 1.828 14.37 12.45 8.25

4 960.5 17.76 1.30 1.773 14.69 13.52 8.33

5 961.2 17.32 1.15 1.739 14.43 12.66 8.38

24 16B L SM450

1 960.2 17.48 1.30 1.826 14.36 12.54 8.58

2 960.9 17.85 1.19 1.797 14.86 12.79 8.83

3 958.6 17.19 1.17 1.842 14.18 12.68 8.53

4 963.4 17.59 1.04 1.776 14.77 12.93 8.55

5 952.1 17.71 1.15 1.778 14.78 12.95 8.40

25 16C L LX20

1 951.1 17.10 1.32 1.753 14.02 13.41 8.24

2 959.0 16.59 1.18 1.782 13.63 13.50 8.67

3 960.2 17.25 1.13 1.835 14.28 13.58 8.54

4 957.7 17.09 1.14 1.801 14.15 13.42 8.46

5 956.0 16.94 1.22 1.744 13.97 13.55 8.65

26 16D R RM20H

1 950.9 17.47 1.27 1.711 14.49 13.56 7.92

2 955.3 17.31 1.31 1.713 14.29 13.45 7.88

3 952.6 17.30 1.35 1.713 14.24 13.95 7.82

4 952.5 17.27 1.27 1.723 14.28 13.53 7.75

5 960.9 16.88 1.39 1.717 13.77 12.70 7.96

16 27 17 L SM450

1 961.7 17.15 1.33 1.638 14.18 12.90 7.95

2 964.4 16.18 1.10 1.605 13.48 12.45 7.70

3 958.5 16.53 1.25 1.600 13.68 12.28 7.85

4 953.8 16.18 1.25 1.555 13.38 12.53 7.78

5 949.5 16.20 1.28 1.583 13.34 11.55 7.85

Page 59: Routine Analytical Chemistry Sub-Group · RAC-134-CTR CM8 Coll. Study 2017 – November 2017 6/103 Table 5: WEIGHT mean and standard deviation per laboratory code Lab Code Machine

RAC-134-CTR CM8 Coll. Study 2017 – November 2017 59/103

Lab count

Machine Count

Lab Code

Machine Class

Machine Type

Run

No.

Cond. Weight

(mg/t.p)

TPM (mg/t.p.)

Water

(mg/t.p)

Nicotine

(mg/t.p)

NFDPM

(mg/t.p)

CO

(mg/t.p)

Puff Count

17 28 18 L SM450

1 953.0 18.33 1.70 1.723 14.91 14.25 7.73

2 957.0 18.48 1.69 1.728 15.06 15.35 7.88

3 956.0 18.55 1.73 1.745 15.08 13.80 7.90

4 960.0 18.10 1.40 1.670 15.03 15.53 7.80

5 950.0 19.55 1.83 1.725 15.99 13.58 8.05

18 29 19 L SM450

1 955.1 18.70 1.94 1.785 14.97 14.07 8.03

2 949.9 18.03 1.55 1.770 14.71 13.85 7.70

3 947.1 18.05 1.61 1.733 14.71 13.69 7.90

4 953.2 17.75 1.55 1.723 14.48 13.86 8.03

5 943.6 18.16 1.76 1.753 14.65 14.14 7.93

19 30 20 L SM450

1 934.2 18.83 0.94 1.879 16.01 13.35 7.76

2 949.9 17.34 1.16 1.662 14.52 12.56 7.25

3 953.0 16.47 1.04 1.556 13.88 11.62 7.26

4 948.6 20.08 1.78 1.765 16.54 14.28 7.49

5 949.0 17.10 1.00 1.637 14.46 12.54 7.36

20 31 21 L SM450

1 963.5 17.86 1.32 1.682 14.85 13.16 8.08

2 960.5 18.80 1.28 1.731 15.79 13.81 7.98

3 963.7 18.03 1.33 1.718 14.98 13.27 8.03

4 960.7 17.88 1.32 1.645 14.92 13.47 7.85

5 960.4 17.65 1.33 1.716 14.61 13.23 7.83

21

32 22A R RM20H

1 959.0 17.07 2.05 1.570 13.45 13.23 7.66

2 962.0 17.55 2.27 1.610 13.67 13.87 7.81

3 960.0 17.37 2.07 1.630 13.67 13.49 7.54

4 960.0 17.25 2.02 1.610 13.62 13.12 7.64

5 960.0 17.26 2.12 1.610 13.53 13.62 7.52

33 22B R RM200A

1 963.0 17.33 2.16 1.630 13.54 13.67 7.40

2 962.0 16.99 2.11 1.570 13.31 13.75 7.40

3 959.0 17.27 2.05 1.630 13.59 13.67 7.40

4 961.0 17.40 2.02 1.610 13.77 13.70 7.40

5 960.0 17.52 2.08 1.630 13.81 13.58 7.54

22 34 24 L SM450

1 949.0 15.78 1.34 1.506 12.93 11.34 7.08

2 955.3 15.99 1.38 1.491 13.12 11.80 7.37

3 952.2 16.49 1.43 1.556 13.51 12.15 7.36

4 953.1 16.56 1.42 1.529 13.61 11.34 7.43

5 957.2 17.48 1.56 1.625 14.30 12.42 7.75

23 35 25 L SM450

1 964.2 16.96 1.25 1.714 13.99 12.56 8.13

2 963.2 18.63 1.52 1.781 15.33 12.61 8.20

3 959.8 16.47 1.22 1.688 13.57 12.24 7.75

4 971.3 17.28 1.23 1.696 14.35 12.81 8.05

5 970.8 17.06 1.28 1.661 14.13 13.21 7.80

24 36 26 R RM200A 1 975.6 18.00 2.39 1.645 13.97 13.11 8.12

2 960.5 17.76 2.40 1.625 13.74 13.50 7.90

Page 60: Routine Analytical Chemistry Sub-Group · RAC-134-CTR CM8 Coll. Study 2017 – November 2017 6/103 Table 5: WEIGHT mean and standard deviation per laboratory code Lab Code Machine

RAC-134-CTR CM8 Coll. Study 2017 – November 2017 60/103

Lab count

Machine Count

Lab Code

Machine Class

Machine Type

Run

No.

Cond. Weight

(mg/t.p)

TPM (mg/t.p.)

Water

(mg/t.p)

Nicotine

(mg/t.p)

NFDPM

(mg/t.p)

CO

(mg/t.p)

Puff Count

3 966.1 18.12 2.35 1.664 14.10 13.96 7.90

4 965.9 17.70 2.21 1.619 13.87 13.15 7.98

5 973.3 18.27 2.33 1.681 14.26 13.37 8.20

25 37 27 L LX20

1 962.7 16.78 1.25 1.683 13.85 12.59 7.83

2 963.5 17.07 1.55 1.700 13.82 12.77 7.90

3 962.3 16.46 1.27 1.705 13.49 11.97 7.72

4 960.4 16.42 1.21 1.675 13.54 13.12 7.67

5 961.2 16.52 1.22 1.701 13.60 13.98 7.86

26 38 28 L SM450

1 975.0 17.94 1.76 1.655 14.52 13.43 8.26

2 962.0 17.48 1.70 1.723 14.06 12.62 8.10

3 958.0 17.00 1.57 1.645 13.78 12.90 7.97

4 961.0 17.21 1.48 1.713 14.02 12.21 8.21

5 964.0 17.48 1.69 1.688 14.11 12.44 8.13

27 39 29 L SM450

1 951.4 17.44 1.62 1.863 13.88 12.02 7.60

2 962.9 17.44 1.66 1.877 14.20 12.50 7.43

3 956.3 17.21 1.38 1.823 13.77 12.09 7.43

4 957.7 17.48 1.37 1.857 15.20 11.90 7.43

5 963.0 17.02 1.68 1.820 13.41 11.70 7.43

28 40 30 R RM200A

1 955.6 16.89 1.96 1.666 13.26 13.25 7.42

2 953.2 16.78 1.68 1.654 13.45 12.98 7.56

3 956.9 16.90 1.85 1.652 13.40 13.12 7.45

4 957.8 16.85 1.75 1.667 13.43 12.99 7.52

5 960.2 17.00 2.03 1.652 13.32 13.25 7.51

29 41 31 R RM20

1 952.2 17.98 2.16 1.860 13.96 13.50 7.58

2 958.3 18.07 1.85 1.900 14.32 13.50 7.75

3 963.8 17.80 1.85 1.860 14.09 13.30 7.72

4 946.3 17.78 2.37 1.830 13.58 14.00 7.48

5 958.6 17.52 1.91 1.820 13.79 13.50 7.72

Page 61: Routine Analytical Chemistry Sub-Group · RAC-134-CTR CM8 Coll. Study 2017 – November 2017 6/103 Table 5: WEIGHT mean and standard deviation per laboratory code Lab Code Machine

RAC-134-CTR CM8 Coll. Study 2017 – November 2017 61/103

Lab count

Machine Count

Lab Code

Machine Class

Machine Type

Run

No.

Cond. Weight

(mg/t.p)

TPM (mg/t.p.)

Water

(mg/t.p)

Nicotine

(mg/t.p)

NFDPM

(mg/t.p)

CO

(mg/t.p)

Puff Count

30 42 32 L SM450

1 968.3 16.75 1.53 1.804 13.41 11.52 8.85

2 971.2 15.10 1.60 1.808 11.69 11.98 8.50

3 975.0 15.80 1.62 1.846 12.33 12.74 8.85

4 981.0 15.57 1.73 1.800 9.02 12.19 8.55

5 929.5 16.60 2.26 1.855 12.48 11.85 8.75

31 43 33 L LM20X

1 955.4 18.56 1.61 1.796 15.15 13.34 8.17

2 955.6 17.45 1.46 1.722 14.27 13.52 7.92

3 958.7 18.24 1.75 1.779 14.71 13.39 7.99

4 957.0 17.97 1.74 1.747 14.48 13.74 8.08

5 954.9 18.51 1.67 1.772 15.07 13.86 8.07

32 44 34 L SM450

1 947.1 16.76 1.85 1.591 13.33 11.99 8.00

2 954.8 17.20 2.16 1.582 13.47 12.49 7.98

3 961.9 16.98 1.57 1.552 13.86 12.88 7.98

4 955.9 17.00 1.63 1.589 13.78 13.36 8.00

5 948.9 17.56 1.72 1.595 14.24 13.24 7.95

33 45 35 R RM20M

1 957.8 16.98 2.09 1.673 13.22 12.94 7.75

2 957.6 16.68 2.08 1.621 12.98 13.25 7.68

3 966.5 16.63 2.04 1.638 12.96 13.18 7.62

4 963.8 16.36 1.77 1.682 12.90 12.63 7.64

5 961.8 16.70 1.94 1.633 13.13 13.01 7.46

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RAC-134-CTR CM8 Coll. Study 2017 – November 2017 62/103

Table 2: Raw data for CM8 – Intense Smoking regime

Lab count

Machine Count

Lab Code

Machine Class

Machine Type

Run

No.

TPM (mg/t.p.)

Water

(mg/t.p)

Nicotine

(mg/t.p)

NFDPM

(mg/t.p)

CO

(mg/t.p)

Puff Count

1 1 1A R RM200A

1 38.68 8.62 3.202 26.85 24.54 10.65

2 38.21 8.54 3.218 26.45 23.66 10.65

3 38.60 8.66 3.245 26.70 23.97 10.89

4 38.84 8.75 3.200 26.89 24.57 10.71

5 38.42 8.50 3.229 26.69 24.34 11.11

2 1B L SM450 1 45.53 12.47 3.580 29.49 24.48 11.38

2 45.16 12.11 3.470 29.58 24.31 11.46

3 44.68 12.04 3.370 29.26 24.67 11.18

4 45.41 12.38 3.450 29.59 24.61 11.27

5 44.67 12.14 3.460 29.07 23.86 11.44

2 3 2A R RM200A

1 42.02 9.19 3.320 29.50 26.23 10.99

2 41.67 8.95 3.285 29.43 26.22 10.89

3 40.73 8.37 3.307 29.04 25.81 10.77

4 41.24 8.71 3.361 29.16 25.33 11.07

5 40.41 8.48 3.308 28.62 25.50 10.90

4 2B L SM450 1 45.97 10.93 3.340 31.70 25.81 11.48

2 45.08 10.30 3.370 31.41 26.39 11.44

3 45.12 10.45 3.430 31.23 25.50 11.46

4 45.76 10.96 3.430 31.37 26.28 11.52

5 44.03 10.60 3.350 30.08 25.37 11.63

3 5 4A R RM200A

1 42.46 9.27 3.520 29.68 25.38 10.85

2 42.38 9.41 3.516 29.46 25.56 10.80

3 42.06 9.56 3.477 29.03 25.17 10.90

4 42.11 9.38 3.442 29.30 25.35 10.70

5 42.68 9.01 3.482 30.18 25.50 10.85

6 4B R RM20D 1 41.98 9.63 3.300 29.05 24.85 10.55

2 42.27 9.57 3.293 29.42 25.17 10.70

3 41.57 9.54 3.280 28.76 24.27 10.85

4 41.47 9.59 3.177 28.71 25.00 10.70

5 43.33 10.04 3.337 29.96 25.19 10.70

4 7 6A R RM200A

1 41.91 9.31 3.426 29.17 25.67 10.71

2 43.28 9.92 3.437 29.92 25.65 10.78

3 42.77 9.70 3.478 29.59 26.39 10.94

4 42.86 9.76 3.448 29.65 26.86 10.94

5 42.52 9.69 3.380 29.45 26.53 10.86

8 6B R RM200A

1 42.04 9.18 3.407 29.45 25.84 11.22

2 42.40 9.45 3.509 29.44 26.02 10.97

3 42.59 9.52 3.500 29.57 26.21 11.02

4 42.09 9.74 3.406 28.95 26.34 11.07

5 41.59 9.18 3.392 29.02 26.09 11.05

5 9 7 R RM20H 1 40.61 9.04 3.106 28.46 24.95 10.91

Page 63: Routine Analytical Chemistry Sub-Group · RAC-134-CTR CM8 Coll. Study 2017 – November 2017 6/103 Table 5: WEIGHT mean and standard deviation per laboratory code Lab Code Machine

RAC-134-CTR CM8 Coll. Study 2017 – November 2017 63/103

Lab count

Machine Count

Lab Code

Machine Class

Machine Type

Run

No.

TPM (mg/t.p.)

Water

(mg/t.p)

Nicotine

(mg/t.p)

NFDPM

(mg/t.p)

CO

(mg/t.p)

Puff Count

2 42.08 9.42 3.282 29.37 25.72 11.01

3 41.42 9.42 3.215 28.79 25.53 10.99

4 41.72 9.14 3.417 29.16 26.05 11.18

5 42.10 9.12 3.308 29.67 26.24 11.08

6 10 8 R RM20H 1 41.59 9.62 3.337 28.64 25.72 10.86

2 41.03 9.06 3.500 28.47 25.73 11.01

3 41.05 9.51 3.420 28.12 25.80 10.84

4 41.38 9.77 3.555 28.06 25.84 10.95

5 41.72 10.10 3.594 28.03 25.84 11.21

7 11 10 L SM450 1 47.93 11.84 3.750 32.34 23.70 11.28

2 44.18 9.64 3.300 31.25 23.64 10.99

3 47.10 10.65 3.550 32.90 23.93 11.19

4 46.75 10.86 3.220 32.65 24.08 11.10

5 45.58 10.84 3.860 30.91 22.20 11.58

8 12 11 L SM450 1 45.44 11.15 3.430 30.87 23.06 11.34

2 46.07 11.84 3.500 30.74 23.66 10.84

3 46.23 11.48 3.510 31.25 23.50 11.19

4 44.66 11.09 3.550 30.04 23.48 11.03

5 46.83 12.32 3.620 30.89 23.51 11.31

9 13 12 R RM200A

1 41.07 10.25 3.461 27.35 25.06 11.18

2 41.82 9.87 3.422 28.53 25.19 11.26

3 41.60 10.78 3.436 27.39 25.30 10.78

4 41.14 9.89 3.498 27.75 24.68 10.85

5 40.65 9.41 3.442 27.79 25.08 11.04

10 14 16A L SM450 1 45.73 10.05 3.550 32.13 24.01 12.16

2 44.33 9.54 3.500 31.29 25.02 11.71

3 42.49 9.01 3.430 30.06 23.41 11.78

4 44.14 9.65 3.610 30.88 24.16 11.70

5 43.90 9.14 3.480 31.28 24.29 11.60

10 15 16B L SM450 1 44.57 10.54 3.520 30.51 23.72 12.25

2 45.42 10.78 3.570 31.07 24.25 12.04

3 44.85 9.72 3.480 31.64 23.83 11.99

4 44.15 10.09 3.610 30.45 23.85 12.08

5 44.87 10.56 3.610 30.70 23.40 12.46

16 16C L LX20 1 41.31 9.01 3.430 28.86 24.61 12.08

2 42.63 9.57 3.530 29.53 25.36 11.97

3 41.20 8.85 3.420 28.93 24.31 11.49

4 41.93 9.43 3.600 28.89 24.98 12.12

5 40.86 9.06 3.450 28.35 24.55 11.85

17 16D R RM20H 1 39.95 7.79 3.258 28.91 24.82 11.41

2 40.00 7.56 3.363 29.08 24.48 11.45

3 40.30 7.87 3.290 29.14 25.33 11.33

Page 64: Routine Analytical Chemistry Sub-Group · RAC-134-CTR CM8 Coll. Study 2017 – November 2017 6/103 Table 5: WEIGHT mean and standard deviation per laboratory code Lab Code Machine

RAC-134-CTR CM8 Coll. Study 2017 – November 2017 64/103

Lab count

Machine Count

Lab Code

Machine Class

Machine Type

Run

No.

TPM (mg/t.p.)

Water

(mg/t.p)

Nicotine

(mg/t.p)

NFDPM

(mg/t.p)

CO

(mg/t.p)

Puff Count

4 39.73 7.96 3.475 28.30 24.77 11.12

5 39.60 7.76 3.346 28.49 24.29 11.38

11 18 17 L SM450 1 42.98 10.02 3.116 29.84 23.50 11.38

2 42.58 10.67 3.380 28.52 22.73 11.36

3 44.85 11.42 3.391 30.04 24.00 11.38

4 42.53 10.32 3.458 28.75 22.87 11.63

5 45.79 10.66 3.450 31.68 24.08 11.26

12 19 18 L SM450 1 47.10 12.12 3.410 31.59 26.04 11.14

2 48.58 13.37 3.440 31.79 26.14 11.19

3 47.68 13.07 3.440 31.18 25.24 11.03

4 48.45 14.08 3.460 30.90 26.14 11.20

5 48.24 13.33 3.370 31.54 24.94 11.11

13 20 19 L SM450 1 47.55 12.88 3.520 31.15 25.96 10.66

2 47.88 12.62 3.490 31.77 26.36 10.90

3 48.97 13.42 3.510 32.04 26.12 10.80

4 47.98 13.28 3.500 31.20 26.06 10.93

5 48.40 12.88 3.480 32.03 25.99 10.79

14 21 20 L SM450 1 46.05 10.74 3.390 31.92 24.40 10.56

2 46.66 12.00 3.470 31.19 25.24 10.63

3 46.84 12.38 3.520 30.95 23.50 10.35

4 46.56 10.84 3.460 32.26 25.51 10.72

5 46.57 11.35 3.540 31.68 23.65 10.35

15 22 21 L SM450 1 49.16 12.21 3.580 33.38 25.40 11.28

2 50.36 13.18 3.580 33.60 25.63 11.45

3 51.05 13.88 3.590 33.58 25.69 11.33

4 50.83 13.79 3.540 33.50 25.90 11.41

5 51.21 13.60 3.540 34.06 25.64 11.13

16 23 22A R RM20H 1 39.56 9.10 3.155 27.31 24.88 10.99

2 40.67 9.61 3.275 27.78 25.31 10.82

3 39.81 9.16 3.210 27.44 24.62 11.05

4 40.12 9.28 3.195 27.65 24.60 10.93

5 40.68 9.64 3.245 27.79 24.60 11.09

24 22B R RM200A

1 40.24 9.69 3.185 27.37 25.14 10.54

2 39.93 9.18 3.250 27.51 25.16 10.21

3 41.54 10.01 3.275 28.26 25.60 10.36

4 41.01 10.41 3.215 27.39 25.16 10.31

5 40.20 9.81 3.145 27.24 25.03 10.54

17 25 24 L Hawktech

1 42.93 10.59 3.240 29.09 23.91 10.81

2 41.36 9.71 3.170 28.49 22.99 10.50

3 43.74 10.88 3.270 29.59 22.89 10.93

4 42.85 10.50 3.230 29.13 23.75 10.49

5 45.14 11.21 3.370 30.56 24.83 11.03

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Lab count

Machine Count

Lab Code

Machine Class

Machine Type

Run

No.

TPM (mg/t.p.)

Water

(mg/t.p)

Nicotine

(mg/t.p)

NFDPM

(mg/t.p)

CO

(mg/t.p)

Puff Count

18 26 25 L SM450 1 44.13 9.60 3.330 31.21 24.50 11.39

2 44.28 9.19 3.240 31.96 23.96 11.38

3 44.46 9.10 3.280 32.06 23.84 11.78

4 46.23 11.09 3.270 31.86 24.38 11.46

5 44.26 9.36 3.290 31.60 23.93 11.36

19 27 26 R RM200A

1 41.18 9.32 3.136 28.71 25.25 11.37

2 40.56 9.57 3.197 27.80 24.48 11.33

3 40.50 9.10 3.164 28.23 24.83 11.05

4 40.01 9.13 3.114 27.76 24.24 11.16

5 39.69 8.75 3.128 27.81 24.66 11.34

20 28 27 L LX20 1 43.74 10.91 3.330 29.50 28.07 10.76

2 45.32 12.03 3.420 29.87 28.51 11.01

3 43.46 11.08 3.460 28.92 27.76 11.07

4 45.09 11.80 3.380 29.90 25.82 11.20

5 43.91 11.00 3.380 29.52 25.86 11.16

21 29 29 L SM450

1 44.84 11.61 3.560 29.68 23.32 10.64

2 44.42 11.27 3.600 29.69 23.15 10.89

3 44.10 11.56 3.580 29.33 22.88 10.53

4 46.30 12.45 3.620 30.22 23.55 10.91

5 44.60 11.68 3.540 29.39 22.51 10.71

22 30 30 R RM200

A

1 40.43 9.33 3.627 27.47 25.51 10.39

2 40.31 9.13 3.623 27.56 24.83 10.51

3 41.03 9.40 3.643 27.99 25.11 10.39

4 40.90 9.36 3.671 27.87 25.04 10.50

5 40.86 9.60 3.594 27.67 25.46 10.41

23 31 31 R RM20

1 41.22 8.59 3.730 28.90 26.30 11.25

2 40.72 7.70 3.760 29.27 25.55 11.16

3 41.24 8.10 3.740 29.40 26.30 11.10

4 40.95 8.03 3.715 29.21 25.90 11.27

5 40.18 7.22 3.720 29.24 25.05 11.34

24 32 33 L LM20X

1 43.33 9.85 3.500 29.98 24.66 11.41

2 44.96 10.63 3.470 30.87 24.99 11.41

3 45.42 11.19 3.520 30.71 24.27 11.04

4 46.54 11.81 3.600 31.13 25.01 11.40

5 44.04 9.85 3.490 30.70 24.66 11.36

25 33 34 L SM450

1 44.65 12.08 3.520 29.04 24.55 11.51

2 43.65 11.58 3.460 28.61 24.68 11.61

3 46.16 12.70 3.520 29.94 25.55 11.45

4 44.88 12.17 3.420 29.28 24.77 11.36

5 44.26 12.58 3.390 28.30 25.14 11.38

26 34 35 R RM20M 1 42.26 9.60 3.444 29.21 24.61 10.91

2 41.14 8.86 3.521 28.76 24.67 11.11

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Lab count

Machine Count

Lab Code

Machine Class

Machine Type

Run

No.

TPM (mg/t.p.)

Water

(mg/t.p)

Nicotine

(mg/t.p)

NFDPM

(mg/t.p)

CO

(mg/t.p)

Puff Count

3 43.26 10.36 3.668 29.23 24.87 11.15

4 42.03 10.29 3.607 28.14 24.61 11.39

5 41.75 10.45 3.551 27.75 25.55 11.04

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APPENDIX E – IUPAC 1994 Harmonized Statistical Procedure

IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE

SCREEN OUT NON

VALID DATA

START OF LOOP

CALCULATE PRECISION

MEASURES

(C)

COCHRAN

OUTLYING LAB?

(G)

SINGLE

GRUBBS

OUTLIER?

(G2)

PAIRED

GRUBBS

OUTLIER?

END REPORT

ORIGINAL & LAST

COMPUTED

PRECISION

MEASURES

DROP LAB UNLESS OVERALL

FRACTION OF LABS DROPPED

WOULD EXCEED 2/9

DROP INDIVIDUAL VALUE

DROP LAB UNLESS OVERALL

FRACTION OF LABS DROPPED

WOULD EXCEED 2/9

ANY LABS

DROPPED IN

THIS LOOP

YES

YES

YES

YES

NO

NO

NO

NO

(Gi)SINGLE GRUBBS

OUTLIER ON INDIVIDUAL VALUES

OF COCHRAN OUTLYING

LAB?

YES

DROP LAB UNLESS OVERALL

FRACTION OF LABS DROPPED

WOULD EXCEED 2/9

NO

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APPENDIX F – Linear – Rotary Comparisons

Figure 1: CM8 under ISO smoking regime – r and R values (conditioned weight)

Figure 2: CM8 under ISO smoking regime – r and R values (TPM)

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Figure 3: CM8 under ISO smoking regime – r and R values (Water)

Figure 4: CM8 under ISO smoking regime – r and R values (Nicotine)

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Figure 5: CM8 under ISO smoking regime – r and R values (NFDPM)

Figure 6: CM8 under ISO smoking regime – r and R values (CO)

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Figure 7: CM8 under intense smoking regime – r and R values (TPM)

Figure 8: CM8 under intense smoking regime – r and R values (Water)

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Figure 9: CM8 under intense smoking regime – r and R values (Nicotine)

Figure 10: CM8 under intense smoking regime – r and R values (NFDPM)

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Figure 11: CM8 under intense smoking regime – r and R values (CO)

Figure 12: CM8 under intense smoking regime – r and R values (Puff count)

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APPENDIX G – Rotary Smoking Machines

1. ISO smoking regime

Figure 1: CM8 Individual observations of mainstream “ISO” TPM

Straggler value in orange

Figure 2: CM8 Individual observations of mainstream “ISO” WATER

Straggler value in orange

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Figure 3: CM8 Individual observations of mainstream “ISO” Nicotine

Straggler value in orange

Figure 4: CM8 Individual observations of mainstream “ISO” NFDPM

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Figure 5: CM8 Individual observations of mainstream “ISO” CO

Figure 6: CM8 Individual observations of mainstream “ISO” PUFF Count

Straggler value in orange

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2. Intense smoking regime

Figure 8: CM8 Individual observations of mainstream “Intense” TPM

Figure 9: CM8 Individual observations of mainstream “Intense” WATER

Straggler value in orange

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Figure 10: CM8 Individual observations of mainstream “Intense” Nicotine

Straggler value in orange

Figure 11: CM8 Individual observations of mainstream “Intense” NFDPM

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Figure 12: CM8 Individual observations of mainstream “Intense” CO

Figure 13: CM8 Individual observations of mainstream “Intense” PUFF Count

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APPENDIX H – Linear Smoking Machines

1. ISO Smoking regime

Figure 1: CM8 Individual observations of mainstream “ISO” TPM

Outlier value in red

Figure 2: CM8 Individual observations of mainstream “ISO” WATER

Outlier value in red, straggler value in orange

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Figure 3: CM8 Individual observations of mainstream “ISO” Nicotine

Outlier values in red

Figure 4: CM8 Individual observations of mainstream “ISO” NFDPM

Outlier values in red

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Figure 5: CM8 Individual observations of mainstream “ISO” CO

Figure 6: CM8 Individual observations of mainstream “ISO” PUFF Count

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2. Intense smoking regime

Figure 8: CM8 Individual observations of mainstream “Intense” TPM

Figure 9: CM8 Individual observations of mainstream “Intense” WATER

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Figure 10: CM8 Individual observations of mainstream “Intense” Nicotine

Outlier values in red

Figure 11: CM8 Individual observations of mainstream “Intense” NFDPM

Outlier value in red

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Figure 12: CM8 Individual observations of mainstream “Intense” CO

Outlier value in red

Figure 13: CM8 Individual observations of mainstream “Intense” PUFF Count

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APPENDIX I – Equipment Survey

Lab Code

Smoking Machine Model Manufacturer

Gas Chromatograph Model/Manufacturer/Column/ Internal Standards

Airflow Meter Model/Manufacturer

NDIR analyser Model/Manufacturer

1A RM200A / Borgwaldt KC Agilent 7890A

Nic Column: Length: 25m i.d.: 0.32mm Film Thickness: 0.3µm Stationary Phase: HP-20M Carbowax

Nicotine I.S. n-Octadecane

Anemometer Type g.440.3s-113/ Schiltknecht

CO-Measuring Unit Model No.70700050/ Borgwaldt KC

Water Column: Length 15m i.d.: 0.32µm Film thickness: 20µm Stationary Phase: HP-PLOT/Q

Water I.S. Ethanol

1B SM450 / Cerulean Agilent 7890A

Nic Column: Length: 25m i.d.: 0.32mm Film Thickness: 0.3µm Stationary Phase: HP-20M Carbowax

Nicotine I.S. n-Octadecane

Anemometer Type g.440.3s-113/ Schiltknecht

COA205/Cerulean

Water Column: Length 15m i.d.: 0.32µm Film thickness: 20µm Stationary Phase: HP-PLOT/Q

Water I.S. Ethanol

4A RM200A / Borgwaldt KC Agilent 6890

Nic Column:

Length: 5m

i.d.: 0.20

Film Thickness: 0.40µm

Stationary Phase: DB-WAXetr,

high polarity polyethylene glycol

Nicotine I.S.n-Heptadecane

Anemometer Schiltknecht CO-Analyser Borgwaldt KC

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Lab Code

Smoking Machine Model Manufacturer

Gas Chromatograph Model/Manufacturer/Column/ Internal Standards

Airflow Meter Model/Manufacturer

NDIR analyser Model/Manufacturer

(PEG)

Water Column: Length: 6' x 1/8" O.D. Stainless Steel Packed i.d.: 2mm Stationary Phase: Porapak Q, cross-linked

Water I.S. Ethanol

4B RM20D / Borgwaldt KC Agilent 6890

Nic Column: Length: 5m i.d.: 0.20 Film Thickness: 0.40µm Stationary Phase: DB-WAXetr, high polarity polyethylene glycol (PEG)

Nicotine I.S. n-Heptadecane

Anemometer Schiltknecht CO-Analyser Borgwaldt KC

Water Column: Length: 1/8"O.D Stainless Steel Packed i.d.: 2mm Stationary Phase: Porapak Q, cross-linked

Water I.S. Ethanol

5A RM20 / Borgwaldt KC Agilent 7890

B

Nic Column: Length: 5m i.d.: 0.20 Film Thickness: 0.40µm Stationary Phase: DB-WAXetr, high polarity polyethylene glycol (PEG)

Nicotine I.S. n-Heptadecane

Anemometer Type g: 440.3s-113 Schiltknecht

CO-Analyser Borgwaldt KC

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Lab Code

Smoking Machine Model Manufacturer

Gas Chromatograph Model/Manufacturer/Column/ Internal Standards

Airflow Meter Model/Manufacturer

NDIR analyser Model/Manufacturer

Water Column: Length: 6' x 1/8"O.D Stainless Steel Packed i.d.: 2mm Stationary Phase: J&W Porapak QS 80-100 mesh

Water I.S. Ethanol

5B RM200A / Borgwaldt KC Agilent 7890B

Nic Column: Length: 5m i.d.: 0.20 Film Thickness: 0.40µm Stationary Phase: DB-WAXetr, high polarity polyethylene glycol (PEG)

Nicotine I.S. n-Heptadecane

Anemometer Type g: 440.3s-113 Schiltknecht

CO-Analyser Borgwaldt KC

Water Column: Length: 6' x 1/8"O.D. Stainless Steel Packed i.d.: 2mm Stationary Phase: J&W Porapak QS 80-100 mesh

Water I.S. Ethanol

6A RM200A2 / Borgwaldt KC 7890 B/ Agilent

Nic Column: INNO Steel, Packed Length: 1.8m i.d.: 2.0mm Stationary Phase: 7.5% Carbowax / 2% KOH, 80/100 Chromosorb-WAW

Nicotine I.S. n-Heptadecane

Schiltknecht CO Module / Borgwaldt KC

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Lab Code

Smoking Machine Model Manufacturer

Gas Chromatograph Model/Manufacturer/Column/ Internal Standards

Airflow Meter Model/Manufacturer

NDIR analyser Model/Manufacturer

Water Column: INNO Steel packed column Length: 3.60m i.d.: 2.0mm Stationary Phase: 60/80 Hayesep-Q, porous polymer

Water I.S. Methanol

6B RM200A2 / Borgwaldt KC 7890 B/ Agilent

Nic Column: INNO Steel, Packed Length: 1.8m i.d.: 2.0mm Stationary Phase: 7.5% Carbowax / 2% KOH, 80/100 Chromosorb-WAW

Nicotine I.S. n-Heptadecane

Schiltknecht CO Module / Borgwaldt KC Water Column: INNO Steel packed column Length: 3.60m i.d.: 2.0mm Stationary Phase: 60/80 Hayesep-Q, porous polymer

Water I.S. Methanol

7 RM20H / Borgwaldt KC 7890 / Agilent

Nic Column: Length: 15m i.d.: 0.32mm Film Thickness: 0.25µm Stationary Phase: DB-WAX

Nicotine I.S. n-Heptadecane

ThermoAir3 / Schiltknecht Integrated CO module /

Borgwaldt KC Water Column: Length: 7.5 m i.d.: 0.53mm Film Thickness: 20µm Stationary Phase: PORAPlot U

Water I.S. Methanol

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Lab Code

Smoking Machine Model Manufacturer

Gas Chromatograph Model/Manufacturer/Column/ Internal Standards

Airflow Meter Model/Manufacturer

NDIR analyser Model/Manufacturer

8 RM20H / Borgwaldt KC Agilent 6890N

Nic Column: Length: 8ft. i.d.: 2mm Film Thickness: 1/8in. Stationary Phase: 10% Carbowax 2M 2% KOH SW-20M 2% KOH Chr-WAW 80-100 mesh

Nicotine I.S. n-Heptadecane

Schiltknecht CO/CO2 analyser C24/Borgwaldt KC

Water Column: Length: 6'x 1/8"O.D Stainless Steel Packed i.d.: 2.1 mm Film thickness: Stationary Phase: PORAPAK Q 80/100 mesh

Water I.S. Ethanol

9A SM450RH / Cerulean Agilent 6890N

Nic Column: Capillary, Agilent CP7424 Length: 25m i.d.: 0.53 Film Thickness: 2.00µm Stationary Phase:CP-Wax

Nicotine I.S. n-Heptadecane

ThermoAir3 / Schiltknecht Cerulean COA200 Water Column: Capillary, Agilent CP7554 Length: 25m i.d.: Film Thickness: Stationary Phase: PoraPLOT Q

Water I.S. Ethanol

9B RM200A / Borgwaldt KC Agilent 6890N

Nic Column: Capillary, Agilent CP7424 Length: 25m i.d.: 0.53 Film Thickness: 2.00µm Stationary Phase:CP-Wax

Nicotine I.S. n-Heptadecane

RM200A / Schiltknecht Integrated NDIR analyser

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Lab Code

Smoking Machine Model Manufacturer

Gas Chromatograph Model/Manufacturer/Column/ Internal Standards

Airflow Meter Model/Manufacturer

NDIR analyser Model/Manufacturer

Water Column: Capillary, Agilent CP7554 Length: 25m i.d.: Film Thickness: Stationary Phase: PoraPLOT Q

Water I.S. Ethanol

10 SM450 / Cerulean Agilent 7890

Nic Column: Capillary Length: 5m i.d.: 0.18mm Film Thickness: 0.30µm Stationary Phase: DB-Wax ETR

Nicotine I.S. Octadecane

ThermoAir2 / Schiltknecht Cerulean COA

Water Column: Packed SS 6 ft x 1/8 in. x 2.1mm 80-100 mesh, Porapak Q

Water I.S. Ethanol 200 proof

11 SM450 / Cerulean Agilent 6890

Nic Column: Capillary, CP WAX 52 CB Length: not given i.d.: 0.53mm Film Thickness: 1µm Stationary Phase:CP-Wax

Nicotine I.S. Decanol

Schiltknecht Cerulean COA205

Water Column: Capillary Length: not given i.d.: 0.53mm Film Thickness: 20µm Stationary Phase: PoraPLOT Q

Water I.S. Ethanol

12 RM200A / Borgwaldt KC HP 6890

Nic Column: Length: 30m i.d.: 0.32mm Film Thickness :0.25µm Stationary Phase: Optima-Wax

Nicotine I.S. Heptadecane

Schiltknecht Sibench/Siemens

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Lab Code

Smoking Machine Model Manufacturer

Gas Chromatograph Model/Manufacturer/Column/ Internal Standards

Airflow Meter Model/Manufacturer

NDIR analyser Model/Manufacturer

Water Column: Length: not given i.d.: not given Film Thickness: not given Stationary Phase: Supelco Q Plott

Water I.S. Methanol

13A RM20H / Borgwaldt KC M1 Agilent 7890B

Nic Column: Length: 5m i.d.: 0.32m Film Thickness: 0.4µm Stationary Phase: DB-WAXETR

Nicotine I.S. n-Heptadecane

Schiltknecht g.440.3S-113

Built in RM20H Water Column: Length: 30m i.d.: 0.32mm Film Thickness: 40µm Stationary Phase: PoraPLOT Q

Water I.S. Ethanol

13B RM20H / Borgwaldt KC M2 Agilent 7890B

Nic Column: Length: 5m i.d.: 0.32mm Film Thickness: 0.4µm Stationary Phase: DB-WAXETR

Nicotine I.S. n-Heptadecane

Schiltknecht g.440.3s-113

Built in RM20H

Water Column: Length: 30m i.d.: 0.32mm Film Thickness: 40µm Stationary Phase: PoraPLOT Q

Ethanol

14 RM200A / Borgwaldt KC Agilent 7890A

Nic Column: Length: 30 i.d.: 0.320mm Film thickness: 0.25 Stationary Phase: HP-INNOWAX

Nicotine I.S. n-Heptadecane

Schiltknecht G.440.3S

Borgwaldt KC KC C24

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Lab Code

Smoking Machine Model Manufacturer

Gas Chromatograph Model/Manufacturer/Column/ Internal Standards

Airflow Meter Model/Manufacturer

NDIR analyser Model/Manufacturer

Water Column: Length: 30m i.d.: 0.320mm Film Thickness: 20µm Stationary Phase: HP-PLOT/Q

Water I.S. Ethanol

15 RM20D_1&2 / Borgwaldt KC HP 6890 Agilent 7890A

Nic Column: Length: 6' stainless steel packed i.d.: not given Film thickness: Stationary Phase: Supelco 10% Carbowax 20M / Chromosorb WAW

Nicotine I.S. n-heptadecane

Schiltknecht Airflow meter ThermoAir

Borgwaldt KC CO/CO2 -C24 Analyser Water Column:

Length: 6'7 x 1/8" O.D. stainless steel i.d.: not given Film Thickness: Stationary Phase: Supelco Haye Sep Q

Water I.S. Methanol

16A

SM450 / Cerulean Agilent 6890

Nic Column: Length: 6' X 1/8" O.D.stainless steel i.d.: Film thickness: Stationary Phase:2% Versamid 900+1%KOH on Chromosorb 750 80/100 mesh

Nicotine I.S. n-heptadecane

ThermoAir2 Schiltknecht

VMD 100 /FILTRONA Cerulean COA 205

Water Column: Length: 6' X 1/8" O.D.stainless steel i.d.: Film Thickness: Stationary Phase: PorapakQ

Water I.S. Methanol

Page 94: Routine Analytical Chemistry Sub-Group · RAC-134-CTR CM8 Coll. Study 2017 – November 2017 6/103 Table 5: WEIGHT mean and standard deviation per laboratory code Lab Code Machine

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Lab Code

Smoking Machine Model Manufacturer

Gas Chromatograph Model/Manufacturer/Column/ Internal Standards

Airflow Meter Model/Manufacturer

NDIR analyser Model/Manufacturer

80/100 mesh

16B SM450 / Cerulean Agilent 6890

Nic Column: Length: 6' X 1/8" O.D.stainless steel i.d.: Film thickness: Stationary Phase:2% Versamid 900+1%KOH on Chromosorb 750 80/100 mesh

Nicotine I.S. n-heptadecane

ThermoAir2 Schiltknecht

VMD 100 /FILTRONA Cerulean COA 205

Water Column: Length: 6' X 1/8" O.D. stainless steel i.d.: Film Thickness: Stationary Phase: PorapakQ 80/100 mesh

Water I.S. Methanol

16C LX20 / Borgwaldt KC Agilent 6890

Nic Column: Length: 6' X 1/8" O.D.stainless steel i.d.: Film thickness: Stationary Phase:2% Versamid 900+1%KOH on Chromosorb 750 80/100 mesh

Nicotine I.S. n-heptadecane

ThermoAir6

Schiltknecht Anemometer

Borgwaldt KC Inbuilt CX25 gas analysis

module

Page 95: Routine Analytical Chemistry Sub-Group · RAC-134-CTR CM8 Coll. Study 2017 – November 2017 6/103 Table 5: WEIGHT mean and standard deviation per laboratory code Lab Code Machine

RAC-134-CTR CM8 Coll. Study 2017 – November 2017 95/103

Lab Code

Smoking Machine Model Manufacturer

Gas Chromatograph Model/Manufacturer/Column/ Internal Standards

Airflow Meter Model/Manufacturer

NDIR analyser Model/Manufacturer

Water Column: Length: 6' X 1/8" O.D. stainless steel i.d.: Film Thickness: Stationary Phase: PorapakQ 80/100 mesh

Water I.S. Methanol

16D RM20H / Borgwaldt KC Agilent 6890

Nic Column: Length: 6' X 1/8" O.D.stainless steel i.d.: Film thickness: Stationary Phase:2% Versamid 900+1%KOH on Chromosorb 750 80/100 mesh

Nicotine I.S. n-heptadecane

Schiltknecht Anemometer Borgwaldt KC

Inbuilt gas analysis module

Water Column: Length: 6' X 1/8" O.D. stainless steel i.d.: Film Thickness: Stationary Phase: PorapakQ 80/100 mesh

Water I.S. Methanol

17 SM450 / Cerulean Agilent 6890N

Nic Column: Length: 10m i.d.: 0.18mm Film thickness: 0.3µm Stationary Phase: Agilent DB-Wax

Nicotine I.S. Anethole

Schiltknecht ThermoAir2 COA205/Cerulean

Page 96: Routine Analytical Chemistry Sub-Group · RAC-134-CTR CM8 Coll. Study 2017 – November 2017 6/103 Table 5: WEIGHT mean and standard deviation per laboratory code Lab Code Machine

RAC-134-CTR CM8 Coll. Study 2017 – November 2017 96/103

Lab Code

Smoking Machine Model Manufacturer

Gas Chromatograph Model/Manufacturer/Column/ Internal Standards

Airflow Meter Model/Manufacturer

NDIR analyser Model/Manufacturer

Water Column: Length: 3' x 1/4" O.D. stainless steel i.d.: Film Thickness: Stationary Phase: Haye Sep Q 60/80 mesh

Water I.S. Methanol

18 SM450 / Cerulean Agilent 6890

Nic Column: Length: 30m i.d.: 0.32mm Film thickness: 0.25µm Stationary Phase: Propylene Glycol

Nicotine I.S. Anethole

Schiltknecht ThermoAir2 Cerulean COA205 Water Column: Length: 30m i.d.: 0.53mm Film Thickness: 40µm Stationary Phase: Polystrene-divinylbenzene

Water I.S. Methanol

19 SM450 / Cerulean

GC2010-TCD/

SHIMADZU (water

analysis) GC14B-FID/ SHIMADZU

(nicotine analysis)

Nic Column: Length: 2 m i.d.: 3 mm Film thickness: Stationary Phase: Polyethyleneglycol 20 M + KOH 10% + 2% Chromosorb W80/100 AW-DMCS Shimadzu

Nicotine I.S. Heptadecane

99.6%

ThermoAire3 / Schiltknecht Cerulean COA 205

Water Column: Length: 2m stainlees steel packed i.d.: 3 mm Film thickness: Stationary Phase: Porapak Q 80/100 Shimadzu

Water I.S. Ethanol 99.8%

Page 97: Routine Analytical Chemistry Sub-Group · RAC-134-CTR CM8 Coll. Study 2017 – November 2017 6/103 Table 5: WEIGHT mean and standard deviation per laboratory code Lab Code Machine

RAC-134-CTR CM8 Coll. Study 2017 – November 2017 97/103

Lab Code

Smoking Machine Model Manufacturer

Gas Chromatograph Model/Manufacturer/Column/ Internal Standards

Airflow Meter Model/Manufacturer

NDIR analyser Model/Manufacturer

20 SM450 / Cerulean Agilent 6890N

Nic Column: Supleco Length: 6'x 1/8" O.D. stainless Steel i.d.: Film thickness: Stationary Phase: Carbowax 20M, 2%KOH, 3%OS-138 on Chromosorb 80/100

Nicotine I.S. n-Heptadecane

Schiltknecht ThermoAir3 Cerulean COA 205

Water Column: Supleco Length: 10'x 1/8" O.D. stainless Steel Packed i.d.: Film thickness: Stationary Phase: Porapak QS 80/100

Water I.S. Ethanol

21 SM450 / Cerulean Agilent 6890N

Nic Column: Length: 2m i.d.: 2mm Film thickness: Stationary Phase: Carbowax 10% + 2% KOH

Nicotine I.S. n-Heptadecane

435-2/Testo Cerulean COA 205 Water Column: Length: 2m i.d.: 2mm Film Thickness: Stationary Phase: 80/100 mesh Porapak QS

Water I.S. Ethanol

22A RM20H / Borgwaldt KC Model No. 70740010

Agilent 7890A

Nic Column: Length: 2m x 1/8" O.D. i.d.: Film thickness: 2.1mm Stationary Phase: 10% Carbowax 20M + 2% KOH

Nicotine I.S. Heptadecane

Schiltknecht g.440.3s-176

70740050/Borgwaldt KC

Page 98: Routine Analytical Chemistry Sub-Group · RAC-134-CTR CM8 Coll. Study 2017 – November 2017 6/103 Table 5: WEIGHT mean and standard deviation per laboratory code Lab Code Machine

RAC-134-CTR CM8 Coll. Study 2017 – November 2017 98/103

Lab Code

Smoking Machine Model Manufacturer

Gas Chromatograph Model/Manufacturer/Column/ Internal Standards

Airflow Meter Model/Manufacturer

NDIR analyser Model/Manufacturer

Water Column: Length: 2m x 1/8" O.D. i.d.: Film Thickness: 2.0mm Stationary Phase: 80/100 mesh Porapak Q

Water I.S. Ethanol

22B RM20D / Borgwaldt KC

Model No.70750020 Agilent 7890A

Nic Column: Length: 2m x 1/8" O.D. i.d.: Film thickness: 2.1mm Stationary Phase: 10% Carbowax 20M + 2% KOH

Nicotine I.S. Heptadecane

Schiltknecht g.440.3s-176

70740050/Borgwaldt KC Water Column: Length: 2m x 1/8" O.D. i.d.: Film Thickness: 2.0mm Stationary Phase: 80/100 mesh Porapak Q

Water I.S. Ethanol

24A SM450RH / Cerulean Agilent 7890B

Nic Column: Length: 15m i.d.: 0.32mm Film thickness: 0.25µm Stationary Phase: Restek # 10821 Stabilwax-DB

Nicotine I.S. Carvone

Schiltknecht Messtechnik ThermoAir6

Cerulean COA 205-15

Water Column: Length: 10' x 1/8" O.D. i.d.: Film Thickness: 2.1mm Stationary Phase: 80/100 mesh Porapak-QS

Water I.S. Ethanol

Page 99: Routine Analytical Chemistry Sub-Group · RAC-134-CTR CM8 Coll. Study 2017 – November 2017 6/103 Table 5: WEIGHT mean and standard deviation per laboratory code Lab Code Machine

RAC-134-CTR CM8 Coll. Study 2017 – November 2017 99/103

Lab Code

Smoking Machine Model Manufacturer

Gas Chromatograph Model/Manufacturer/Column/ Internal Standards

Airflow Meter Model/Manufacturer

NDIR analyser Model/Manufacturer

24B Hawktech 2000 Agilent 7890B

Nic Column: Length: 15m i.d.: 0.32mm Film thickness: 0.25µm Stationary Phase: Restek # 10821 Stabilwax-DB

Nicotine I.S. Carvone

Schiltknecht Messtechnik ThermoAir6

California Analytical Instruments CAI 100

Water Column: Length: 10' x 1/8" O.D. i.d.: Film Thickness: 2.1mm Stationary Phase: 80/100 mesh Porapak-QS

Water I.S. Ethanol

25 SM450 / Cerulean Agilent 6890N

Nic Column: Length: 6' x 1/8"O.D. stainless steel packed Stationary Phase: 7% Carbowax 20M, 2% KOH, 3% OS-138 Chromosorb W-HP, 80/100 mesh

Nicotine I.S. Anethole

ThermoAir2 / Schiltknecht

Cerulean COA 205

Water Column: Length: 10' x 1/8" O.D. stainless steel packed Stationary Phase: Porapak QS, 80/100 mesh

Water I.S. Ethanol

26 RM200A / Borgwaldt KC Agilent 7890A

Nic Column: Length: 30m i.d.: 0.53mm Film thickness: 1.00µm Stationary Phase: DB Wax Crosslinked 5% PHME Siloxane

Nicotine I.S. Heptadecane

ThermoAir3 / Schiltknecht

Integrated CO Module / Borgwaldt KC

Page 100: Routine Analytical Chemistry Sub-Group · RAC-134-CTR CM8 Coll. Study 2017 – November 2017 6/103 Table 5: WEIGHT mean and standard deviation per laboratory code Lab Code Machine

RAC-134-CTR CM8 Coll. Study 2017 – November 2017 100/103

Lab Code

Smoking Machine Model Manufacturer

Gas Chromatograph Model/Manufacturer/Column/ Internal Standards

Airflow Meter Model/Manufacturer

NDIR analyser Model/Manufacturer

Water Column: Length: 8' x 1/8" O.D. stainless steel packed i.d. 2.1mm Film Thickness: Stationary Phase: HayeSep Q 80/100

Water I.S. Ethanol

27 LX20 / Borgwaldt KC Agilent 7890B

Nic Column: Length: 30m i.d.: 0.53mm Film thickness: 1.00µm Stationary Phase: Polyethylene glycol

Nicotine I.S. n-Heptadecane

ThermoAir6 / Schiltknecht

CX25

Water Column: Length: 10m i.d.: 0.53mm Film Thickness: 20µm Stationary Phase: Poraplot

Water I.S. Ethanol

28 SM450 / Cerulean

CLARUS 500

PERKIN ELMER

Nic Column: Length: i.d.: Film thickness: Stationary Phase: 7%CW-20M 3%PMPE 6 RING 2%KOH ON CHROMOSORB WHP

Nicotine I.S. n-Heptadecane

Schiltknecht ThermoAir2

TSI 8910/8470 Cerulean COA 205

Water Column: Length: i.d.: Film Thickness: Stationary Phase: PORAPAK Q Mesh?

Water I.S. Ethanol

Page 101: Routine Analytical Chemistry Sub-Group · RAC-134-CTR CM8 Coll. Study 2017 – November 2017 6/103 Table 5: WEIGHT mean and standard deviation per laboratory code Lab Code Machine

RAC-134-CTR CM8 Coll. Study 2017 – November 2017 101/103

Lab Code

Smoking Machine Model Manufacturer

Gas Chromatograph Model/Manufacturer/Column/ Internal Standards

Airflow Meter Model/Manufacturer

NDIR analyser Model/Manufacturer

29 SM450 / Cerulean Agilent 7890A

Nic Column: Length: 30m i.d.: 0.32mm Film thickness: 0.25µm Stationary Phase: CAM/Base deactivated polyethylene glycol

Nicotine I.S. n-Heptadecane

VFA450RH-1/CERULEAN Cerulean COA 205 Water Column: Length: 2m i.d.: 2mm Film Thickness: Stationary Phase: PORAPAK QS 80/100 mesh

Water I.S. Methanol

30 RM200A Agilent 7890A

Nic Column: Length: 30m i.d.: 0.32mm Film thickness: 0.25µm Stationary Phase: HP-5

Nicotine I.S. n-Heptadecane

- -

Water Column: Length: 30m i.d.: 0.53mm Film Thickness: 40.0µm Stationary Phase: HP-PLOT/Q

Water I.S. Ethanol

31 RM20 Shimadzu

Nic Column: Length: 30m i.d.: 0.53mm Film thickness: 1 µm Stationary Phase: ZB Wax

Nicotine I.S. n-Heptadecane

Integrated Airflow meter Integrated NDIR analyser Water Column: Length: 30m i.d.: 0.53mm Film Thickness: 40 µm Stationary Phase: HP Plot Q

Water I.S. Ethanol

Page 102: Routine Analytical Chemistry Sub-Group · RAC-134-CTR CM8 Coll. Study 2017 – November 2017 6/103 Table 5: WEIGHT mean and standard deviation per laboratory code Lab Code Machine

RAC-134-CTR CM8 Coll. Study 2017 – November 2017 102/103

Lab Code

Smoking Machine Model Manufacturer

Gas Chromatograph Model/Manufacturer/Column/ Internal Standards

Airflow Meter Model/Manufacturer

NDIR analyser Model/Manufacturer

32 SM450 / Cerulean Agilent 7890B

Nic Column: Length: 15m i.d.: 0.32mm Film thickness: 0.25µm Stationary Phase: DB-WAXETR

Nicotine I.S. n-Heptadecane

ThermoAir2/Schiltknecht DGA205/Cerulean Water Column: Length: 30m i.d.: 0.53mm Film Thickness: 40.0µm Stationary Phase: HP Plot Q

Water I.S. Ethanol

33 LM20X / Borgwaldt KC Thermo

Trace GC Ultra

Nic Column: Length: 15m i.d.: 2.0mm Film thickness:1.0µm Stationary Phase: DB-WAXETR

Nicotine I.S. n-Heptadecane

Schiltknecht not provided Water Column: Length: 8' x 1/8"O.D. stainless steel packed i.d.: 2.0mm Film Thickness: Stationary Phase: Custom packed column

Water I.S. Ethanol

34 SM450 / Cerulean

6890 N / Agilent

Technologies 7890 B / Agilent

Technologies

Nic Column: Length: 15m i.d.: 0.530mm Film thickness: 1.00µm Stationary Phase: HP INNOWAX

Nicotine I.S. n-Heptadecane

ThermoAir2. Model f.445.2s-146. Schiltknecht

Messtechnik AG COA 205-15 / Cerulean

Page 103: Routine Analytical Chemistry Sub-Group · RAC-134-CTR CM8 Coll. Study 2017 – November 2017 6/103 Table 5: WEIGHT mean and standard deviation per laboratory code Lab Code Machine

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Lab Code

Smoking Machine Model Manufacturer

Gas Chromatograph Model/Manufacturer/Column/ Internal Standards

Airflow Meter Model/Manufacturer

NDIR analyser Model/Manufacturer

Water Column: Length: 2m x 3.8mm stainless steel packed i.d.: 2.0mm Film Thickness: Stationary Phase: Custom packed columnPorapak Q 80 - 100 Mesh

Water I.S. Ethanol

35 RM20M / Borgwaldt KC KC HP 6890

Nic Column: Length: 30m i.d.: 0.32mm Film thickness: 0.25µm Stationary Phase:Optima Wax

Nicotine I.S. n-Heptadecane

Schiltknecht Sibench/Siemens

Water Column: Length: 15m i.d.: 0.32mm Film Thickness: 20µm Stationary Phase: HP-Plot / Q

Water I.S. Methanol