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Routine Analytical Chemistry Sub-Group
Technical Report
2012 Collaborative Study of CORESTA Monitor #7 (CM7)
for the Determination of Test Piece
Weight, TPM, Water, Nicotine, NFDPM, Carbon Monoxide and Puff Count
Obtained Under Mainstream ‘ISO’ and ‘Intense’ Smoking Regimes
May 28, 2013
Author:
Rémi Julien SEITA Imperial Tobacco Group, France
Study Coordinator
Linda A. Crumpler Cerulean, USA
Sub-Group Coordinator
Linda A. Crumpler Cerulean, USA
CTR-RAC_2012 CM7 Collaborative Study 2 of 73 May 2013
CONTENTS
1. INTRODUCTION .................................................................................................... 3
2. ORGANISATION .................................................................................................... 3
2.1 Participants ......................................................................................................... 3
2.2 Protocol .............................................................................................................. 4
3. RAW - DATA ......................................................................................................... 5
4. STATISTICAL ANALYSIS .................................................................................... 13
4.1 Exclusion of Outliers .......................................................................................... 13
4.1.1 Mandel graphical outlier technique: ............................................................... 13
4.1.2 Numerical outlier technique: Cochran & Grubbs test ....................................... 13
4.1.3 Outlier results .............................................................................................. 14
4.2 Repeatability and Reproducibility estimation ........................................................ 14
5. DATA REPRESENTATION ................................................................................... 15
5.1 ISO smoking regime .......................................................................................... 16
5.2 Intense smoking regime ..................................................................................... 19
6. COMPARISON .................................................................................................... 22
6.1 Comparison of Linear with Rotary smoking machines for test piece results of CM7 . 22
6.2 Comparison with previous studies ....................................................................... 23
7. CONCLUSION ..................................................................................................... 24
APPENDIX A - List of Participating Laboratories ........................................................ 25
APPENDIX B – Experimental Protocol ........................................................................ 26
APPENDIX C – Departures from Experimental Protocol ............................................. 36
APPENDIX D – RAW DATA SET ................................................................................. 37
APPENDIX E – MANDEL’S GRAPH ............................................................................. 39
APPENDIX F – IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE ..................... 46
APPENDIX G - LINEAR – ROTARY COMPARISONS .................................................... 47
APPENDIX H - ROTARY SMOKING MACHINES........................................................... 49
1. ISO smoking regime ........................................................................................... 49
2. Intense smoking regime ...................................................................................... 53
APPENDIX I - LINEAR SMOKING MACHINES .............................................................. 56
1. ISO smoking regime ........................................................................................... 56
2. Intense smoking regime ...................................................................................... 60
APPENDIX J – Equipment Survey .............................................................................. 63
CTR-RAC_2012 CM7 Collaborative Study 3 of 73 May 2013
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 2012 study was designed:
to measure mainstream ISO and Intense smoke yields of nicotine-free dry particulate matter (NFDPM), nicotine and carbon monoxide (CO) to verify the current monitor test piece CM7
to determine intra- and inter-laboratory variability for the measured ISO and Intense smoke yields for the CM7
to verify the conditioned weight for the CM7
2. ORGANISATION
2.1 Participants
In total 38 laboratories participated in the 2012 study. Appendix A lists the participating laboratories in alphabetical order. Note: the mix of labs between ISO and Intense differed. 38 laboratories delivered data for ISO mainstream smoke for the CM7 test piece using 53 smoking machines (25 linear smoking machines and 28 rotary smoking machines). 31 laboratories delivered data for Intense mainstream smoke for the CM7 test piece using 40 smoking machines (22 linear smoking machines and 18 rotary smoking machines). Due to technical reasons some laboratories provided incomplete data sets. Table 1 summarises the number and type of smoking machines used. Table 1: Number of smoking machines Machine Class ISO Intense
Rotary smoking machines 28 18 RM20 type 13 8 RM200 type 15 10 Linear smoking machines 25 22 KC20-X type 2 2 LX-20 type 1 1 SM450 type 22 19
Total 53 40
CTR-RAC_2012 CM7 Collaborative Study 4 of 73 May 2013
Table 2 summarises the number of datasets provided by the parameters reported. Table 2: Number of datasets obtained
Physical Parameter WEIGHT 265
Smoking Parameter ISO Intense TPM 265 200 WATER 264 199 NIC 264 199 NFDPM 264 199 CO 260 200 PUFF 265 200
Total individual data obtained 1582 1197 Total individual data expected 1590 1200
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 CM7 – July 3, 2012” (provided in Appendix B) to analyse the product CM7 and to report the seven parameters listed in Table 3. Table 3: Parameters to be reported
Parameter Number of replicates
Unit Code
Nicotine Free Dry Particulate Matter
5 mg/test piece (t.p.) NFDPM
Smoke Nicotine 5 mg/test piece (t.p.) NIC
Carbon Monoxide 5 mg/test piece (t.p.) CO
Total Particulate Matter 5 mg/test piece (t.p.) TPM
Water content (smoke) 5 mg/test piece (t.p.) WATER
Conditioned Weight 5 mg/test piece (t.p.) WEIGHT
Puff count 5 Puffs/test piece (t.p.) PUFF
CM7 test piece should have been smoked under two different mainstream smoking regimes with a fixed butt length of 32 mm as defined in the following table: Table 4: Mainstream ISO and Intense smoking regime parameter
Smoking Regime
Puff Volume (mL)
Puff Frequency (s)
Puff Duration (s)
Vent. Blocking (%)
ISO 35 60 2 0 Intense 55 30 2 100
The CM7 test piece was purchased by the participants individually via Borgwaldt KC or Cerulean.
CTR-RAC_2012 CM7 Collaborative Study 5 of 73 May 2013
3. RAW - DATA Tables 5 to 11 list the results for the seven reported parameters by smoking regime. Basic statistics (mean and standard deviation) were applied to summarize the raw data for each smoking machine used and parameters reported for CM7 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.
CTR-RAC_2012 CM7 Collaborative Study 6 of 73 May 2013
Table 5: WEIGHT mean and standard deviation per laboratory code
Mean Sd
1 966.8 7.5
2A 953.8 3.7
2B 954.9 1.1
3A 955.2 1.8
3B 960.0 4.1
4 954.6 5.1
5 963.1 6.2
6 947.5 1.3
7 965.1 4.4
8A 955.6 5.2
8B 956.4 2.6
9A 955.2 2.8
9B 956.7 3.2
10 956.6 2.4
10B 954.4 1.1
11B 953.1 4.8
11C 959.1 7.5
12A 959.9 2.7
12B 958.5 3.3
14A 970.8 5.1
14B 964.4 3.2
16 953.5 4.5
17 961.1 2.3
18A 952.4 2.4
18B 957.8 5.4
19 976.9 5.9
21 951.9 4.4
22 955.0 4.1
25A 950.3 7.7
25B 956.1 10.3
26 950.9 5.8
28A 957.7 4.7
28B 958.5 3.5
29A 955.8 4.3
29B 954.5 5.1
29C 955.9 4.9
30 957.4 6.1
31 956.2 5.2
32 955.8 4.1
34 961.0 5.9
35 945.2 2.2
36A 967.6 5.0
36B 968.5 1.6
37 955.3 0.7
39 955.7 2.1
40 947.4 3.5
41 951.6 4.5
42A 962.6 5.0
42B 964.0 3.5
43 956.8 2.6
44 946.5 3.3
46 974.6 8.3
47 955.0 2.5
Laboratory
code
WEIGHT (mg/t.p.)
CTR-RAC_2012 CM7 Collaborative Study 7 of 73 May 2013
Table 6: TPM mean and standard deviation per laboratory code
Mean Sd Mean Sd
1 16.43 0.51 46.46 0.88
2A 15.76 0.25 38.37 0.47
2B 16.34 0.20 42.13 0.37
3A 15.83 0.23 37.99 0.28
3B 16.78 0.17 45.08 0.55
4 17.54 0.25 47.65 0.34
5 17.34 0.22 46.90 0.83
6 16.08 0.19 38.51 0.51
7 16.22 0.17 - -
8A 16.19 0.29 39.20 0.29
8B 16.38 0.18 39.29 0.48
9A 16.23 0.39 - -
9B 16.49 0.14 - -
10 16.36 0.12 - -
10B 15.85 0.05 - -
11B 15.79 0.30 37.74 0.55
11C 16.66 0.19 39.94 0.78
12A 16.62 0.35 46.63 0.46
12B 15.90 0.16 38.88 1.00
14A 16.26 0.26 39.15 0.72
14B 16.07 0.50 41.80 0.62
16 16.01 0.27 37.83 1.07
17 16.71 0.22 - -
18A 16.27 0.15 43.25 0.48
18B 16.64 0.30 39.87 0.40
19 16.53 0.56 44.45 0.65
21 15.55 0.68 - -
22 16.82 0.43 42.90 0.69
25A 15.47 0.36 42.93 1.47
25B 16.27 0.79 45.19 0.75
26 16.28 0.37 38.30 0.34
28A 16.25 0.17 - -
28B 15.68 0.16 - -
29A 16.86 0.19 - -
29B 16.25 0.39 - -
29C 16.20 0.08 39.90 0.30
30 15.44 0.38 41.89 0.45
31 16.80 0.26 43.60 0.33
32 16.21 0.17 38.94 0.45
34 16.24 0.23 39.34 0.37
35 16.31 0.45 43.69 0.79
36A 15.64 0.12 - -
36B 15.33 0.75 42.69 1.63
37 14.70 0.14 37.55 0.28
39 17.75 0.29 48.94 1.04
40 16.28 0.23 45.41 0.24
41 16.83 0.44 43.49 0.97
42A 15.85 0.13 38.09 0.46
42B 16.10 0.25 39.65 0.33
43 16.27 0.26 - -
44 15.98 0.28 42.20 0.93
46 16.88 0.26 44.50 1.16
47 15.60 0.27 44.72 1.79
TPM (mg/t.p.)
ISO IntenseLaboratory
code
CTR-RAC_2012 CM7 Collaborative Study 8 of 73 May 2013
Table 7: WATER mean and standard deviation per laboratory code
Mean Sd Mean Sd
1 1.55 0.13 13.41 0.69
2A 1.85 0.06 9.48 0.25
2B 1.27 0.06 11.41 0.32
3A 1.77 0.11 8.58 0.11
3B 1.49 0.05 11.33 0.47
4 1.98 0.12 14.02 0.63
5 1.56 0.11 12.63 0.61
6 2.16 0.06 9.18 0.12
7 2.09 0.04 - -
8A 2.09 0.06 9.63 0.29
8B 2.15 0.20 9.73 0.35
9A 1.62 0.21 - -
9B 2.09 0.29 - -
10 2.01 0.05 - -
10B 1.78 0.10 - -
11B 1.98 0.15 9.32 0.30
11C 1.92 0.06 8.73 0.24
12A 1.78 0.16 13.66 0.45
12B 2.15 0.16 10.18 0.42
14A 2.18 0.10 10.35 0.55
14B 1.33 0.08 9.76 0.32
16 1.93 0.18 8.05 0.53
17 1.61 0.07 - -
18A 1.44 0.04 12.40 0.65
18B 2.11 0.07 9.69 0.52
19 1.59 0.09 11.83 0.48
21 1.27 0.25 - -
22 - - - -
25A 1.16 0.13 8.75 1.08
25B 1.62 0.23 11.93 1.17
26 1.95 0.17 8.67 0.61
28A 2.13 0.21 - -
28B 1.96 0.13 - -
29A 2.15 0.15 - -
29B 2.10 0.08 - -
29C 2.10 0.04 9.55 0.12
30 1.12 0.10 10.36 0.27
31 1.68 0.07 12.10 0.38
32 2.10 0.11 9.59 0.42
34 2.01 0.19 9.95 0.11
35 1.22 0.11 6.53 0.15
36A 1.75 0.11 - -
36B 1.02 0.23 11.90 0.75
37 1.79 0.05 11.77 0.17
39 1.85 0.24 13.60 0.41
40 1.40 0.10 10.95 0.28
41 1.82 0.13 12.64 0.77
42A 2.00 0.14 9.77 0.29
42B 2.05 0.17 10.40 0.24
43 1.51 0.16 - -
44 1.53 0.25 11.85 0.53
46 1.48 0.10 10.75 0.60
47 1.01 0.20 12.25 0.88
Laboratory
code
WATER (mg/t.p.)
ISO Intense
CTR-RAC_2012 CM7 Collaborative Study 9 of 73 May 2013
Table 8: Nicotine mean and standard deviation per laboratory code
Mean Sd Mean Sd
1 1.278 0.029 2.687 0.056
2A 1.194 0.010 2.420 0.036
2B 1.250 0.011 2.505 0.032
3A 1.179 0.020 2.387 0.028
3B 1.265 0.015 2.582 0.013
4 1.296 0.019 2.629 0.030
5 1.244 0.013 2.487 0.038
6 1.129 0.021 2.369 0.033
7 1.270 0.020 - -
8A 1.196 0.041 2.459 0.025
8B 1.163 0.017 2.376 0.023
9A 1.228 0.031 - -
9B 1.228 0.008 - -
10 1.230 0.011 - -
10B 1.224 0.016 - -
11B 1.215 0.011 2.466 0.018
11C 1.260 0.018 2.442 0.023
12A 1.240 0.016 2.544 0.018
12B 1.216 0.017 2.420 0.031
14A 1.125 0.155 2.461 0.040
14B 1.035 0.026 2.193 0.046
16 1.200 0.016 2.385 0.052
17 1.270 0.024 - -
18A 1.203 0.032 2.484 0.045
18B 1.185 0.032 2.393 0.045
19 1.198 0.042 2.377 0.140
21 1.161 0.037 - -
22 - - - -
25A 1.181 0.069 2.382 0.059
25B 1.217 0.020 2.474 0.060
26 1.268 0.024 2.570 0.037
28A 1.174 0.021 - -
28B 1.172 0.023 - -
29A 1.209 0.012 - -
29B 1.202 0.019 - -
29C 1.181 0.004 2.280 0.034
30 1.228 0.016 2.603 0.065
31 1.251 0.015 2.545 0.044
32 1.199 0.025 2.348 0.096
34 1.224 0.018 2.497 0.020
35 1.294 0.038 1.593 0.030
36A 1.123 0.027 - -
36B 1.150 0.034 2.415 0.056
37 1.057 0.012 1.127 0.028
39 1.208 0.013 2.366 0.039
40 1.314 0.019 2.671 0.033
41 1.307 0.051 2.536 0.046
42A 1.170 0.010 2.316 0.031
42B 1.178 0.004 2.375 0.017
43 1.272 0.013 - -
44 1.249 0.023 2.518 0.067
46 1.200 0.015 2.369 0.059
47 1.321 0.065 2.622 0.115
Laboratory
code
NIC (mg/t.p.)
ISO Intense
CTR-RAC_2012 CM7 Collaborative Study 10 of 73 May 2013
Table 9: NFDPM mean and standard deviation per laboratory code
Mean Sd Mean Sd
1 13.61 0.42 30.36 0.37
2A 12.72 0.19 26.47 0.25
2B 13.81 0.15 28.22 0.26
3A 12.88 0.16 27.03 0.30
3B 14.03 0.17 31.16 0.55
4 14.27 0.21 31.01 0.34
5 14.53 0.17 31.78 0.70
6 12.79 0.17 26.96 0.45
7 12.86 0.15 - -
8A 12.91 0.27 27.10 0.23
8B 13.07 0.16 27.19 0.31
9A 13.38 0.22 - -
9B 13.17 0.20 - -
10 13.13 0.12 - -
10B 12.85 0.11 - -
11B 12.59 0.20 25.95 0.29
11C 13.47 0.16 28.77 0.61
12A 13.60 0.31 30.43 0.62
12B 12.54 0.26 26.28 0.57
14A 12.96 0.24 26.35 0.24
14B 13.72 0.42 29.84 0.35
16 12.88 0.37 27.40 1.11
17 13.83 0.13 - -
18A 13.63 0.10 28.36 0.30
18B 13.34 0.21 27.78 0.20
19 13.74 0.56 30.24 0.91
21 13.12 0.61 - -
22 - - - -
25A 13.13 0.26 31.79 0.57
25B 13.43 0.59 30.78 1.14
26 13.05 0.30 27.07 0.37
28A 12.94 0.19 - -
28B 12.55 0.05 - -
29A 13.51 0.22 - -
29B 12.95 0.33 - -
29C 12.92 0.10 28.07 0.38
30 13.10 0.40 28.93 0.26
31 13.87 0.18 28.95 0.39
32 12.91 0.11 27.00 0.55
34 13.01 0.24 26.89 0.36
35 13.80 0.33 35.57 0.72
36A 12.77 0.14 - -
36B 13.16 0.53 28.37 1.12
37 11.85 0.11 23.52 0.34
39 14.69 0.17 32.89 0.91
40 13.57 0.20 31.79 0.43
41 13.70 0.37 28.31 0.40
42A 12.68 0.11 26.01 0.24
42B 12.88 0.13 26.88 0.23
43 13.49 0.34 - -
44 13.20 0.33 27.83 0.62
46 14.19 0.28 31.38 1.04
47 13.26 0.23 29.84 1.13
Laboratory
code
NFDPM (mg/t.p.)
ISO Intense
CTR-RAC_2012 CM7 Collaborative Study 11 of 73 May 2013
Table 10: CO mean and standard deviation per laboratory code
Mean Sd Mean Sd
1 13.10 0.33 24.85 0.33
2A 13.26 0.09 25.18 0.28
2B 12.70 0.22 24.15 0.44
3A 12.85 0.20 24.38 0.32
3B 13.26 0.14 24.90 0.24
4 13.26 0.25 25.39 0.35
5 13.02 0.30 25.10 0.47
6 12.37 0.27 24.30 0.21
7 12.90 0.26 - -
8A 12.96 0.12 24.76 0.23
8B 13.11 0.17 24.35 0.48
9A 12.08 0.15 - -
9B 12.76 0.21 - -
10 13.68 0.15 - -
10B 13.19 0.18 - -
11B 13.38 0.23 25.21 0.41
11C 13.08 0.27 24.09 0.42
12A 13.14 0.22 25.06 0.40
12B 13.00 0.15 24.47 0.66
14A 13.93 0.15 26.06 0.30
14B 12.98 0.25 26.34 0.38
16 13.26 0.26 25.13 0.83
17 - - - -
18A 12.74 0.18 24.63 0.21
18B 13.55 0.24 25.16 0.30
19 12.15 0.38 23.51 0.29
21 12.00 0.62 - -
22 12.79 0.29 23.69 0.28
25A 11.87 0.34 23.90 0.90
25B 12.02 0.33 24.29 0.73
26 13.09 0.11 25.17 0.41
28A 13.57 0.23 - -
28B 13.21 0.18 - -
29A 13.58 0.21 - -
29B 12.80 0.18 - -
29C 13.16 0.17 24.58 0.11
30 11.92 0.29 24.05 0.33
31 12.18 0.37 24.10 0.15
32 12.92 0.13 25.20 0.22
34 13.79 0.09 26.22 0.39
35 11.83 0.22 23.75 0.67
36A 12.94 0.17 - -
36B 12.05 0.55 23.85 0.42
37 11.34 0.23 23.47 0.19
39 15.93 0.32 29.63 0.88
40 12.42 0.16 24.36 0.56
41 12.44 0.39 22.60 0.44
42A 13.37 0.38 25.30 0.26
42B 12.55 0.23 24.63 0.41
43 12.72 0.47 - -
44 12.67 0.50 25.01 0.50
46 12.90 0.34 23.84 0.69
47 12.91 0.83 25.11 0.73
Laboratory
code
CO (mg/t.p.)
ISO Intense
CTR-RAC_2012 CM7 Collaborative Study 12 of 73 May 2013
Table 11: Puff count mean and standard deviation per laboratory code
Mean Sd Mean Sd
1 8.68 0.15 12.00 0.17
2A 7.82 0.08 11.18 0.16
2B 8.29 0.03 11.50 0.12
3A 7.98 0.07 12.03 0.23
3B 8.83 0.06 12.32 0.13
4 8.44 0.08 11.71 0.05
5 8.89 0.19 12.19 0.26
6 8.34 0.10 11.94 0.25
7 8.14 0.10 - -
8A 7.98 0.09 11.37 0.19
8B 7.88 0.09 11.24 0.09
9A 8.28 0.17 - -
9B 8.24 0.06 - -
10 8.52 0.09 - -
10B 8.22 0.08 - -
11B 8.17 0.09 11.87 0.10
11C 8.63 0.17 12.30 0.21
12A 8.63 0.17 11.77 0.12
12B 8.09 0.11 11.43 0.09
14A 8.41 0.08 12.17 0.17
14B 8.34 0.13 11.77 0.11
16 8.26 0.07 11.85 0.18
17 8.65 0.08 - -
18A 8.30 0.20 11.60 0.12
18B 8.10 0.16 11.44 0.21
19 9.01 0.39 12.52 0.25
21 8.60 0.20 - -
22 8.86 0.15 12.40 0.14
25A 7.71 0.16 11.57 0.39
25B 8.15 0.80 12.28 0.23
26 8.13 0.09 11.52 0.12
28A 7.93 0.07 - -
28B 8.19 0.14 - -
29A 8.57 0.19 - -
29B 8.30 0.12 - -
29C 8.32 0.12 11.97 0.19
30 8.26 0.13 11.63 0.05
31 8.67 0.11 12.27 0.17
32 8.23 0.08 11.79 0.11
34 8.15 0.03 11.58 0.18
35 8.25 0.13 11.63 0.13
36A 8.86 0.08 - -
36B 9.23 0.14 12.98 0.14
37 8.21 0.07 11.97 0.13
39 8.82 0.12 12.10 0.10
40 8.25 0.11 11.47 0.10
41 8.70 0.23 12.23 0.15
42A 8.09 0.02 11.45 0.21
42B 8.40 0.08 12.12 0.09
43 8.19 0.02 - -
44 8.31 0.11 11.68 0.19
46 8.75 0.11 12.15 0.15
47 8.50 0.14 11.59 0.24
PUFF (/t.p.)
ISO IntenseLaboratory
code
CTR-RAC_2012 CM7 Collaborative Study 13 of 73 May 2013
4. STATISTICAL ANALYSIS
4.1 Exclusion of Outliers
4.1.1 Mandel graphical outlier technique:
The graphical representation of the Mandel’s tests was examined first.
ISO 5725-2 Tests Consistency
Mandel’s k Within-laboratory variability Mandel’s h Between-laboratory variability
Examination of h and k plots indicated the presence of any suspicious result regarding the within-laboratory standard deviation or any extreme laboratory mean value compared to others. In the simple bar plots, lines were drawn indicating 0.95 straggling and 0.99 outlying limits. Please note that at this stage definite decisions were delayed until completion of numerical outlier techniques mentioned in 5.1.2. Mandel h and k plots are available in the Appendix E additional folder.
4.1.2 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. Note: ISO 5725-2 only provides critical values of the Cochran C and Grubbs statistics up to n=40. Since there were up to n=53 machines included in this study, the critical values
applied for n>40 were determined by the software “R”2 for the Cochran test, and as
described in the article3 “Extension of Sample Sizes and Percentage Points for Significance
Tests of Outlying Observations” for the Grubbs’ test.
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% (for this study =2/9) in the original number of laboratories would occur (see flowchart in Appendix F).
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 2 R Development Core Team (2011). R: A language and environment for statistical computing. R
Foundation for Statistical Computing, Vienna, Austria. ISBN 3-900051-07-0, URL http://www.R-project.org/. 3 Frank E. Grubbs And Glenn Beck, Extension of Sample Sizes and Percentage Points for
Significance Tests of Outlying Observations, TECHNOMETRICS, vol.14(4) (1972).
CTR-RAC_2012 CM7 Collaborative Study 14 of 73 May 2013
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% (2 of 9 laboratories) would be removed. 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.
4.1.3 Outlier results
Table 12 lists the laboratories which were rejected (by parameter and smoking regime), and states the outlier exclusion technique used. A total of 11 smoking machines have been rejected at least once for either one product, one smoking regime or one parameter (14A, 14B, 19, 21, 25A, 25B, 35, 36B, 37, 39, 47). A large number of outliers (70%) is related to within-laboratory variability. The outliers detected by Cochran’s test are mainly attributable to two laboratories (47 and 25B).
Table 12: List of Outliers
Smoking Regime
Parameter
All smoking machines
Cochran’s Outliers Grubbs’ Outliers
Grubbs for individual Outliers
WEIGHT - - -
ISO
TPM 21, 25B, 36B - WATER - - - NIC 14A, 25A, 47 14B, 37 - NFDPM - - - CO 47 39 - PUFF 19, 25B - -
Intense
TPM 36B, 47 - - WATER 25B - - NIC 19, 47 35, 37 - NFDPM - - - CO - 39 - PUFF - - -
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 13, 14 and 15. The corresponding graphs named “individual values” are given in Part 5 of this report.
CTR-RAC_2012 CM7 Collaborative Study 15 of 73 May 2013
Table 13: r&R estimations of CM7 test piece weight Nbr of
LabsMean
Straggling
LabsNo data
sr r sR R C G/G2
53 957.6 4.6 13.0 7.7 21.7 19, 25B, 46
Parameter Repeatability Reproducibility Outlying Labs
WEIGHT Table 14: r&R estimations for CM7 under ISO smoking regime
ParameterMachine
Class
Nbr of
LabsMean
Straggling
LabsNo data
sr r sR R C G/G2
ALL 50 16.28 0.28 0.80 0.59 1.67 21, 25B, 36B
LINEAR 25 16.41 0.41 1.17 0.74 2.08
ROTARY 27 16.16 0.22 0.63 0.37 1.03 37
ALL 53 1.75 0.15 0.41 0.37 1.03
LINEAR 25 1.46 0.16 0.44 0.30 0.84
ROTARY 28 1.99 0.14 0.38 0.20 0.57 9B, 36A, 43
ALL 48 1.221 0.023 0.066 0.051 0.143 14A, 25A, 47 14B, 37 41
LINEAR 24 1.243 0.033 0.093 0.056 0.158 14B 25A
ROTARY 27 1.197 0.019 0.054 0.050 0.142 14A 8A, 36A, 37
ALL 53 13.29 0.27 0.78 0.61 1.73 21
LINEAR 25 13.71 0.34 0.95 0.54 1.54
ROTARY 28 12.92 0.21 0.58 0.38 1.07 12B, 37
ALL 50 12.84 0.27 0.78 0.62 1.75 47 39 21 17
LINEAR 22 12.52 0.33 0.94 0.57 1.62 47 39
ROTARY 27 13.15 0.22 0.62 0.43 1.20 37 43
ALL 51 8.36 0.12 0.34 0.33 0.93 19, 25B
LINEAR 23 8.53 0.14 0.40 0.34 0.97 19, 25B
ROTARY 28 8.23 0.10 0.28 0.25 0.70 11C, 36A
Repeatability Reproducibility Outlying Labs
TPM
NIC
WATER
PUFF
CO
NFDPM
Table 15: r&R estimations for CM7 under intense smoking regime
ParameterMachine
Class
Nbr of
LabsMean
Straggling
LabsNo data
sr r sR R C G/G2
ALL 38 41.78 0.67 1.91 3.31 9.36 36B, 47 25A
LINEAR 22 44.39 0.89 2.53 2.14 6.05 47
ROTARY 18 38.81 0.56 1.57 0.93 2.63
ALL 39 10.64 0.48 1.36 1.77 5.01 25B 25A
LINEAR 22 11.56 0.61 1.73 1.82 5.16 25A, 35
ROTARY 18 9.59 0.35 0.99 0.89 2.51
ALL 36 2.458 0.043 0.123 0.115 0.326 19, 47 35, 37 32
LINEAR 19 2.502 0.047 0.133 0.127 0.361 19, 47 35
ROTARY 16 2.413 0.032 0.091 0.076 0.214 32 37
ALL 40 28.76 0.59 1.67 2.41 6.81
LINEAR 22 30.37 0.69 1.95 1.93 5.46 35, 39
ROTARY 16 26.99 0.37 1.05 0.81 2.31 16 37 11C, 29C
ALL 39 24.62 0.45 1.27 0.88 2.48 39
LINEAR 21 24.40 0.49 1.39 0.92 2.61 39
ROTARY 18 24.87 0.40 1.12 0.76 2.15 16
ALL 40 11.86 0.17 0.49 0.42 1.18
LINEAR 21 11.99 0.16 0.45 0.42 1.20 25A
ROTARY 18 11.73 0.17 0.48 0.37 1.04
PUFF
Repeatability Reproducibility Outlying Labs
TPM
WATER
NIC
NFDPM
CO
5. DATA REPRESENTATION The following figures show the raw data for CM7 and for all parameter. 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 green and red respectively. Lab codes of participants that did not provide data are marked with an asterisk.
CTR-RAC_2012 CM7 Collaborative Study 16 of 73 May 2013
5.1 ISO smoking regime
Figure 1: CM7 Individual observations of conditioned test piece WEIGHT
CONDITIONED WEIGHT_CM7
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.)
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25B 26
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36B 37
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42B 43
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47
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Figure 2: CM7 Individual observations of mainstream “ISO” TPM
TPM_ CM7_ISO
Labs
TP
M (
mg
/t.p
.)
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2B
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47
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++C-out
C-out
C-out
CTR-RAC_2012 CM7 Collaborative Study 17 of 73 May 2013
Figure 3: CM7 Individual observations of mainstream “ISO” WATER
WATER_ CM7_ISO
Labs
WA
TE
R (
mg
/t.p
.)
1
2A
2B
3A
3B 4 5 6 7
8A
8B
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9B 10
10B
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11C
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17
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41
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42B 43
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47
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+
Figure 4: CM7 Individual observations of mainstream “ISO” Nicotine
NIC_ CM7_ISO
Labs
NIC
(m
g/t
.p.)
1
2A
2B
3A
3B 4 5 6 7
8A
8B
9A
9B 10
10B
11B
11C
12A
12B
14A
14B 16
17
18A
18B 19
21
22
25A
25B 26
28A
28B
29A
29B
29C 30
31
32
34
35
36A
36B 37
39
40
41
42A
42B 43
44
46
47
0.85
0.90
0.95
1.00
1.05
1.10
1.15
1.20
1.25
1.30
1.35
1.40
++
+
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+++++++++++++++++++++++++
+++++++++++++++++++++++++
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++ +++++++++++++++++++++++++
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+++++++++++++++++++++++++ +
++++++++++++++++++++++++
++++
+
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++
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+++
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C-out
C-out
C-out
G2_out_l
G2_out_l
CTR-RAC_2012 CM7 Collaborative Study 18 of 73 May 2013
Figure 5: CM7 Individual observations of mainstream “ISO” NFDPM
NFDPM_ CM7_ISO
Labs
NF
DP
M (
mg
/t.p
.)
1
2A
2B
3A
3B 4 5 6 7
8A
8B
9A
9B 10
10B
11B
11C
12A
12B
14A
14B 16
17
18A
18B 19
21
22
25A
25B 26
28A
28B
29A
29B
29C 30
31
32
34
35
36A
36B 37
39
40
41
42A
42B 43
44
46
47
11.0
11.5
12.0
12.5
13.0
13.5
14.0
14.5
15.0
15.5
+
+
+
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+++++
+++++
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+++++
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++++++++++++++++++++
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+++
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+++
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+++++++++++++++++++++++++
+
++++
+
++++
+
++++
+
++++
+
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++
+
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+
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+++++++++++++++++++++++++
+
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+++++
++
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+
+
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+
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+
+
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+
+
+
++
+
Figure 6: CM7 Individual observations of mainstream “ISO” CO
CO_ CM7_ISO
Labs
CO
(m
g/t
.p.)
1
2A
2B
3A
3B 4 5 6 7
8A
8B
9A
9B 10
10B
11B
11C
12A
12B
14A
14B 16
17*
18A
18B 19
21
22
25A
25B 26
28A
28B
29A
29B
29C 30
31
32
34
35
36A
36B 37
39
40
41
42A
42B 43
44
46
47
10.5
11.0
11.5
12.0
12.5
13.0
13.5
14.0
14.5
15.0
15.5
16.0
16.5
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++ ++
+++++++++++++++++++++++
+++
++
+++
++
+++
++
+++
++
+++
++
++
+++
++
+++
++
+++
++
+++
++
++++
+
++++
+
++++
+
++++
+
++++
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+++
+
+
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+
++
+
+
+
++
+
+
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++
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+
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++
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+
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+
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+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+
+
+++
+
+
+++
+
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+++
+
+
+++
+
+
++
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++
+
++
++
+
++
++
+
++
++
+
++
++ ++++
+
+++++
+++++
+++++
+++++ +
+++
++
+++
++
+++
++
+++
++
+++
+
+++++
+++++
+++++
+++++
+++++
+
+
++++
+
++++
+
++++
+
++++
+
+++
+++
+++++
+++++
+++++
+++++
++
++
+
++++
+
++++
+
++++
+
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+++++++++++++++++++++++++
+++++
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+++++++++++++++++++++++++
+
++++
+
++++
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++++
+
++++
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++++
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+++++
+++++
+++++
+++++
++++
+
++
+
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+++
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++
+
+
C-out
G_out_h
CTR-RAC_2012 CM7 Collaborative Study 19 of 73 May 2013
Figure 7: CM7 Individual observations of mainstream “ISO” PUFF Count
PUFF_ CM7_ISO
Labs
PU
FF
(/t
.p.)
1
2A
2B
3A
3B 4 5 6 7
8A
8B
9A
9B 10
10B
11B
11C
12A
12B
14A
14B 16
17
18A
18B 19
21
22
25A
25B 26
28A
28B
29A
29B
29C 30
31
32
34
35
36A
36B 37
39
40
41
42A
42B 43
44
46
47
6.8
7.0
7.2
7.4
7.6
7.8
8.0
8.2
8.4
8.6
8.8
9.0
9.2
9.4
9.6
9.8
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
++++
+++++
+++++
+++++
+++++
+
+++++++++++++++++++++++++
+
++++
+
++++
+
++++
+
++++
+
++++
+++
+++++
+++++
+++++
+++++
++
+
++++
+
++++
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++++
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++++
++
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+
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++++
+
++++
+
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++++
+
+++ +
+++
++
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+++
++
+++
+
+
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++++
+
++++
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++++
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++++
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+++
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+++
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+
++
+
+
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++
+
+
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+ +++++++++++++++++++++++++
+
+
++++
+
++++
+
++++
+
++++
+
+++
+
+
++++
+
++++
+
++++
+
++++
+
+++
+++++++++++++++++++++++++
+
+
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++++
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+
+
++
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++++
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+++++
+++++
+++++
+++
++
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++++
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++
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+++
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+++
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+++
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+
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++ +
+
+
+++
+
+
+++
+
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+++
+
+
+++
+
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+
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++
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+
++++
+
++++
+
++++
+
++++
+
+++
+++++++++++++++++++++++++ +
+
+
+
+
+
+
+
+
+
+
+
+
+
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+
+
+
+
+
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+++
+
++++
+
++++
+
++++
+
++++
+
+
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+
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+
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+
+
+
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+
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+
+
+
++++
+
++++
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++++
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++++
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++
+
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+
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+
+
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+
+++++++++++++++++++++++++
++++
+++++
+++++
+++++
+++++
+
++++++++++++++++++++++++++++
+
++++
+
++++
+
++++
+
++++
+
+
++
+
+
+++
+
+
+++
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+
+
+++
+
+
+
+++
+
++++
+
++++
+
++++
+
++++
+
+
C-out
C-out
5.2 Intense smoking regime
Figure 8: CM7 Individual observations of mainstream “Intense” TPM
TPM_ CM7_Intense
Labs
TP
M (
mg
/t.p
.)
1
2A
2B
3A
3B 4 5 6 7*
8A
8B
9A
*
9B
*
10*
10B
*
11B
11C
12A
12B
14A
14B 16
17*
18A
18B 19
21*
22
25A
25B 26
28A
*
28B
*
29A
*
29B
*
29C 30
31
32
34
35
36A
*
36B 37
39
40
41
42A
42B
43*
44
46
47
30
32
34
36
38
40
42
44
46
48
50
52
54
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
++
+++++
+++++
+++++
+++++
+++
+++++++++++++++++++++++++
+++++++++++++++++++++++++
+++++++++++++++++++++++++
+++++++++++++++++++++++++
++
+
++
++
+
++
++
+
++
++
+
++
++
+
++
+++++++++++++++++++++++++
+++++++++++++++++++++++++
+
+++++
+++++
+++++
+++++
++++
++++
+
++++
+
++++
+
++++
+
++++
+
++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+
+++++++++++++++++++++++++
+
++
+++
++
+++
++
+++
++
+++
++
++
+
++++
+
++++
+
++++
+
++++
+
++++
++++
+
++++
+
++++
+
++++
+
++++
+
++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+
++
+++++
+++++
+++++
+++++
+++
+++
+++++
+++++
+++++
+++++
++
++
+++++
+++++
+++++
+++++
+++
++++
+
++++
+
++++
+
++++
+
++++
+ ++++
+
++++
+
++++
+
++++
+
++++
++
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+++++++++++++++++++++++++
+++++++++++++++++++++++++
+++++++++++++++++++++++++
+++++++++++++++++++++++++
++++
+
++++
+
++++
+
++++
+
++++
++++++++++++++++++++++++++
+++
++
+++
++
+++
++
+++
++
+++
++
++
++
+
++
++
+
++
++
+
++
++
+
++
++
+
+++++++++++++++++++++++++
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+++++++++++++++++++++++++
+
+
++++
+
++++
+
++++
+
++++
+
+++
+++++++++++++++++++++++++
+++++++++++++++++++++++++
+
+++
++
+++
++
+++
++
+++
++
+++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+++
++
+++
++
+++
++
+++
++
+++
+C-out
C-out
CTR-RAC_2012 CM7 Collaborative Study 20 of 73 May 2013
Figure 9: CM7 Individual observations of mainstream “Intense” WATER
WATER_ CM7_Intense
Labs
WA
TE
R (
mg
/t.p
.)
1
2A
2B
3A
3B 4 5 6 7*
8A
8B
9A
*
9B
*
10*
10B
*
11B
11C
12A
12B
14A
14B 16
17*
18A
18B 19
21*
22
25A
25B 26
28A
*
28B
*
29A
*
29B
*
29C 30
31
32
34
35
36A
*
36B 37
39
40
41
42A
42B
43*
44
46
47
5
6
7
8
9
10
11
12
13
14
15
16
17
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++++
+++++
+++++
+++++
++++
++++
+
++++
+
++++
+
++++
+
++++
+
+++++++++++++++++++++++++
++
+
++
++
+
++
++
+
++
++
+
++
++
+
++
+
++++
+
++++
+
++++
+
++++
+
++++
++++
+
++++
+
++++
+
++++
+
++++
+
+++++++++++++++++++++++++ +
+++++
+++++
+++++
+++++
++++
+
+++++
+++++
+++++
+++++
++++
++++
+
++++
+
++++
+
++++
+
++++
+ +++
+++++
+++++
+++++
+++++
++
+
+++++
+++++
+++++
+++++
++++
+
+++++
+++++
+++++
+++++
++++
+
++++
+
++++
+
++++
+
++++
+
++++
++++
+++++
+++++
+++++
+++++
+
++
+++
++
+++
++
+++
++
+++
++
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
++++++++++++++++++++
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
++
++
+
++
++
+
++
++
+
++
++
+
++
++
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+ +++++++++++++++++++++++++
+++++++++++++++++++++++++
+++++
+++++
+++++
+++++
+++++
+++
+
++++
+
++++
+
++++
+
++++
+
++++++++++++++++++++++++++
+++++++++++++++++++++++++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+++++++++++++++++++++++++
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
++
+
++++
+
++++
+
++++
+
++++
+
++
+
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
++
++
+++++
+++++
+++++
+++++
+++
+
+++++
+++++
+++++
+++++
++++
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
+
C-out
Figure 10: CM7 Individual observations of mainstream “Intense” Nicotine
NIC_ CM7_Intense
Labs
NIC
(m
g/t
.p.)
1
2A
2B
3A
3B 4 5 6 7*
8A
8B
9A
*
9B
*
10*
10B
*
11B
11C
12A
12B
14A
14B 16
17*
18A
18B 19
21*
22
25A
25B 26
28A
*
28B
*
29A
*
29B
*
29C 30
31
32
34
35
36A
*
36B 37
39
40
41
42A
42B
43*
44
46
47
1.0
1.2
1.4
1.6
1.8
2.0
2.2
2.4
2.6
2.8
3.0
++
+
++++
+
++++
+
++++
+
++++
+
++
+++++++++++++++++++++++++
+++++++++++++++++++++++++
+++++++++++++++++++++++++
+++++++++++++++++++++++++ +++
++++++++++++++++++++++
+++
+++++
+++++
+++++
+++++
++
+++++++++++++++++++++++++
+++++++++++++++++++++++++
+++++++++++++++++++++++++
+++++++++++++++++++++++++
+++++++++++++++++++++++++
+++++++++++++++++++++++++
+++++++++++++++++++++++++ +
++
+++++
+++++
+++++
+++++
++
+
++++
+
++++
+
++++
+
++++
+
++++
+
+
++++
+
++++
+
++++
+
++++
+
+++
+++
++
+++
++
+++
++
+++
++
+++
++ +
+
++++
+
++++
+
++++
+
++++
+
+++
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
++++++++++++++++++++
+++++
+++++
+++++
+++++
+++++ +++
++
+++
++
+++
++
+++
++
+++
++
+++++
+++++
+++++
+++++
+++++
+++++++++++++++++++++++++
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+++++++++++++++++++++++++
+
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
+
+++++++++++++++++++++++++
+++++++++++++++++++++++++
+
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
++
+++++++++++++++++++++++++
+++
+++++
+++++
+++++
+++++
++
+++
+++++
+++++
+++++
+++++
++
+++++++++++++++++++++++++
+++++++++++++++++++++++++
+++++++++++++++++++++++++
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
++
+++
++
+++
++
+++
++
+++
++
++
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
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CTR-RAC_2012 CM7 Collaborative Study 21 of 73 May 2013
Figure 11: CM7 Individual observations of mainstream “Intense” NFDPM
NFDPM_ CM7_Intense
Labs
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Figure 12: CM7 Individual observations of mainstream “Intense” CO
CO_ CM7_Intense
Labs
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(m
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.p.)
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CTR-RAC_2012 CM7 Collaborative Study 22 of 73 May 2013
Figure 13: CM7 Individual observations of mainstream “Intense” PUFF Count
PUFF_ CM7_Intense
Labs
PU
FF
(/t
.p.)
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6. COMPARISON
6.1 Comparisons of linear with rotary smoking machines for test piece results of CM7
It should be noted that a statistical evaluation of differences in linear and rotary smoking machine results on the basis of just one product (CM7) 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 seems to have limited value. Graphical comparison of smoke data separated for linear and rotary smoking machines are available in appendix G.
CTR-RAC_2012 CM7 Collaborative Study 23 of 73 May 2013
6.2 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 16 lists the averages, reproducibility and repeatability limits for the test pieces CM4, CM5, CM6 and CM7 under ISO smoking regime. Table 16: Averages, repeatability, reproducibility of CORESTA collaborative studies from 2004 to 2012 for different test pieces under ISO smoking conditions
Year 2004 2005 2006 2007 2008 2010 2011 2011 2012
Test Piece CM4 CM5 CM5 CM6 CM6 CM6 CM6 CM7 CM7
Average
TPM 17.53 16.71 16.58 17.71 17.54 17.37 17.43 16.37 16.28 WATER 2.23 2.44 2.44 1.91 1.87 1.81 1.84 1.78 1.75 NIC 1.295 1.078 1.083 1.384 1.390 1.366 1.362 1.236 1.221 NFDPM 13.98 13.20 13.03 14.40 14.28 14.18 14.21 13.34 13.29 CO 13.14 14.07 13.88 14.82 14.83 14.56 14.42 12.93 12.84 PUFF 9.10 7.72 7.64 9.18 9.15 9.09 9.00 8.36 8.36
Repeatability (r)
TPM 0.95 1.13 1.14 0.84 0.83 0.81 0.94 0.93 0.80 WATER 0.48 0.53 0.55 0.43 0.43 0.40 0.47 0.41 0.41 NIC 0.080 0.075 0.080 0.096 0.080 0.074 0.084 0.075 0.066 NFDPM 0.75 0.87 0.75 0.92 0.71 0.63 0.80 0.77 0.78 CO 0.78 1.01 1.04 1.07 0.82 0.92 0.95 0.95 0.78 PUFF 0.42 0.38 0.34 0.37 0.37 0.39 0.33 0.38 0.34
Reproducibility (R)
TPM 1.89 2.58 2.78 1.81 1.77 1.54 1.72 1.77 1.67 WATER 1.51 1.21 1.22 1.07 1.11 1.09 0.98 0.97 1.03 NIC 0.158 0.140 0.147 0.167 0.131 0.150 0.173 0.150 0.143 NFDPM 1.90 2.17 2.29 1.92 1.80 1.53 1.92 1.88 1.73 CO 1.98 1.82 1.62 1.84 1.64 1.96 1.83 1.94 1.75 PUFF - 0.78 0.93 0.89 0.88 0.82 0.69 0.86 0.93
The data in Table 16 indicate that the mean values for the listed smoke parameters are quite stable for the CM7 between 2011 and 2012. The CM7 test piece shows comparable reproducibility and repeatability data with the CM6 test piece for all parameters as already mentioned in the 2011 collaborative study. A graphical comparison of the reproducibility for the parameter TPM for all studies since 2004 (Figure 14) shows only two increased figures for repeatability and reproducibility limits of TPM. These data (2005 and 2006) relate to the test piece CM5 which had noticeable higher weight variations (Table 16) compared to other test pieces. TPM repeatability and reproducibility for the CM7 test piece is in line with CM6 and lower with other test pieces in previous collaborative studies.
CTR-RAC_2012 CM7 Collaborative Study 24 of 73 May 2013
Figure 14: TPM Repeatability and Reproducibility of CORESTA collaborative studies for various test pieces
R & r estimations from 2004 to 2012
TP
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.)
14
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2004-CM4 2005-CM5 2006-CM5 2007-CM6 2008-CM6 2010-CM6 2011-CM6 2011-CM7 2012-CM7
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Table 17 lists the averages, reproducibility and repeatability limits of weight that are quite stable for the CM7 between 2011 and 2012. Table 17: Average weight data, repeatability and reproducibility for test pieces CM7
Study CM7 2011 CM7 2012
Weight (mg/t.p.) 957.2 957.6 Repeatability (r) 13.0 13.0
Reproducibility (R) 20.0 21.7
7. CONCLUSION In summary the analytical results for the CM7 test piece lead to the conclusion that it can be used as a monitor test piece in smoke analysis.
CTR-RAC_2012 CM7 Collaborative Study 25 of 73 May 2013
APPENDIX A – List of Participating Laboratories
Arista Europe Karelia Tobacco Company
Arista Laboratories Inc. KT&G
BAT Germany GmbH Laboratoire National De Metrologie Et D’Essais
BAT GR&D Laboratorio Agroalimentario Sevilla
BAT Korea* Labstat International
Borgwaldt KC GmbH Landewyck Group sarl.
C.I.T. Monte Paz S.A. Lorillard Tobacco Company
China National Tobacco Supervision & Test Center
Massalin Particulares
Enthalpy MST/Vectis
Filtrona Technology Centre PMI R&D
Global Laboratory Services PSS Stellenbosch
Imperial Tobacco Joure* PT HM Sampoerna Tbk.
Imperial Tobacco Nottingham* Reemtsma/Imperial Tobacco Central Lab
Imperial Tobacco Maroc* R.J. Reynolds Tobacco Company (Lancaster Laboratories)
Imperial Tobacco Polska S.A.* Seita Imperial Tobacco Group
ITC Limited Souza Cruz RPC-Americas
Japan Tobacco Inc. SWM Intl
JTI Gallaher U.K. TIOJ*
JTI Germany GmbH Papierfabrik Wattens
* CM7 ISO Regime Only
CTR-RAC_2012 CM7 Collaborative Study 26 of 73 May 2013
APPENDIX B – Experimental Protocol
Annual Study of the CORESTA Monitor Test Piece CM7– July 03, 2012 Experimental protocol 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 CM7. 2. Objectives This year’s study will have expanded objectives that include smoking the monitor test piece(s) 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 CM7 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. Normative References The relevant Standards for ISO smoking: Definitions and standard conditions ISO 3308:2000 Conditioning ISO 3402:1999 TPM / NFDPM ISO 4387:2000/Amd 1:2008 Carbon monoxide ISO 8454:2007 Nicotine ISO 10315:2000 Water (GC) ISO 10362-1:1999
Intense smoking (in addition to the ISO Standards above): Ventilation zone blocking, puffing parameters and number of test pieces smoked
Health Canada Method T-115 paragraph 16.1 http://www.hc-sc.gc.ca/hc-ps/alt_formats/hecs-sesc/pdf/tobac-tabac/legislation/reg/indust/method/_main-principal/nicotine-eng.pdf
Data analysis ISO 5725-2:1994/Cor 1:2002
CTR-RAC_2012 CM7 Collaborative Study 27 of 73 May 2013
4. METHODS
4.1. 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 cigarette 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 32 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: Athough 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 2 0.02 100 Intense
* Time from the start of one puff to the start of the next puff.
4.2 Sampling The study will use the CORESTA Monitor CM7. Each participating laboratory is responsible for procuring their own supply of CM7 through the normal sources (Borgwaldt KC or Cerulean – Appendix 1). 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. 4.3 Ventilation Zone Blocking 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.
CTR-RAC_2012 CM7 Collaborative Study 28 of 73 May 2013
4.4 Butt Marking For the purpose of this study the CM test pieces (CM7) will be butt marked to a fixed butt length of 32 mm. 4.5 Conditioning The composite samples should 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 should 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 cigarettes with visible defects should be discarded.
4.3. Weight of the Test 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.
4.4. 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.
4.5. Smoking Plans The smoking plans will incorporate one product (CM7), shown as M in the smoking plans. These plans are designed to smoke the CM7 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 2-4)
CTR-RAC_2012 CM7 Collaborative Study 29 of 73 May 2013
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 number of cigarettes 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 ten ports, smoking three test pieces per port (Tables 5-7). 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. .
CTR-RAC_2012 CM7 Collaborative Study 30 of 73 May 2013
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 16-port Linear Machines for ISO smoking (5 test pieces per pad)
Day
Port number
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16
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 4: Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test articles per pad)
Day Run Test Piece
1 1 M
2 2 M
3 3 M
4 4 M
5 5 M
CTR-RAC_2012 CM7 Collaborative Study 31 of 73 May 2013
Table 5: 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 M
7 M M M M M
2 8 M M M M M
9 M M M M M
3 10 M M M M M
11 M M M M M
4 12 M M M M M
13 M M M M M
5 14 M M M M M
15 M M M M M
CTR-RAC_2012 CM7 Collaborative Study 32 of 73 May 2013
Table 6: Smoking Plan for 16-port Linear Machines for Intense smoking (3 test articles per pad)
Table 7: Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test articles per pad)
Day Run Test article
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
Day
Port number
Run 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16
1 6 M M M M M
7 M M M M M
2 8 M M M M M
9 M M M M M
3 10 M M M M M
11 M M M M M
4 12 M M M M M
13 M M M M M
5 14 M M M M M
15 M M M M M
5. 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
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 test
Type 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 ###.#
CTR-RAC_2012 CM7 Collaborative Study 34 of 73 May 2013
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. 6. STUDY TIMING and DATA SUBMISSION The smoking should be performed between July and August, 2012. 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 September 28, 2012. Data not received by September 3, 2012 will be excluded from the formal statistical analysis. 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 [email protected] Encl: Reporting format
CTR-RAC_2012 CM7 Collaborative Study 35 of 73 May 2013
APPENDIX 1 – CM7 SOURCE INFORMATION
Borgwaldt KC GmbH Cerulean
Spare Parts Department, Rockingham Drive Schnackenburgallee 15, Linford Wood East
D-22525 Hamburg Milton Keynes MK14 6LY
Germany, United Kingdom
Tel: +49 40 85 31 380 Tel: +44 1908 23 38 33
Fax: +49 40 850 56 00 e-mail: [email protected]
Fax: +44 1908 23 53 33 e-mail: [email protected]
CTR-RAC_2012 CM7 Collaborative Study 36 of 73 May 2013
APPENDIX C – Departures from Experimental Protocol No departures from the experimental protocol were reported.
CTR-RAC_2012 CM7 Collaborative Study 37 of 73 May 2013
APPENDIX D – RAW DATA SET
Raw data: CM7 - ISO Lab Code
Conditioned
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 Lab Code
Conditioned
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
958.7 16.24 1.42 1.248 13.58 12.98 8.55 960.4 17.22 1.31 1.326 14.58 12.54 9.03
978.2 15.71 1.51 1.261 12.94 12.58 8.75 956.1 16.74 0.99 1.252 14.50 12.77 8.89
961.8 16.88 1.59 1.307 13.99 13.28 8.55 952.5 16.60 0.88 1.253 14.47 13.20 8.80
966.4 16.34 1.47 1.264 13.61 13.39 8.63 949.7 16.26 - - - 12.49 8.65
968.6 16.97 1.74 1.311 13.92 13.25 8.90 956.5 17.29 1.51 1.320 14.46 12.93 8.94
955.9 15.38 1.75 1.187 12.44 13.25 7.79 940.2 15.92 1.38 1.273 13.27 12.10 7.83
954.0 15.82 1.86 1.199 12.76 13.17 7.90 945.0 15.05 1.08 1.142 12.83 11.93 7.45
956.8 15.87 1.88 1.196 12.79 13.40 7.87 951.1 15.37 1.18 1.235 12.96 12.22 7.75
954.9 16.06 1.90 1.206 12.96 13.24 7.85 957.7 15.76 1.13 1.138 13.50 11.36 7.85
947.4 15.67 1.85 1.181 12.64 13.22 7.71 957.4 15.24 1.05 1.115 13.07 11.76 7.65
953.8 16.64 1.36 1.258 14.02 12.89 8.30 942.8 15.63 1.43 1.198 13.00 11.54 7.80
955.4 16.13 1.21 1.236 13.68 12.74 8.26 948.4 16.49 1.58 1.215 13.70 12.10 8.35
953.8 16.22 1.29 1.240 13.69 12.93 8.26 962.7 16.40 1.53 1.243 13.63 11.99 8.88
956.5 16.39 1.22 1.260 13.91 12.51 8.31 967.9 17.41 2.03 1.233 14.15 12.46 8.78
954.8 16.31 1.28 1.257 13.77 12.44 8.34 958.6 15.41 1.55 1.198 12.66 12.00 6.93
955.0 15.81 1.72 1.180 12.91 12.70 8.05 956.1 15.79 1.93 1.244 12.62 13.16 8.15
953.0 15.46 1.62 1.170 12.67 12.58 7.93 943.8 16.09 1.81 1.280 13.00 12.91 8.02
957.0 16.04 1.81 1.207 13.02 13.05 8.03 957.4 16.52 1.82 1.295 13.41 13.11 8.24
957.0 15.83 1.92 1.152 12.76 12.97 7.99 947.0 16.24 1.98 1.241 13.02 13.11 8.16
954.0 15.99 1.77 1.184 13.04 12.97 7.88 950.4 16.74 2.23 1.281 13.23 13.18 8.07
958.0 16.60 1.45 1.262 13.89 13.16 8.87 951.2 16.42 2.48 1.201 12.75 13.80 7.88
963.0 16.95 1.47 1.289 14.20 13.50 8.87 960.1 16.00 2.02 1.154 12.82 13.33 7.87
961.0 16.60 1.52 1.259 13.82 13.25 8.86 962.3 16.24 2.03 1.189 13.02 13.58 8.01
954.0 16.85 1.43 1.265 14.15 13.14 8.72 954.4 16.37 1.97 1.170 13.24 13.34 8.00
964.0 16.90 1.56 1.249 14.10 13.26 8.82 960.3 16.22 2.18 1.154 12.89 13.80 7.90
950.4 17.73 1.87 1.296 14.56 13.48 8.31 961.8 15.96 2.18 1.193 12.59 13.40 8.12
960.1 17.11 1.87 1.265 13.97 12.88 8.48 953.8 15.65 1.86 1.186 12.60 13.15 8.07
960.2 17.64 2.03 1.315 14.30 13.42 8.50 958.4 15.64 1.95 1.153 12.53 13.03 8.43
952.1 17.59 1.98 1.306 14.31 13.14 8.48 962.2 15.59 1.92 1.141 12.53 13.41 8.18
950.3 17.65 2.16 1.298 14.19 13.39 8.45 956.5 15.56 1.89 1.184 12.49 13.06 8.17
961.5 17.28 1.48 1.246 14.55 12.54 8.73 962.9 16.59 2.24 1.216 13.13 13.53 8.89
958.8 17.05 1.49 1.232 14.33 13.22 8.76 956.0 16.99 2.13 1.215 13.65 13.48 8.53
959.2 17.49 1.50 1.265 14.73 13.13 8.96 954.4 16.81 1.91 1.216 13.68 13.34 8.39
973.8 17.62 1.74 1.240 14.65 13.28 9.19 954.1 17.07 2.32 1.210 13.54 13.90 8.48
962.3 17.26 1.60 1.239 14.41 12.95 8.83 951.6 16.86 2.13 1.188 13.54 13.66 8.56
946.7 15.89 2.20 1.111 12.57 12.19 8.36 953.7 16.57 2.18 1.204 13.19 12.82 8.34
946.4 16.06 2.20 1.147 12.70 12.81 8.49 953.0 16.69 2.18 1.228 13.28 12.83 8.49
947.2 16.23 2.20 1.135 12.89 12.17 8.27 951.1 16.29 2.01 1.209 13.07 13.08 8.27
947.6 15.93 2.06 1.102 12.76 12.41 8.32 951.3 15.88 2.06 1.182 12.64 12.60 8.20
949.6 16.31 2.15 1.148 13.02 12.26 8.26 963.4 15.83 2.09 1.185 12.56 12.68 8.22
959.6 16.08 2.05 1.299 12.73 12.60 8.26 951.6 16.14 2.15 1.182 12.81 13.20 8.50
969.4 16.30 2.15 1.268 12.88 13.20 8.09 956.5 16.23 2.10 1.178 12.95 13.26 8.22
968.6 16.48 2.11 1.277 13.10 13.10 8.03 964.1 16.32 2.09 1.175 13.06 12.86 8.37
961.3 16.09 2.09 1.246 12.76 12.70 8.10 952.8 16.15 2.04 1.184 12.93 13.28 8.22
966.7 16.13 2.05 1.260 12.82 12.90 8.24 954.5 16.15 2.11 1.184 12.86 13.22 8.28
962.0 16.36 2.01 1.243 13.11 12.90 8.05 955.0 15.76 1.26 1.240 13.26 12.27 8.28
954.0 15.82 2.07 1.147 12.60 12.86 7.83 967.0 15.75 1.06 1.213 13.48 12.12 8.45
950.0 16.47 2.15 1.195 13.13 12.95 7.99 951.0 15.20 1.12 1.233 12.85 11.61 8.10
960.0 15.94 2.15 1.164 12.63 12.93 7.97 955.0 15.58 1.00 1.208 13.37 11.94 8.28
952.0 16.37 2.06 1.231 13.08 13.16 8.05 959.0 14.90 1.14 1.245 12.52 11.66 8.18
960.0 16.26 2.04 1.162 13.06 13.19 7.96 948.3 16.60 1.63 1.227 13.75 11.84 8.55
958.0 16.38 1.90 1.154 13.33 12.95 7.84 954.8 16.80 1.67 1.247 13.88 12.35 8.77
954.0 16.28 2.23 1.142 12.91 13.00 7.75 959.6 16.69 1.65 1.263 13.78 11.96 8.56
954.0 16.29 2.13 1.188 12.97 13.06 7.90 956.4 17.24 1.81 1.260 14.17 12.74 8.76
956.0 16.68 2.44 1.170 13.07 13.36 7.97 961.7 16.66 1.64 1.259 13.76 12.01 8.72
957.8 16.81 1.98 1.280 13.55 12.30 8.50 952.3 16.51 2.25 1.243 13.02 13.00 8.25
956.9 16.35 1.58 1.233 13.54 12.10 8.33 951.5 16.08 2.17 1.181 12.73 12.70 8.13
951.7 15.98 1.60 1.203 13.18 12.00 8.08 960.5 16.23 2.08 1.187 12.96 13.00 8.32
952.5 16.21 1.48 1.215 13.52 12.10 8.15 959.7 16.12 2.02 1.186 12.91 13.00 8.28
957.0 15.78 1.48 1.210 13.09 11.90 8.34 955.1 16.13 1.99 1.199 12.94 12.90 8.17
959.2 16.44 2.10 1.220 13.12 12.60 8.30 956.1 16.27 2.34 1.215 12.72 13.88 8.10
957.6 16.39 2.00 1.220 13.17 13.10 8.30 955.7 16.38 1.99 1.238 13.15 13.67 8.16
955.0 16.46 2.20 1.230 13.03 12.80 8.20 959.5 16.00 1.90 1.220 12.88 13.74 8.18
959.8 16.42 1.67 1.230 13.52 12.60 8.20 963.7 16.03 1.86 1.201 12.97 13.85 8.16
952.0 16.73 2.46 1.240 13.03 12.70 8.20 969.9 16.53 1.96 1.247 13.32 13.82 8.14
959.1 16.22 1.95 1.231 13.04 13.63 8.51 943.5 15.80 1.14 1.240 13.42 11.47 8.17
958.6 16.44 2.06 1.223 13.16 13.64 8.64 948.6 16.46 1.16 1.290 14.01 12.01 8.44
955.9 16.26 2.05 1.217 12.99 13.49 8.41 946.3 16.58 1.23 1.320 14.03 11.82 8.23
953.2 16.40 2.03 1.233 13.14 13.89 8.48 943.8 15.89 1.15 1.280 13.46 11.84 8.10
956.0 16.50 1.95 1.245 13.31 13.77 8.56 944.0 16.84 1.41 1.340 14.09 12.02 8.30
955.5 15.82 1.86 1.204 12.76 13.08 8.30 958.8 15.82 1.88 1.159 12.78 13.10 8.88
953.1 15.88 1.67 1.214 13.00 13.24 8.11 969.0 15.62 1.61 1.104 12.91 12.70 8.93
955.1 15.77 1.71 1.227 12.83 12.94 8.27 970.0 15.68 1.73 1.094 12.86 12.90 8.91
953.5 15.90 1.91 1.246 12.74 13.38 8.15 968.9 15.56 1.68 1.114 12.77 13.10 8.73
955.0 15.86 1.73 1.230 12.90 13.30 8.26 971.3 15.52 1.83 1.142 12.55 12.90 8.87
952.3 15.89 1.99 1.222 12.68 13.37 8.16 966.6 16.24 1.30 1.180 13.75 12.29 9.20
957.0 16.13 2.10 1.228 12.80 13.62 8.27 968.6 14.96 0.76 1.119 13.08 11.73 9.43
959.0 15.96 2.08 1.205 12.67 13.59 8.24 967.3 15.00 1.02 1.119 12.86 11.50 9.25
947.6 15.48 1.99 1.202 12.29 13.10 8.15 969.9 15.98 1.17 1.191 13.62 12.89 9.20
949.8 15.47 1.73 1.218 12.52 13.21 8.05 970.2 14.47 0.83 1.139 12.49 11.82 9.05
968.5 16.94 2.00 1.263 13.67 13.47 8.84 955.7 14.62 1.78 1.047 11.79 11.30 8.17
948.9 16.51 1.94 1.235 13.33 12.90 8.39 955.0 14.87 1.86 1.055 11.95 11.50 8.30
962.9 16.48 1.93 1.251 13.29 12.76 8.71 955.8 14.84 1.81 1.047 11.98 11.60 8.16
960.4 16.59 1.83 1.272 13.49 13.15 8.68 954.2 14.59 1.76 1.064 11.77 11.30 8.15
954.7 16.77 1.91 1.280 13.58 13.11 8.55 955.8 14.59 1.74 1.074 11.77 11.00 8.27
959.4 16.04 1.68 1.213 13.15 12.89 8.38 953.3 17.48 1.68 1.211 14.59 15.50 8.80
962.9 16.94 1.73 1.253 13.96 13.01 8.68 954.4 17.95 2.15 1.209 14.59 15.79 8.83
956.6 16.83 1.89 1.248 13.69 13.07 8.55 958.7 17.67 1.90 1.204 14.57 16.17 8.95
962.4 16.61 1.61 1.235 13.77 13.31 8.78 955.6 17.49 1.55 1.191 14.74 16.31 8.63
958.0 16.69 2.00 1.250 13.44 13.41 8.75 956.3 18.15 1.96 1.226 14.96 15.86 8.88
960.6 16.06 2.24 1.230 12.59 13.06 8.07 948.5 16.60 1.55 1.298 13.76 12.21 8.43
963.1 15.71 2.31 1.190 12.21 13.20 7.93 951.8 16.18 1.41 1.340 13.43 12.47 8.25
957.5 15.97 2.09 1.230 12.65 13.04 8.21 947.8 16.25 1.28 1.310 13.67 12.57 8.13
956.0 16.01 1.91 1.220 12.88 12.89 8.07 942.1 15.98 1.39 1.295 13.29 12.30 8.25
955.3 15.77 2.19 1.210 12.37 12.83 8.19 946.6 16.40 1.35 1.325 13.72 12.53 8.20
964.0 15.82 2.06 1.103 12.66 13.70 8.28 954.3 17.38 2.02 1.345 14.01 12.88 8.90
966.8 16.44 2.25 1.203 12.99 13.93 8.42 952.2 16.20 1.86 1.225 13.12 12.00 8.40
973.0 16.33 2.08 1.234 13.02 13.96 8.48 954.2 17.03 1.65 1.353 14.02 12.50 8.83
974.3 16.43 2.26 0.863 13.31 14.10 8.46 943.8 16.70 1.81 1.295 13.60 12.08 8.50
975.9 16.30 2.26 1.224 12.82 13.96 8.43 953.6 16.85 1.78 1.318 13.75 12.75 8.85
964.3 16.67 1.37 1.050 14.26 13.30 8.48 960.0 15.64 1.89 1.180 12.57 13.90 8.11
969.4 16.47 1.44 1.051 13.98 13.14 8.45 955.0 15.88 2.04 1.160 12.68 13.58 8.07
965.2 15.42 1.26 0.992 13.16 12.69 8.20 967.0 15.82 1.83 1.160 12.83 12.95 8.10
962.0 15.92 1.29 1.031 13.60 13.01 8.33 965.0 15.97 2.20 1.170 12.60 13.16 8.10
961.3 15.89 1.27 1.051 13.58 12.78 8.23 966.0 15.95 2.03 1.180 12.74 13.24 8.07
946.9 15.96 1.71 1.218 13.03 13.20 8.25 961.0 16.34 2.20 1.180 12.96 12.80 8.46
955.4 16.04 1.80 1.188 13.06 13.20 8.34 963.0 15.93 2.05 1.170 12.71 12.35 8.42
956.8 16.45 1.95 1.204 13.30 13.60 8.28 966.0 16.00 1.87 1.180 12.95 12.50 8.31
957.5 15.88 2.05 1.180 12.65 13.40 8.31 961.0 16.40 2.23 1.180 12.99 12.76 8.32
950.7 15.73 2.15 1.210 12.37 12.90 8.15 969.0 15.84 1.89 1.180 12.77 12.32 8.47
962.9 16.58 1.57 1.250 13.76 - 8.59 954.1 16.06 1.64 1.260 13.16 12.30 8.18
962.0 16.91 1.64 1.293 13.97 - 8.76 960.6 16.26 1.24 1.270 13.75 12.20 8.21
957.9 16.66 1.62 1.262 13.78 - 8.63 955.1 16.00 1.63 1.280 13.09 13.30 8.19
959.5 16.97 1.69 1.298 13.98 - 8.57 956.2 16.62 1.56 1.260 13.80 13.00 8.18
963.3 16.45 1.52 1.246 13.68 - 8.71 957.9 16.41 1.48 1.290 13.64 12.80 8.21
951.5 16.14 1.44 1.176 13.52 12.81 8.15 947.4 16.38 1.46 1.273 13.64 13.37 8.30
956.0 16.23 1.47 1.205 13.56 12.91 8.35 947.3 15.70 1.46 1.247 12.99 12.33 8.35
953.5 16.53 1.49 1.251 13.78 12.88 8.45 940.7 15.77 1.19 1.237 13.34 12.11 8.43
951.0 16.23 1.39 1.210 13.63 12.59 8.50 948.0 16.13 1.66 1.217 13.25 12.91 8.13
950.0 16.23 1.40 1.173 13.66 12.50 8.03 949.2 15.94 1.87 1.269 12.79 12.62 8.33
949.5 16.59 2.12 1.206 13.27 13.39 7.85 983.5 16.85 1.38 1.218 14.25 12.74 8.72
964.0 16.17 1.99 1.134 13.04 13.23 8.21 965.6 16.80 1.39 1.191 14.22 12.63 8.79
959.5 16.96 2.19 1.210 13.56 13.74 8.26 966.5 16.50 1.60 1.191 13.71 13.29 8.58
960.0 16.63 2.15 1.174 13.31 13.61 8.04 981.7 17.15 1.54 1.214 14.39 13.24 8.89
956.0 16.85 2.11 1.202 13.54 13.79 8.14 975.8 17.08 1.49 1.184 14.40 12.61 8.76
972.8 15.95 1.55 1.165 13.24 11.68 8.73 953.7 15.30 0.96 1.399 12.93 12.77 8.60
978.3 16.38 1.75 1.143 13.48 12.03 9.68 956.9 15.81 0.99 1.278 13.54 13.70 8.55
978.9 17.33 1.53 1.223 14.58 12.73 8.95 954.9 15.94 1.34 1.264 13.33 13.71 8.59
984.8 16.15 1.58 1.213 13.36 12.15 8.95 958.2 15.43 0.81 1.280 13.34 12.64 8.27
969.7 16.83 1.53 1.245 14.06 12.15 8.73 951.7 15.51 0.96 1.386 13.16 11.73 8.50
956.5 16.22 1.29 1.208 13.71 12.57 8.67
951.5 16.24 1.34 1.171 13.73 12.64 8.40
953.9 15.47 1.17 1.162 13.14 11.91 8.85
952.6 15.19 1.62 1.159 12.41 11.70 8.69
944.8 14.65 0.93 1.105 12.61 11.16 8.41
44
46
47
39
40
41
42A
42B
43
34
35
36A
36B
37
29C
30
31
32
28A
28B
29A
29B
22
25A
25B
26
17
18A
18B
19
21
12A
12B
14A
14B
16
9B
10
10B
11B
11C
5
6
7
8A
8B
9A
1
2A
2B
3A
3B
4
CTR-RAC_2012 CM7 Collaborative Study 38 of 73 May 2013
Raw data: CM7 - Intense Lab Code
TPM
(mg/t.p.)
Water
(mg/t.p.)
Nicotine
(mg/t.p.)
NFDPM
(mg/t.p.)
CO
(mg/t.p)Puff count Lab Code
TPM
(mg/t.p.)
Water
(mg/t.p.)
Nicotine
(mg/t.p.)
NFDPM
(mg/t.p.)
CO
(mg/t.p)Puff count
45.77 12.60 2.659 30.51 24.41 11.79 43.23 9.98 2.616 30.64 23.90 12.30
46.15 13.21 2.620 30.32 24.79 12.16 43.26 10.11 2.555 30.60 23.69 12.43
45.74 13.23 2.766 29.75 24.70 11.87 42.82 10.13 2.509 30.18 23.67 12.34
46.80 13.52 2.676 30.60 25.07 12.02 43.47 - - - 23.94 12.63
47.84 14.49 2.715 30.64 25.26 12.18 41.74 9.80 2.544 29.39 23.23 12.28
38.14 9.26 2.447 26.43 25.04 11.27 41.55 8.19 2.335 31.03 23.29 11.32
39.02 9.89 2.449 26.67 25.47 11.42 42.01 7.57 2.349 32.09 23.74 11.30
37.99 9.45 2.376 26.16 24.98 11.06 42.49 8.78 2.348 31.36 23.41 11.36
38.01 9.30 2.387 26.32 24.92 11.08 43.31 8.76 2.401 32.15 23.58 11.63
38.72 9.51 2.442 26.76 25.49 11.10 45.29 10.47 2.477 32.34 25.49 12.22
42.49 11.28 2.559 28.65 24.49 11.69 46.20 13.08 2.451 30.67 24.22 12.27
42.09 11.64 2.490 27.96 24.18 11.44 45.18 12.53 2.438 30.21 23.59 12.01
41.85 11.21 2.505 28.13 24.10 11.49 44.63 12.68 2.414 29.53 23.58 12.17
41.70 11.07 2.477 28.15 23.44 11.38 45.60 10.50 2.501 32.60 25.12 12.30
42.52 11.83 2.494 28.20 24.52 11.51 44.32 10.85 2.565 30.90 24.95 12.64
37.75 8.70 2.360 26.69 24.31 12.18 38.56 8.65 2.624 27.29 25.79 11.48
38.42 8.62 2.432 27.37 23.86 12.26 37.71 7.77 2.560 27.38 25.27 11.46
37.74 8.62 2.377 26.74 24.67 11.89 38.41 8.55 2.579 27.28 24.67 11.73
38.04 8.55 2.393 27.10 24.60 12.10 38.37 8.94 2.566 26.87 25.09 11.47
38.01 8.41 2.373 27.23 24.46 11.71 38.47 9.44 2.520 26.51 25.03 11.45
44.30 10.80 2.578 30.92 25.17 12.22 - - - - - -
45.03 11.05 2.563 31.42 24.72 12.52 - - - - - -
45.33 11.97 2.581 30.78 24.85 12.28 - - - - - -
45.80 11.21 2.594 32.00 25.12 12.38 - - - - - -
44.93 11.64 2.595 30.70 24.64 12.22 - - - - - -
47.06 12.99 2.607 31.47 25.05 11.74 - - - - - -
47.78 13.92 2.605 31.26 25.95 11.71 - - - - - -
47.75 14.28 2.608 30.86 25.45 11.65 - - - - - -
47.95 14.63 2.661 30.66 25.30 11.68 - - - - - -
47.71 14.26 2.663 30.78 25.19 11.78 - - - - - -
46.26 12.03 2.513 31.71 24.74 12.29 - - - - - -
46.10 12.31 2.465 31.32 24.59 11.87 - - - - - -
48.07 12.53 2.537 33.00 25.56 12.15 - - - - - -
46.67 12.66 2.444 31.56 24.99 12.06 - - - - - -
47.42 13.63 2.476 31.31 25.62 12.56 - - - - - -
38.51 9.33 2.316 26.86 24.39 11.81 - - - - - -
39.15 9.25 2.375 27.53 24.31 11.96 - - - - - -
38.81 9.18 2.362 27.26 24.58 11.77 - - - - - -
38.27 9.07 2.397 26.81 24.01 12.37 - - - - - -
37.83 9.07 2.394 26.36 24.22 11.80 - - - - - -
- - - - - - 40.29 9.55 2.293 28.45 24.54 12.08
- - - - - - 40.11 9.38 2.245 28.48 24.75 11.93
- - - - - - 39.70 9.53 2.285 27.89 24.50 11.72
- - - - - - 39.55 9.70 2.251 27.59 24.66 11.92
- - - - - - 39.88 9.60 2.328 27.96 24.48 12.21
39.03 9.20 2.482 27.34 25.10 11.12 42.05 10.44 2.544 29.07 24.19 11.59
39.55 9.94 2.444 27.17 24.91 11.56 41.22 10.11 2.644 28.47 23.66 11.69
38.81 9.65 2.435 26.73 24.53 11.42 41.72 10.06 2.580 29.09 23.73 11.57
39.38 9.86 2.442 27.08 24.60 11.53 42.05 10.52 2.551 28.98 24.24 11.64
39.22 9.53 2.490 27.20 24.69 11.24 42.42 10.67 2.696 29.05 24.42 11.65
39.89 10.10 2.366 27.42 24.80 11.30 44.12 12.42 2.606 29.10 24.12 12.50
38.81 9.22 2.397 27.20 24.65 11.29 43.66 12.30 2.566 28.79 24.21 12.27
39.01 9.55 2.395 27.07 23.55 11.22 43.26 12.34 2.503 28.42 24.15 12.22
39.02 9.95 2.342 26.73 24.35 11.11 43.39 11.92 2.504 28.96 24.19 12.03
39.72 9.83 2.382 27.51 24.40 11.31 43.56 11.52 2.545 29.49 23.85 12.32
- - - - - - 39.16 9.57 2.362 27.22 25.15 11.80
- - - - - - 38.98 9.34 2.222 27.42 25.20 11.80
- - - - - - 38.95 9.16 2.318 27.47 25.15 11.74
- - - - - - 39.41 10.25 2.489 26.67 25.55 11.95
- - - - - - 38.20 9.65 2.352 26.20 24.95 11.65
- - - - - - 38.91 9.92 2.482 26.51 26.23 11.72
- - - - - - 39.03 9.91 2.479 26.65 26.12 11.45
- - - - - - 39.37 10.11 2.512 26.75 25.66 11.82
- - - - - - 39.81 9.99 2.525 27.30 26.73 11.41
- - - - - - 39.58 9.82 2.488 27.27 26.39 11.52
- - - - - - 44.69 6.61 1.592 36.49 24.33 11.49
- - - - - - 44.08 6.57 1.572 35.94 24.14 11.49
- - - - - - 43.62 6.38 1.612 35.64 22.63 11.72
- - - - - - 42.56 6.39 1.556 34.62 23.98 11.75
- - - - - - 43.49 6.72 1.632 35.14 23.69 11.69
- - - - - - - - - - - -
- - - - - - - - - - - -
- - - - - - - - - - - -
- - - - - - - - - - - -
- - - - - - - - - - - -
38.22 9.41 2.455 26.35 25.11 11.76 40.74 10.61 2.441 27.69 23.91 12.75
37.63 9.23 2.487 25.91 24.84 12.04 41.67 11.91 2.339 27.42 23.40 13.10
37.61 9.30 2.446 25.86 25.42 11.85 43.31 12.46 2.491 28.36 24.36 13.05
38.30 9.76 2.481 26.06 25.82 11.85 42.74 12.20 2.406 28.13 23.46 12.93
36.93 8.92 2.459 25.55 24.88 11.85 45.01 12.34 2.398 30.27 24.12 13.07
39.37 8.83 2.418 28.12 23.75 12.44 37.17 11.68 1.095 23.31 23.55 11.99
40.20 8.63 2.467 29.10 24.34 12.35 37.88 11.55 1.105 24.13 23.75 11.86
39.08 8.45 2.417 28.22 24.14 12.19 37.63 11.92 1.136 23.44 23.30 12.03
41.09 9.07 2.455 29.56 24.63 12.52 37.69 11.97 1.167 23.39 23.45 12.15
39.97 8.65 2.452 28.86 23.60 11.99 37.37 11.74 1.134 23.36 23.30 11.82
46.38 14.29 2.528 29.56 25.04 11.72 47.51 13.20 2.363 31.51 28.74 12.12
46.09 13.14 2.555 30.40 24.40 11.74 48.94 13.56 2.372 33.01 29.61 12.22
46.63 13.46 2.523 30.65 25.46 11.70 50.23 13.75 2.428 34.05 30.67 12.15
47.33 13.50 2.565 31.27 25.26 11.72 48.47 13.26 2.336 32.87 30.33 12.02
46.71 13.91 2.548 30.25 25.15 11.98 49.55 14.21 2.330 33.01 28.79 11.98
39.75 10.44 2.420 26.89 25.60 11.45 45.49 10.70 2.656 32.14 24.20 11.33
37.58 9.61 2.380 25.59 23.89 11.46 45.63 10.84 2.675 32.12 23.55 11.54
38.07 9.91 2.400 25.76 24.16 11.29 45.42 11.38 2.627 31.41 24.69 11.43
39.25 10.27 2.455 26.52 24.35 11.54 45.50 10.77 2.717 32.02 25.05 11.44
39.75 10.67 2.445 26.64 24.38 11.43 45.00 11.08 2.681 31.24 24.31 11.59
37.93 9.43 2.426 26.07 25.59 12.23 43.51 13.16 2.528 27.82 22.32 12.11
39.38 10.62 2.467 26.28 26.31 12.36 41.85 11.40 2.471 27.98 22.03 12.47
39.17 10.41 2.505 26.25 26.08 12.25 44.30 13.37 2.542 28.39 23.09 12.24
39.55 10.40 2.415 26.73 26.00 12.02 43.67 12.48 2.599 28.59 22.60 12.21
39.76 10.87 2.493 26.40 26.34 11.97 44.11 12.81 2.541 28.76 22.94 12.12
41.58 9.92 2.120 29.53 26.87 11.77 38.29 10.05 2.295 25.95 25.68 11.36
41.56 9.69 2.227 29.64 25.98 11.92 38.08 9.85 2.315 25.92 25.30 11.28
41.34 9.36 2.194 29.78 25.99 11.66 37.32 9.35 2.280 25.69 25.31 11.57
41.62 9.63 2.187 29.80 26.32 11.66 38.24 9.60 2.330 26.31 24.94 11.30
42.89 10.22 2.239 30.43 26.52 11.83 38.52 9.99 2.360 26.17 25.29 11.77
38.69 7.82 2.414 28.45 26.05 12.08 39.96 10.63 2.390 26.94 25.02 12.08
38.08 7.40 2.296 28.39 25.75 12.02 39.45 10.12 2.360 26.98 24.30 12.22
36.09 7.89 2.391 25.81 23.95 11.73 39.47 10.16 2.355 26.96 24.24 12.15
37.62 8.34 2.398 26.88 25.10 11.67 39.34 10.49 2.380 26.48 24.49 11.97
38.68 8.77 2.427 27.48 24.80 11.78 40.05 10.60 2.390 27.07 25.13 12.17
- - - - - - - - - - - -
- - - - - - - - - - - -
- - - - - - - - - - - -
- - - - - - - - - - - -
- - - - - - - - - - - -
43.47 12.64 2.516 28.32 24.75 11.72 43.44 12.51 2.624 28.30 25.42 11.84
43.93 13.42 2.498 28.01 24.86 11.59 41.16 11.31 2.490 27.36 24.50 11.90
42.72 12.03 2.533 28.15 24.60 11.66 41.71 12.22 2.478 27.01 24.47 11.44
42.87 11.80 2.441 28.63 24.30 11.60 41.82 11.33 2.457 28.03 25.11 11.54
43.24 12.11 2.433 28.70 24.66 11.41 42.85 11.86 2.541 28.45 25.53 11.67
39.58 9.18 2.410 27.99 24.71 11.13 44.19 9.83 2.342 32.02 23.90 12.16
39.84 9.70 2.329 27.82 25.08 11.50 45.73 10.86 2.425 32.44 24.50 12.09
40.53 10.41 2.416 27.70 25.27 11.63 43.17 10.86 2.427 29.89 22.98 12.05
39.52 9.22 2.369 27.92 25.52 11.35 43.73 10.70 2.288 30.74 23.31 12.06
39.90 9.96 2.445 27.49 25.26 11.61 45.70 11.51 2.362 31.82 24.50 12.41
43.66 11.60 2.225 29.84 23.03 12.13 43.10 11.22 2.499 29.37 24.23 11.22
44.13 12.31 2.314 29.51 23.53 12.77 45.78 13.12 2.653 30.01 25.21 11.63
45.38 11.55 2.531 31.30 23.76 12.62 46.08 12.38 2.524 31.17 25.82 11.54
44.75 11.31 2.294 31.15 23.52 12.41 46.17 13.07 2.651 30.45 25.78 11.83
44.31 12.37 2.519 29.42 23.70 12.66 42.45 11.47 2.784 28.20 24.49 11.75
- - - - - -
- - - - - -
- - - - - -
- - - - - -
- - - - - -
43
44
46
47
39
40
41
42A
42B
34
35
36A
36B
37
29B
29C
30
31
32
26
28A
28B
29A
21
22
25A
25B
16
17
18A
18B
19
11C
12A
12B
14A
14B
9A
9B
10
10B
11B
4
5
6
7
8A
8B
1
2A
2B
3A
3B
CTR-RAC_2012 CM7 Collaborative Study 39 of 73 May 2013
APPENDIX E – MANDEL’S GRAPH 1. WEIGHT
CTR-RAC_2012 CM7 Collaborative Study 40 of 73 May 2013
2. TPM
1
2A
2B
3A
3B 4 5 6 7
8A
8B
9A
9B 10
10B
11B
11C
12A
12B
14A
14B 16
17
18A
18B 19
21
22
25A
25B 26
28A
28B
29A
29B
29C 30
31
32
34
35
36A
36B 37
39
40
41
42A
42B 43
44
46
47
CM7_ISO
CM7_Intense
Mandel's test h
Labs
-4
-2
0
2
4
1
2A
2B
3A
3B 4 5 6 7
8A
8B
9A
9B 10
10B
11B
11C
12A
12B
14A
14B 16
17
18A
18B 19
21
22
25A
25B 26
28A
28B
29A
29B
29C 30
31
32
34
35
36A
36B 37
39
40
41
42A
42B 43
44
46
47
CM7_ISO
CM7_Intense
Mandel's test k
Labs
0
1
2
3
4
CTR-RAC_2012 CM7 Collaborative Study 41 of 73 May 2013
3. WATER
1
2A
2B
3A
3B 4 5 6 7
8A
8B
9A
9B 10
10B
11B
11C
12A
12B
14A
14B 16
17
18A
18B 19
21
22
25A
25B 26
28A
28B
29A
29B
29C 30
31
32
34
35
36A
36B 37
39
40
41
42A
42B 43
44
46
47
CM7_ISO
CM7_Intense
Mandel's test h
Labs
-4
-2
0
2
4
1
2A
2B
3A
3B 4 5 6 7
8A
8B
9A
9B 10
10B
11B
11C
12A
12B
14A
14B 16
17
18A
18B 19
21
22
25A
25B 26
28A
28B
29A
29B
29C 30
31
32
34
35
36A
36B 37
39
40
41
42A
42B 43
44
46
47
CM7_ISO
CM7_Intense
Mandel's test k
Labs
0
1
2
3
4
CTR-RAC_2012 CM7 Collaborative Study 42 of 73 May 2013
4. NICOTINE
1
2A
2B
3A
3B 4 5 6 7
8A
8B
9A
9B 10
10B
11B
11C
12A
12B
14A
14B 16
17
18A
18B 19
21
22
25A
25B 26
28A
28B
29A
29B
29C 30
31
32
34
35
36A
36B 37
39
40
41
42A
42B 43
44
46
47
CM7_ISO
CM7_Intense
Mandel's test h
Labs
-4
-2
0
2
4
1
2A
2B
3A
3B 4 5 6 7
8A
8B
9A
9B 10
10B
11B
11C
12A
12B
14A
14B 16
17
18A
18B 19
21
22
25A
25B 26
28A
28B
29A
29B
29C 30
31
32
34
35
36A
36B 37
39
40
41
42A
42B 43
44
46
47
CM7_ISO
CM7_Intense
Mandel's test k
Labs
0
1
2
3
4
CTR-RAC_2012 CM7 Collaborative Study 43 of 73 May 2013
5. NFDPM
1
2A
2B
3A
3B 4 5 6 7
8A
8B
9A
9B 10
10B
11B
11C
12A
12B
14A
14B 16
17
18A
18B 19
21
22
25A
25B 26
28A
28B
29A
29B
29C 30
31
32
34
35
36A
36B 37
39
40
41
42A
42B 43
44
46
47
CM7_ISO
CM7_Intense
Mandel's test h
Labs
-4
-2
0
2
4
1
2A
2B
3A
3B 4 5 6 7
8A
8B
9A
9B 10
10B
11B
11C
12A
12B
14A
14B 16
17
18A
18B 19
21
22
25A
25B 26
28A
28B
29A
29B
29C 30
31
32
34
35
36A
36B 37
39
40
41
42A
42B 43
44
46
47
CM7_ISO
CM7_Intense
Mandel's test k
Labs
0
1
2
3
4
CTR-RAC_2012 CM7 Collaborative Study 44 of 73 May 2013
6. CO
1
2A
2B
3A
3B 4 5 6 7
8A
8B
9A
9B 10
10B
11B
11C
12A
12B
14A
14B 16
17
18A
18B 19
21
22
25A
25B 26
28A
28B
29A
29B
29C 30
31
32
34
35
36A
36B 37
39
40
41
42A
42B 43
44
46
47
CM7_ISO
CM7_Intense
Mandel's test h
Labs
-4
-2
0
2
4
1
2A
2B
3A
3B 4 5 6 7
8A
8B
9A
9B 10
10B
11B
11C
12A
12B
14A
14B 16
17
18A
18B 19
21
22
25A
25B 26
28A
28B
29A
29B
29C 30
31
32
34
35
36A
36B 37
39
40
41
42A
42B 43
44
46
47
CM7_ISO
CM7_Intense
Mandel's test k
Labs
0
1
2
3
4
CTR-RAC_2012 CM7 Collaborative Study 45 of 73 May 2013
7. PUFF
1
2A
2B
3A
3B 4 5 6 7
8A
8B
9A
9B 10
10B
11B
11C
12A
12B
14A
14B 16
17
18A
18B 19
21
22
25A
25B 26
28A
28B
29A
29B
29C 30
31
32
34
35
36A
36B 37
39
40
41
42A
42B 43
44
46
47
CM7_ISO
CM7_Intense
Mandel's test h
Labs
-4
-2
0
2
4
1
2A
2B
3A
3B 4 5 6 7
8A
8B
9A
9B 10
10B
11B
11C
12A
12B
14A
14B 16
17
18A
18B 19
21
22
25A
25B 26
28A
28B
29A
29B
29C 30
31
32
34
35
36A
36B 37
39
40
41
42A
42B 43
44
46
47
CM7_ISO
CM7_Intense
Mandel's test k
Labs
0
1
2
3
4
CTR-RAC_2012 CM7 Collaborative Study 46 of 73 May 2013
APPENDIX F – 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
CTR-RAC_2012 CM7 Collaborative Study 47 of 73 May 2013
APPENDIX G – LINEAR – ROTARY COMPARISONS
1. TPM
CM7 ISO
TP
M (
mg/t
.p.)
789
10111213141516171819202122232425
All
Lin
ear
Rota
ry
CM7 Intense
TP
M (
mg/t
.p.)
33343536373839404142434445464748495051
All
Lin
ear
Rota
ry
Index
1
R r
Index
1
R r
2. WATER
CM7 ISO
WA
TE
R (
mg/t
.p.)
-2
-1
0
1
2
3
4
5
6
All
Lin
ear
Rota
ry
CM7 Intense
WA
TE
R (
mg/t
.p.)
7
8
9
10
11
12
13
14
15
All
Lin
ear
Rota
ry
Index
1
R r
Index
1
R r
3. NICOTINE
CM7 ISO
NIC
OT
INE
(m
g/t
.p.)
1.0
1.1
1.2
1.3
1.4
1.5
1.6
1.7
1.8
1.9
2.0
All
Lin
ear
Rota
ry
CM7 Intense
NIC
OT
INE
(m
g/t
.p.)
2.0
2.1
2.2
2.3
2.4
2.5
2.6
2.7
2.8
2.9
3.0
All
Lin
ear
Rota
ry
Index
1
R r
Index
1
R r
CTR-RAC_2012 CM7 Collaborative Study 48 of 73 May 2013
4. NFDPM
CM7 ISO
NF
DP
M (
mg/t
.p.)
7
8
9
10
11
12
13
14
15
16
17
18
19
All
Lin
ear
Rota
ry
CM7 Intense
NF
DP
M (
mg/t
.p.)
23
24
25
26
27
28
29
30
31
32
33
34
35
All
Lin
ear
Rota
ry
Index
1
R r
Index
1
R r
5. CO
CM7 ISO
CO
(m
g/t
.p.)
11.0
11.5
12.0
12.5
13.0
13.5
14.0
14.5
15.0
All
Lin
ear
Rota
ry
CM7 Intense
CO
(m
g/t
.p.)
23.0
23.5
24.0
24.5
25.0
25.5
26.0
26.5
27.0A
ll
Lin
ear
Rota
ry
Index
1
R r
Index
1
R r
6. PUFF CM7 ISO
PU
FF
(/t
.p.)
7.0
7.5
8.0
8.5
9.0
All
Lin
ear
Rota
ry
CM7 Intense
PU
FF
(/t
.p.)
11.0
11.5
12.0
12.5
13.0
All
Lin
ear
Rota
ry
1
R r
1
R r
CTR-RAC_2012 CM7 Collaborative Study 49 of 73 May 2013
APPENDIX H – ROTARY SMOKING MACHINES r&R estimation for Rotary smoking machines under ISO and Intense smoking regime
Smoking
RegimeParameter
Nbr of
LabsMean
Straggling
LabsNo data
sr r sR R C G/G2
TPM 27 16.16 0.22 0.63 0.37 1.03 37
WATER 28 1.99 0.14 0.38 0.20 0.57 9B, 36A, 43
NIC 27 1.197 0.019 0.054 0.050 0.142 14A 8A, 36A, 37
NFDPM 28 12.92 0.21 0.58 0.38 1.07 12B, 37
CO 27 13.15 0.22 0.62 0.43 1.20 37 43
PUFF 28 8.23 0.10 0.28 0.25 0.70 11C, 36A
TPM 18 38.81 0.56 1.57 0.93 2.63
WATER 18 9.59 0.35 0.99 0.89 2.51
NIC 16 2.413 0.032 0.091 0.076 0.214 32 37
NFDPM 16 26.99 0.37 1.05 0.81 2.31 16 37 11C, 29C
CO 18 24.87 0.40 1.12 0.76 2.15 16
PUFF 18 11.73 0.17 0.48 0.37 1.04
Repeatability Reproducibility Outlying Labs
ISO
Intense
1. ISO smoking regime
Figure 1: CM7 Individual observations of mainstream “ISO” conditioned WEIGHT
WEIGHT_Rotary_ CM7_ISO
Labs
WE
IGH
T (
mg
/t.p
.)
2A
3A 6 7
8A
8B
9B 10
10B
11B
11C
12B
14A 16
18B 26
28A
28B
29A
29B
29C 32
34
36A 37
42A
42B 43
935
940
945
950
955
960
965
970
975
980
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+++++++++++++++++++++++++
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+++
+
+
+++
+
+
+++
CTR-RAC_2012 CM7 Collaborative Study 50 of 73 May 2013
Figure 2: CM7 Individual observations of mainstream “ISO” TPM
TPM_Rotary_ CM7_ISO
Labs
TP
M (
mg
/t.p
.)
2A
3A 6 7
8A
8B
9B 10
10B
11B
11C
12B
14A 16
18B 26
28A
28B
29A
29B
29C 32
34
36A 37
42A
42B 43
14.4
14.6
14.8
15.0
15.2
15.4
15.6
15.8
16.0
16.2
16.4
16.6
16.8
17.0
17.2
17.4
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++ +
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G_out_l
Figure 3: CM7 Individual observations of mainstream “ISO” WATER
WATER_Rotary_ CM7_ISO
Labs
WA
TE
R (
mg
/t.p
.)
2A
3A 6 7
8A
8B
9B 10
10B
11B
11C
12B
14A 16
18B 26
28A
28B
29A
29B
29C 32
34
36A 37
42A
42B 43
1.2
1.3
1.4
1.5
1.6
1.7
1.8
1.9
2.0
2.1
2.2
2.3
2.4
2.5
2.6
2.7
+
++++
+
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+
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+
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CTR-RAC_2012 CM7 Collaborative Study 51 of 73 May 2013
Figure 4: CM7 Individual observations of mainstream “ISO” Nicotine
NIC_Rotary_ CM7_ISO
Labs
NIC
(m
g/t
.p.)
2A
3A 6 7
8A
8B
9B 10
10B
11B
11C
12B
14A 16
18B 26
28A
28B
29A
29B
29C 32
34
36A 37
42A
42B 43
0.85
0.90
0.95
1.00
1.05
1.10
1.15
1.20
1.25
1.30
1.35
1.40
++++
+++++
+++++
+++++
+++++
+ ++
+
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+++++
+++++
+++++
+++++
++
+++++++++++++++++++++++++
+++++++++++++++++++++++++
+++++
+++++
+++++
+++++
+++++ ++
+++++
+++++
+++++
+++++
+++
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+++++
+++++
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++++
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+
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+
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+
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+
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++ +++++++++++++++++++++++++
+
++++
+
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+
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+
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+
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+
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+
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+
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+++++
+++++
+++++
+++++
+++++++++++++++++++++++++ +
++++++++++++++++++++++++
++++
+
++++
+
++++
+
++++
+
++++
+
C-out
Figure 5: CM7 Individual observations of mainstream “ISO” NFDPM
NFDPM_Rotary_ CM7_ISO
Labs
NF
DP
M (
mg
/t.p
.)
2A
3A 6 7
8A
8B
9B 10
10B
11B
11C
12B
14A 16
18B 26
28A
28B
29A
29B
29C 32
34
36A 37
42A
42B 43
11.6
11.8
12.0
12.2
12.4
12.6
12.8
13.0
13.2
13.4
13.6
13.8
14.0
14.2
+
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CTR-RAC_2012 CM7 Collaborative Study 52 of 73 May 2013
Figure 6: CM7 Individual observations of mainstream “ISO” CO
CO_Rotary_ CM7_ISO
Labs
CO
(m
g/t
.p.)
2A
3A 6 7
8A
8B
9B 10
10B
11B
11C
12B
14A 16
18B 26
28A
28B
29A
29B
29C 32
34
36A 37
42A
42B 43
11.0
11.5
12.0
12.5
13.0
13.5
14.0
14.5
++
+
++++
+
++++
+
++++
+
++++
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+++
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+ ++++
+
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+
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+
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+
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+ +
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G_out_l
Figure 7: CM7 Individual observations of mainstream “ISO” PUFF Count
PUFF_Rotary_ CM7_ISO
Labs
PU
FF
(/t
.p.)
2A
3A 6 7
8A
8B
9B 10
10B
11B
11C
12B
14A 16
18B 26
28A
28B
29A
29B
29C 32
34
36A 37
42A
42B 43
7.4
7.6
7.8
8.0
8.2
8.4
8.6
8.8
9.0
+
+++
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+
+++++++++++++++++++++++++
+++
+
++++
+
++++
+
++++
+
++++
+
+
+
+
++
+
+
+
++
+
+
+
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+
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+
+
+
++
+
+++++++++++++++++++++++++
++
++
+++
++
+++
++
+++
++
+++
++
+
+++++++++++++++++++++++++
CTR-RAC_2012 CM7 Collaborative Study 53 of 73 May 2013
2. Intense smoking regime
Figure 8: CM7 Individual observations of mainstream “Intense” TPM
TPM_Rotary_ CM7_Intense
Labs
TP
M (
mg
/t.p
.)
2A
3A 6 7*
8A
8B
9B
*
10*
10B
*
11B
11C
12B
14A 16
18B 26
28A
*
28B
*
29A
*
29B
*
29C 32
34
36A
*
37
42A
42B
43*
35.5
36.0
36.5
37.0
37.5
38.0
38.5
39.0
39.5
40.0
40.5
41.0
41.5
42.0
+
+
++
+
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+
+
+++
+
+
+
+
+++
++
+++
++
+++
++
+++
++
+++
+
Figure 9: CM7 Individual observations of mainstream “Intense” WATER
WATER_Rotary_ CM7_Intense
Labs
WA
TE
R (
mg
/t.p
.)
2A
3A 6 7*
8A
8B
9B
*
10*
10B
*
11B
11C
12B
14A 16
18B 26
28A
*
28B
*
29A
*
29B
*
29C 32
34
36A
*
37
42A
42B
43*
6.5
7.0
7.5
8.0
8.5
9.0
9.5
10.0
10.5
11.0
11.5
12.0
12.5
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+++++
+++++
+++++
+++++
+++++
+++++
+++++
+++++
+++++
+++++
+
+
++
+
+
+
++
+
+
+
++
+
+
+
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+
++
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++
+
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++
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+ +++
+
++++
+
++++
+
++++
+
++++
+
+
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++++++++++++++++++++++++++ +
++
+
++++
+
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+
++++
+
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+
+
+++++++++++++++++++++++++
++
+++++
+++++
+++++
+++++
+++
++
+
+
+++
+
+
+++
+
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+++
+
+
+++
+
+
+
+
++
+++
++
+++
++
+++
++
+++
++
++
CTR-RAC_2012 CM7 Collaborative Study 54 of 73 May 2013
Figure 10: CM7 Individual observations of mainstream “Intense” Nicotine
NIC_Rotary_ CM7_Intense
Labs
NIC
(m
g/t
.p.)
2A
3A 6 7*
8A
8B
9B
*
10*
10B
*
11B
11C
12B
14A 16
18B 26
28A
*
28B
*
29A
*
29B
*
29C 32
34
36A
*
37
42A
42B
43*
1.0
1.2
1.4
1.6
1.8
2.0
2.2
2.4
2.6
2.8
++
+++++
+++++
+++++
+++++
+++
+
+++++
+++++
+++++
+++++
++++
+++++
+++++
+++++
+++++
+++++
+++++++++++++++++++++++++
+++++++++++++++++++++++++
+++++++++++++++++++++++++
+++++++++++++++++++++++++
+++++++++++++++++++++++++ +
++
+
++++
+
++++
+
++++
+
++++
+
+
+
+
++++
+
++++
+
++++
+
++++
+
+++ +
+
++
++
+
++
++
+
++
++
+
++
++
+
++
+
+++++
+++++
+++++
+++++
+++++
++++
+++++
+++++
+++++
+++++
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
+
+++++++++++++++++++++++++
+++++++++++++++++++++++++
+++++++++++++++++++++++++
+++++++++++++++++++++++++
C-out
G_out_l
Figure 11: CM7 Individual observations of mainstream “Intense” NFDPM
NFDPM_Rotary_ CM7_Intense
Labs
NF
DP
M (
mg
/t.p
.)
2A
3A 6 7*
8A
8B
9B
*
10*
10B
*
11B
11C
12B
14A 16
18B 26
28A
*
28B
*
29A
*
29B
*
29C 32
34
36A
*
37
42A
42B
43*
23.0
23.5
24.0
24.5
25.0
25.5
26.0
26.5
27.0
27.5
28.0
28.5
29.0
29.5
30.0
++
++
+
++
++
+
++
++
+
++
++
+
++
++
+ +
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
++
+
++++
+
++++
+
++++
+
++++
+
++
+++
+
++++
+
++++
+
++++
+
++++
+
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
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+
++
+++
++
+++
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+++
++
+++
++
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++++
+
++++
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++++
+
++++
+
++++
++++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
++
+
+
+
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C-out
G_out_l
CTR-RAC_2012 CM7 Collaborative Study 55 of 73 May 2013
Figure 12: CM7 Individual observations of mainstream “Intense” CO
CO_Rotary_ CM7_Intense
Labs
CO
(m
g/t
.p.)
2A
3A 6 7*
8A
8B
9B
*
10*
10B
*
11B
11C
12B
14A 16
18B 26
28A
*
28B
*
29A
*
29B
*
29C 32
34
36A
*
37
42A
42B
43*
22.5
23.0
23.5
24.0
24.5
25.0
25.5
26.0
26.5
27.0
27.5
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Figure 13: CM7 Individual observations of mainstream “Intense” PUFF Count
PUFF_Rotary_ CM7_Intense
Labs
PU
FF
(/t
.p.)
2A
3A 6 7*
8A
8B
9B
*
10*
10B
*
11B
11C
12B
14A 16
18B 26
28A
*
28B
*
29A
*
29B
*
29C 32
34
36A
*
37
42A
42B
43*
10.4
10.6
10.8
11.0
11.2
11.4
11.6
11.8
12.0
12.2
12.4
12.6
12.8
13.0
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CTR-RAC_2012 CM7 Collaborative Study 56 of 73 May 2013
APPENDIX I – LINEAR SMOKING MACHINES r&R estimation for Linear smoking machines under ISO and Intense smoking regime
Smoking
RegimeParameter
Nbr of
LabsMean
Straggling
LabsNo data
sr r sR R C G/G2
TPM 25 16.41 0.41 1.17 0.74 2.08
WATER 25 1.46 0.16 0.44 0.30 0.84
NIC 24 1.243 0.033 0.093 0.056 0.158 14B 25A
NFDPM 25 13.71 0.34 0.95 0.54 1.54
CO 22 12.52 0.33 0.94 0.57 1.62 47 39 17
PUFF 23 8.53 0.14 0.40 0.34 0.97 19, 25B
TPM 22 44.39 0.89 2.53 2.14 6.05 47
WATER 22 11.56 0.61 1.73 1.82 5.16 25A, 35
NIC 19 2.502 0.047 0.133 0.127 0.361 19, 47 35
NFDPM 22 30.37 0.69 1.95 1.93 5.46 35, 39
CO 21 24.40 0.49 1.39 0.92 2.61 39
PUFF 21 11.99 0.16 0.45 0.42 1.20 25A
ISO
Intense
Repeatability Reproducibility Outlying Labs
1. ISO smoking regime
Figure 1: CM7 Individual observations of mainstream “ISO” conditioned WEIGHT
WEIGHT_Linear_ CM7_ISO
Labs
WE
IGH
T (
mg
/t.p
.)
1
2B
3B 4 5
9A
12A
14B 17
18A 19
21
22
25A
25B 30
31
35
36B 39
40
41
44
46
47
925
930
935
940
945
950
955
960
965
970
975
980
985
990
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CTR-RAC_2012 CM7 Collaborative Study 57 of 73 May 2013
Figure 2: CM7 Individual observations of mainstream “ISO” TPM
TPM_Linear_ CM7_ISO
Labs
TP
M (
mg
/t.p
.)
1
2B
3B 4 5
9A
12A
14B 17
18A 19
21
22
25A
25B 30
31
35
36B 39
40
41
44
46
47
14.0
14.5
15.0
15.5
16.0
16.5
17.0
17.5
18.0
18.5
19.0
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Figure 3: CM7 Individual observations of mainstream “ISO” WATER
WATER_Linear_ CM7_ISO
Labs
WA
TE
R (
mg
/t.p
.)
1
2B
3B 4 5
9A
12A
14B 17
18A 19
21
22
25A
25B 30
31
35
36B 39
40
41
44
46
47
0.4
0.6
0.8
1.0
1.2
1.4
1.6
1.8
2.0
2.2
2.4
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CTR-RAC_2012 CM7 Collaborative Study 58 of 73 May 2013
Figure 4: CM7 Individual observations of mainstream “ISO” Nicotine
NIC_Linear_ CM7_ISO
Labs
NIC
(m
g/t
.p.)
1
2B
3B 4 5
9A
12A
14B 17
18A 19
21
22
25A
25B 30
31
35
36B 39
40
41
44
46
47
0.95
1.00
1.05
1.10
1.15
1.20
1.25
1.30
1.35
1.40
1.45
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+++
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+++
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+++
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++++
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++++
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++++
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++++
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++++
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+
++++
+++++
+++++
+++++
+++++
+
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++
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+
+
++
+
+
+
+++
++
+++
++
+++
++
+++
++
+++
+
G_out_l
Figure 5: CM7 Individual observations of mainstream “ISO” NFDPM
NFDPM_Linear_ CM7_ISO
Labs
NF
DP
M (
mg
/t.p
.)
1
2B
3B 4 5
9A
12A
14B 17
18A 19
21
22
25A
25B 30
31
35
36B 39
40
41
44
46
47
12.0
12.5
13.0
13.5
14.0
14.5
15.0
15.5
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
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+
+
+
++
++
+
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+
++
+
+
+
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+
+
+
++
+
+
+
++
+
++
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
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+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
++
++
+
++
++
+
++
++
+
++
++
+
++
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++
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+
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+
++
++
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++
++
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++
++
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++
++
+
++
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+
+
+
+
+
+
+
+
+
+
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++++++++++++++++++++
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
++
++
+
+
+
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+
+
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++
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++
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+++
+
++++
+
++++
+
++++
+
++++
+
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+++
+
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+
+
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+
++
+
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+
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++
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+
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+
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++
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+
++
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+
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++
+
+
+
++
+
+
+
++
+
+
+
++
+
CTR-RAC_2012 CM7 Collaborative Study 59 of 73 May 2013
Figure 6: CM7 Individual observations of mainstream “ISO” CO
CO_Linear_ CM7_ISO
Labs
CO
(m
g/t
.p.)
1
2B
3B 4 5
9A
12A
14B
17*
18A 19
21
22
25A
25B 30
31
35
36B 39
40
41
44
46
47
10.5
11.0
11.5
12.0
12.5
13.0
13.5
14.0
14.5
15.0
15.5
16.0
16.5
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+++
++
+++
++
+++
++
+++
++
+++
++
+
+
++++
+
++++
+
++++
+
++++
+
+++
+
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+++++
+++++
+++++
+++++
+++++
+++
++
+++
++
+++
++
+++
++
+++
++
++
+
++
++
+
++
++
+
++
++
+
++
++
+
++ +
++
++
+++
++
+++
++
+++
++
+++
++
+
+
+
++
+
+
+
++
+
+
+
++
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+
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++
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+
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++
++
++
+
++
++
+
++
++
+
++
++
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++
++
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++
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+
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++
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+
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++
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++
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+
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++
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++
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+
+
++
+
+
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+
++
+
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+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
+
+
++++
+
++++
+
++++
+
++++
+
++++
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
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+
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++
+
++
++
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+
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+
+
+
++
+
+
+
++
+
+
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+++
++
+++
++
+++
++
+++
++
+++
++
++
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
C-out
G_out_h
Figure 7: CM7 Individual observations of mainstream “ISO” PUFF Count
PUFF_Linear_ CM7_ISO
Labs
PU
FF
(/t
.p.)
1
2B
3B 4 5
9A
12A
14B 17
18A 19
21
22
25A
25B 30
31
35
36B 39
40
41
44
46
47
6.8
7.0
7.2
7.4
7.6
7.8
8.0
8.2
8.4
8.6
8.8
9.0
9.2
9.4
9.6
9.8
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+++++++++++++++++++++++++
+++
+++++
+++++
+++++
+++++
++
+
++++
+
++++
+
++++
+
++++
+
++++
++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+ +
+
+
++
+
+
+
++
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+
++
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++
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+
+
++
++
+
++
++
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++
++
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++
++
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++
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++
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+
++
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+
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++
+
+
+
++
+
+
+
++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+
++
++
+
++
++
+
++
++
+
++
++
+
++
++
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
++
+
++
++
+
++
++
+
++
++
+
++
++
+
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
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++
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+
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++
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+
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++
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++
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+++
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+++
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+++
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+++
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++
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++
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+
+
+
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+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
+
+++
+
++++
+
++++
+
++++
+
++++
+
+
++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+
+++
+
++++
+
++++
+
++++
+
++++
+
+
C-out
C-out
CTR-RAC_2012 CM7 Collaborative Study 60 of 73 May 2013
2. Intense smoking regime
Figure 8: CM7 Individual observations of mainstream “Intense” TPM
TPM_Linear_ CM7_Intense
Labs
TP
M (
mg
/t.p
.)
1
2B
3B 4 5
9A
*
12A
14B
17*
18A 19
21*
22
25A
25B 30
31
35
36B 39
40
41
44
46
47
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
++++
+++++
+++++
+++++
+++++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
++++
+
++++
+
++++
+
++++
+
++++
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
+++
+
++++
+
++++
+
++++
+
++++
+
+
++++
+
++++
+
++++
+
++++
+
++++
+++
+++++
+++++
+++++
+++++
+++
++
+
++
++
+
++
++
+
++
++
+
++
++
+
++
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+ +++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
+++++
+++++
+++++
+++++
++++
+++++++++++++++++++++++++
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+++++++++++++++++++++++++
+
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
++
+
+++
++
+++
++
+++
++
+++
++
+++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
Figure 9: CM7 Individual observations of mainstream “Intense” WATER
WATER_Linear_ CM7_Intense
Labs
WA
TE
R (
mg
/t.p
.)
1
2B
3B 4 5
9A
*
12A
14B
17*
18A 19
21*
22
25A
25B 30
31
35
36B 39
40
41
44
46
47
5
6
7
8
9
10
11
12
13
14
15
16
17
18
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
++++
+
++++
+
++++
+
++++
+
++++
+
++
+
++
++
+
++
++
+
++
++
+
++
++
+
++
+
++++
+
++++
+
++++
+
++++
+
++++
++++
+
++++
+
++++
+
++++
+
++++
+
+
+++++
+++++
+++++
+++++
++++
++++
+++++
+++++
+++++
+++++
+
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
++++++++++++++++++++
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
++
++
+
++
++
+
++
++
+
++
++
+
++
++
+++++++++++++++++++++++++
+++++
+++++
+++++
+++++
+++++
+++++++++++++++++++++++++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
++++
+
++++
+
++++
+
++++
+
++++
+
++
+
++++
+
++++
+
++++
+
++++
+
++
+
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
++
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
+
CTR-RAC_2012 CM7 Collaborative Study 61 of 73 May 2013
Figure 10: CM7 Individual observations of mainstream “Intense” Nicotine
NIC_Linear_ CM7_Intense
Labs
NIC
(m
g/t
.p.)
1
2B
3B 4 5
9A
*
12A
14B
17*
18A 19
21*
22
25A
25B 30
31
35
36B 39
40
41
44
46
47
1.5
1.6
1.7
1.8
1.9
2.0
2.1
2.2
2.3
2.4
2.5
2.6
2.7
2.8
2.9
++
+
++++
+
++++
+
++++
+
++++
+
++
+
++++
+
++++
+
++++
+
++++
+
++++
+++++++++++++++++++++++++ +++
++
+++++
+++++
+++++
+++++
++
+
++++
+
++++
+
++++
+
++++
+
++
+++++++++++++++++++++++++
+
++++
+
++++
+
++++
+
++++
+
++++
+++
++
+++
++
+++
++
+++
++
+++
++
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+++
+
+++
+
+++
+
+++
+
+++
++++
+
++++
+
++++
+
++++
+
++++
++++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+ +
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
++
+++
++
+++
++
+++
++
+++
++
+++
++++
+++++
+++++
+++++
+++++
+
+
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
++++
+
++++
+
++++
+
++++
+
++++
+
++
+++
+++++
+++++
+++++
+++++
++
+
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C-out
C-out
G_out_l
Figure 11: CM7 Individual observations of mainstream “Intense” NFDPM
NFDPM_Linear_ CM7_Intense
Labs
NF
DP
M (
mg
/t.p
.)
1
2B
3B 4 5
9A
*
12A
14B
17*
18A 19
21*
22
25A
25B 30
31
35
36B 39
40
41
44
46
47
24
25
26
27
28
29
30
31
32
33
34
35
36
37
++
+
++++
+
++++
+
++++
+
++++
+
++
+
+++++
+++++
+++++
+++++
++++
++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+
+++++
+++++
+++++
+++++
+++++
++
+
++++
+
++++
+
++++
+
++++
+
++
+
++
+
+
+
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+
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+
+
+
++
+
+
+
++
+
+
++++
+
++++
+
++++
+
++++
+
++++
+
+++++++++++++++++++++++++
++
++
+++
++
+++
++
+++
++
+++
++
+
+++
+
+++
+
+++
+
+++
+
+++
+
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+
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+++
+
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+++
+
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+++
+
+
+
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+
++++
+
++++
+
++++
+
++++
+
+++ +++
+
++++
+
++++
+
++++
+
++++
+
+
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++
+
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++
+
+
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+++++
+++++
+++++
+++++
+++++
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++
+++
++
+++
++
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++
+++
++
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+
+
+
CTR-RAC_2012 CM7 Collaborative Study 62 of 73 May 2013
Figure 12: CM7 Individual observations of mainstream “Intense” CO
CO_Linear_ CM7_Intense
Labs
CO
(m
g/t
.p.)
1
2B
3B 4 5
9A
*
12A
14B
17*
18A 19
21*
22
25A
25B 30
31
35
36B 39
40
41
44
46
47
21
22
23
24
25
26
27
28
29
30
31
+++++
+++++
+++++
+++++
+++++
+++
+
++++
+
++++
+
++++
+
++++
+
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+
++++
+
++++
+
++++
+
++++
+
+++
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
+
+
++++
+
++++
+
++++
+
++++
+
+++
+
+++++
+++++
+++++
+++++
++++
+++++++++++++++++++++++++
+
++++
+
++++
+
++++
+
++++
+
++++
++++
+
++++
+
++++
+
++++
+
++++
+ +
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
++
++
+
++
++
+
++
++
+
++
++
+
++
++
+
++
+++
++
+++
++
+++
++
+++
++
++
+++++++++++++++++++++++++
++
+
++
++
+
++
++
+
++
++
+
++
++
+
++
+
+
+
+
++
+
+
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+
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+
+
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++
+
++
++
+
++
++
+
++
++
+
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+
+
+
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++
+
++
++
+
++
++
+
++
++
+
++
+
++
+
++
++
+
++
++
+
++
++
+
++
++
+
++
+
++
+
++
++
+
++
++
+
++
++
+
++
++
+
+
+
+
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+
+
+
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+
+
+
++
+
+
+
++
+
+
+
++
++
+
++
++
+
++
++
+
++
++
+
++
++
+
++
+
G_out_h
Figure 13: CM7 Individual observations of mainstream “Intense” PUFF Count
PUFF_Linear_ CM7_Intense
Labs
PU
FF
(/t
.p.)
1
2B
3B 4 5
9A
*
12A
14B
17*
18A 19
21*
22
25A
25B 30
31
35
36B 39
40
41
44
46
47
10.6
10.8
11.0
11.2
11.4
11.6
11.8
12.0
12.2
12.4
12.6
12.8
13.0
13.2
13.4
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+
++
++
+
++
++
+
++
++
+
++
++
+
++
+
+++++++++++++++++++++++++
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
++++
+
++++
+
++++
+
++++
+
++++
+
+
+
++
++
+
++
++
+
++
++
+
++
++
+
++
++
+++
+
+
+++
+
+
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+
+
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+
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+
+
+
+
+
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+
+
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+
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++
+
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+
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+
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+
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+
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+
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+
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+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
+
++
+++++
+++++
+++++
+++++
+++
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
++
+++
++
+++
++
+++
++
+++
++
+++
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+
++
+
+
+++
++
+++
++
+++
++
+++
++
+++
++
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+++
+
+
+
++++
+
++++
+
++++
+
++++
+
+++
++
++
+
++
++
+
++
++
+
++
++
+
++
++
+
++++
+
++++
+
++++
+
++++
+
++++
+
+
++
++
+
++
++
+
++
++
+
++
++
+
++
++
C-out
APPENDIX J – Equipment Survey Lab Code
Smoking machine Model/Manufacturer
Gas chromatograph Model/Manufacturer/Internal Standards
Air flow meter Model/Manufacturer
NDIR analyzer Model/Manufacturer
1 Cerulean SM 450
Agilent GC/TCD/FID 6890N
Nic Column: 30m x 0.53mm WCOT (CP-WAX 52CB)
Nicotine I.S. n-heptadecane
Schiltknecht Thermoair 6
Cerulean COA205
Water Column: 27m x 0.53mm fused silica containing Poraplot Q
Water I.S. Ethanol
2A RM200 Agilent 7890/ Agilent Agilent 6890/ Agilent Agilent 6890N/ Agilent
Nic Column: 30m x 0.53mm WCOT (CP-WAX 52CB)
Nicotine I.S. n-heptadecane
CLIMOMASTER MODEL6543/KANOMAX
CO-Measuring Unit Model No.70700050/ Borgwaldt
Water Column: 27m x 0.53mm fused silica containing Poraplot Q
Water I.S. Ethanol
2B SM450 Agilent 7890/ Agilent Agilent 6890/ Agilent Agilent 6890N/ Agilent
Nic Column: 30m x 0.53mm WCOT (CP-WAX 52CB)
Nicotine I.S. n-heptadecane
Schiltknecht Thermoair 7
Cerulean COA206
Water Column: 27m x 0.53mm fused silica containing Poraplot Q
Water I.S. Ethanol
3A RM200 Agilent 6890/7890 Nic Column: 30m x 0.53mm WCOT (CP-WAX 52CB)
Nicotine I.S. n-heptadecane
Schiltknecht Thermoair 3 g.440.3s-113
Module RM200
Water Column: 27m x 0.53mm fused silica containing Poraplot Q
Water I.S. Ethanol
3B SM450 Agilent 6890/7890 Nic Column: 30m x 0.53mm WCOT (CP-WAX 52CB)
Nicotine I.S. n-heptadecane
Schiltknecht Thermoair 2
Cerulean COA205
CTR-RAC_2012 CM7 Collaborative Study 64 of 73 May 2013
Water Column: 27m x 0.53mm fused silica containing Poraplot Q
Water I.S. Ethanol
4 SM450 Agilent 6890 (G1530A) Nic Column: 2m x 1.8" x 2.0mm nickel column packed with 10% Carbowax 20M + 2% KOH on Chromosorb WHP 80-100 Mesh
Nicotine I.S. n-heptadecane
Schiltknecht Thermoair 2
Cerulean COA205
Water Column: 2m x 1.8" x 2.0mm nickel column packed with Porapak QS 80-100 Mesh
Water I.S. Ethanol
5 SM450 Agilent 6890N Nic Column: 6’ x 1/8” OD, stainless steel, 7% Carbowax-20M, 2% KOH, and 3% OS-138 on Chromosorb 80/100 mesh packing
Nicotine I.S. n-heptadecane
Schiltknecht ThermoAir3
Cerulean COA205
Water Column: 10’ x 1/8” OD, stainless steel,Porapak QS 80/100 mesh packing
Water I.S. Ethanol
6 RM200 7890A/ Agilent Nic Column: Agilent 1909N-113 : 30m x 320μm x 0.25μm
Nicotine I.S. n-heptadecane
R 24.00/ Borgwaldt 70700050/ Borgwaldt
Water Column: J&W 19091P-Q04 : 30m x 320μm x 20μm
Water I.S. Ethanol
7 RM200 Agilent 6890/HP Nic Column: DB-Wax
Nicotine I.S. n-heptadecane
g.440.3s-113 Schiltknecht Messtechnik AG
99033403 Borgwaldt
Water Column: HP-Plot Q
Water I.S. Ethanol
CTR-RAC_2012 CM7 Collaborative Study 65 of 73 May 2013
8A RM200A Agilent 6890 Nic Column: 5m, i.d. 0.2 mm, film 0.40 µm DB Wax etr
Nicotine I.S. n-heptadecane
Anemometer Schiltknecht
CO-Analyser Borgwaldt
Water Column: steel, 6ft, i.d. 2 mm Porapak Q
Water I.S. Ethanol
8B RM20D Agilent 6890 Nic Column: 5m, i.d. 0.2 mm, film 0.40 µm DB Wax etr
Nicotine I.S. n-heptadecane
Anemometer Schiltknecht
CO-Analyser Borgwaldt
Water Column: steel, 6ft, i.d. 2 mm Porapak Q
Water I.S. Ethanol
9A Cerulean SM450 Agilent 6890N Nic Column: 128-7323 DB-WAXTER 5m 0.2mm Narrowbore
Nicotine I.S. n-heptadecane
Schiltknecht - Airflow meter
Cerulean COA205
Water Column: Glass packed porapak QS
Water I.S. Ethanol
9B RM200 Agilent 6890N Nic Column: 128-7323 DB-WAXTER 5m 0.2mm Narrowbore
Nicotine I.S. n-heptadecane
Schiltknecht - Airflow meter
CO-Measuring Unit Model No.70700050/ Borgwaldt
Water Column: Glass packed porapak QS
Water I.S. Ethanol
10 RM20 HP 6890 Series GC System Agilent Tech.7890 A GC System
Nic Column: 5m, i.d. 0.2 mm, film 0.40µm DB Waxetr
Nicotine I.S.n-heptadecane
Anemometer g.440.3s-113Schiltknecht Messtechnik AG
CO-Analyser Borgwaldt
Water Column: steel, Packing: Chromosorb 102 80/100 Tubing:1/8" SS Length 6'
Water I.S. Ethanol
CTR-RAC_2012 CM7 Collaborative Study 66 of 73 May 2013
10B RM200A HP 6890 Series GC System Agilent Tech.7890 A GC System
Nic Column: 5m, i.d. 0.2 mm, film 0.40µm DB Waxetr
Nicotine I.S. n-heptadecane
Anemometer g.440.3s-113 Schiltknecht Messtechnik AG
CO-Analyser Borgwaldt
Water Column: steel, Packing: Chromosorb 102 80/100 Tubing:1/8" SS Length 6'
Water I.S. Ethanol
11B RM200A 6890 N / Agilent Nic Column: 7.5% Carbowax / 2% KOH, 80/100 Chromosorb-WAW, 1.8 m x 2.0 mm INNO steel-columns, packed
Nicotine I.S. n-heptadecane
Schiltknecht CO Module / Borgwaldt
Water Column: 60/80 Hayesep-Q, 3.60 m x 2.0mm INNO Steel-columns, packed
Water I.S. Methanol
11C RM20 CSR 6890 N / Agilent Nic Column: 7.5% Carbowax / 2% KOH, 80/100 Chromosorb-WAW, 1.8 m x 2.0 mm INNO steel-columns, packed
Nicotine I.S. n-heptadecane
Schiltknecht CO Module / Borgwaldt
Water Column: 60/80 Hayesep-Q, 3.60 m x 2.0mm INNO Steel-columns, packed
Water I.S. Methanol
12A SM450 Agilent 6890 Nic Column: Capillary Column (, L 25m, i.d. 0.mm, d.f. um)
Nicotine I.S. n-heptadecane
Schiltknecht ThermoAir3
Cerulean COA205
Water Column: Capillary Column (PoraPlot L 25m, i.d. 0.53mm, d.f. 20um)
Water I.S. Ethanol
CTR-RAC_2012 CM7 Collaborative Study 67 of 73 May 2013
12B RM200 Agilent 6890 Nic Column: Capillary Column (, L 25m, i.d. 0.mm, d.f. um)
Nicotine I.S. n-heptadecane
Info. not supplied Info. not supplied
Water Column: Capillary Column (PoraPlot L 25m, i.d. 0.53mm, d.f. 20um)
Water I.S. Ethanol
14A RM20H 7890 Series/Agilent Nic Column: 10% Carbowax 20 M plus KOH (80~100 mesh)
Nicotine I.S. n-heptadecane
Included in smoking machine
Included in smoking machine
Water Column: Porapak Q, 2 m packed
Water I.S. Ethanol
14B SM450 7890 Series/Agilent Nic Column: 10% Carbowax 20 M plus KOH (80~100 mesh)
Nicotine I.S. n-heptadecane
Schiltknecht, ThermoAir2
Included in smoking machine
Water Column: Porapak Q, 2 m packed
Water I.S. Ethanol
16 RM20 Agilent 6890 Nic Column: Chromosorb WHP (80-100 mesh) with 10% Carbowax 20M and 2% KOH 6ftx1/8"
Nicotine I.S. n-heptadecane
Integrated Air flow meter
Integrated NDIR analyser
Water Column: Porapak Q (80-100 mesh) 6ftx1/8"
Water I.S. Ethanol
17 SM450 7890A / Agilent Nic Column: 15 m x 0.53 mm i.d. ( 1 micro m thickness) capillary column Stabilwax-DB
Nicotine I.S. n-Octadecane
Schiltknecht Thermoair 6
Cerulean COA205
CTR-RAC_2012 CM7 Collaborative Study 68 of 73 May 2013
Water Column: 1.8 m x 2 mm i.d. glass column Gaskuropack 54 (80/100mesh)
Water I.S. Ethanol
18A SM450 6890N / Agilent Technologies
Nic Column: capillary columnCP7424 / Varian
Nicotine I.S.n-heptadecane
ThermoAir3 / Schiltknecht
Cerulean COA205
Water Column: capillary column CP7554 / Varian
Water I.S. Ethanol
18B RM200A 6890N / Agilent Technologies
Nic Column: capillary column CP7424 / Varian
Nicotine I.S. n-heptadecane
included into RM200A / Schiltknecht
included into RM200A / Borgwaldt
Water Column: capillary column CP7554 / Varian
Water I.S. Ethanol
19 SM450 Agilent 6890 Nic Column: DB-Wax 2m diam 0.18x0.3 film
Nicotine I.S. Octadecane
Schilltknecht Thermo Air 2
Cerulean COA and COA-15
Water Column: 80/100 Porapak Q 6 ft. 1/8 in x 2.1 mm
Water I.S. 200 Proof Ethyl Alcohol
21 SM450-08 HP 5890 GC Nic Column: 16% Apiezon L + 2% KOH + 2% Carbowax 20 M 80/100 2m x 3.2 mm o.d.
Nicotine I.S. Anethole
VFA450/Cerulean +ThermoAir2/Schiltnecht
Cerulean COA205
Water Column: Porapak Q 80/100 2m x 3.2 mm o.d.
Water I.S Methanol
22 Borgwaldt LM20X Info. not supplied Nic Column: Info. not supplied
Nicotine I.S. Info. not supplied
Info. not supplied Info. not supplied
CTR-RAC_2012 CM7 Collaborative Study 69 of 73 May 2013
Water Column: Info. not supplied
Water I.S. Info. not supplied
25A & B
SM450 Aligent 6890 Nic Column: DB Wax 52 25m x 0.53 ID
Nicotine I.S. Decanol
Schiltknecht Anemometer
Cerulean COA205
Water Column: Poroplot Q 25m x 0.53 ID
Water I.S. Ethanol
26 RM 200A HP 6890 Nic Column: CS-FS-FFAP 30m x 032
Nicotine I.S. n-heptadecane
Schildknecht Sibench/Siemens
Water Column: Supelco Q Plott
Water I.S. Methanol
28A & B
RM20H Agilent 6890 Nic Column: Agilent-INNOWAX*
Nicotine I.S. n-heptadecane
Schiltknecht type g.440.3s-113
Built in RM20H
Water Column: Agilent Poraplot Q**
Water I.S. Ethanol
29A RM20-CSR Nicotine 6890 N Agilent Water : 7890 A Agilent
Nic Column: HP - Innowax 30,0m x 320mm x 0,25mm
Nicotine I.S. n-heptadecane
Lambrecht Therm. Anemometer 642F
Borgwaldt KC C24
Water Column: HP - PLOT Q 30,0m x 320mm x 20,0mm
Water I.S. Ethanol
29B RM20 Nicotine 6890 N Agilent Water : 7890 A Agilent
Nic Column: HP - Innowax 30,0m x 320mm x 0,25mm
Nicotine I.S. n-heptadecane
Lambrecht Therm. Anemometer 642F
Borgwaldt KC C24
Water Column: HP - PLOT Q 30,0m x 320mm x 20,0mm
Water I.S. Ethanol
29C RM20CSR - Burghardt
Nicotine 6890 N Agilent Water : 7890 A Agilent
Nic Column: HP - Innowax 30,0m x 320mm x 0,25mm
Nicotine I.S. n-heptadecane
Lambrecht Therm. Anemometer 642F
Borgwaldt KC C24
Water Column: HP - PLOT Q 30,0m x 320mm x 20,0mm
Water I.S. Ethanol
CTR-RAC_2012 CM7 Collaborative Study 70 of 73 May 2013
30 SM450 CLARUS 500 PERKIN ELMER
Nic Column: 7%CW-20M 3%PMPE 6 RING 2%KOH
Nicotine I.S. n-heptadecane
SCHILTKNECHT THERMOAIR 2 TSI 8910/8470
Cerulean COA205
Water Column: PORAPAK Q
Water I.S. Ethanol
31 SM450 Hewlett Packard 6890 Series
Nic Column: Carbowax 20M 10% HOK 2% Support Chomosorb WHP 80/!00
Nicotine I.S. L-Carvona
g.445.2s-146 Schiltknecht (cerulean)
COA 205 SIGNAL AMBITECH
Water Column: Porapak QS 80/100
Water I.S. Ethanol
32 RM200 Thermo Trace GC Nic Column: HP5 (30m x0,32mm X 0,25mm)
Nicotine I.S. R-Carvone
g.440.3s-113 Borgwaldt
Borgwaldt
Water Column: Varian PoraplotQ (25m, 0,53mm i.d.,20mm)
Water I.S. Ethanol
34 RM20H 7890A/ Agilent Nic Column: HP-50+
Nicotine I.S. n-heptadecane
Schiltknecht/Swiss COA205
Water Column: Packed Column: Porapak Q, 80-100 mesh
Water I.S. Ethanol
35 Borgwaldt KC 20X Agillent 7890A Nic Column: Wcot fused silica 25M*0.53mm Coating CP-WAX52CB
Nicotine I.S. n-heptadecane
Borgwaldt integrated air-flow meter
Borgwaldt KC - C25
Water Column: Wcot fused silica 25M*0.53mm Coating CP-WAX52CB
Water I.S. Ethanol
36A RM200 Agilent 6890 Nic Column: 6ft x 1/8" SS column packed with 2% Versamid 900+1%KOH on
Nicotine I.S. n-heptadecane
INBUILT SCHILTKNECHT
BORGWALDT INTEGRATED CO ANALYSER
CTR-RAC_2012 CM7 Collaborative Study 71 of 73 May 2013
Chromosorb 750,80/100 mesh
Water Column: 6ft x 1/8" SS column packed with Porapak Q 80/100 mesh
Water I.S. Methanol
36B SM450 Agilent 6890 Nic Column: 6ft x 1/8" SS column packed with 2% Versamid 900+1%KOH on Chromosorb 750,80/100 mesh
Nicotine I.S. n-heptadecane
THERMO AIR 2 SCHILTKNECHT
Cerulean COA205
Water Column: 6ft x 1/8" SS column packed with Porapak Q 80/100 mesh
Water I.S. Methanol
37 RM20 HP 6890 - Agilent Nic Column: HP-5MS (Crosslinked 5%PHME Siloxane) 30m x 0,25mm x 0,25µm Film Thickness
Nicotine I.S. n-heptadecane
Schiltknecht Flow Meter
Borgwaldt CO Analyzer
Water Column: HP-PLOT Q (Divenylbenzene/styrene Porous Polymer) 30m x 0,32mm x 20,0µm Film Thickness
Water I.S. Methanol
39 SM450 Agilent 7890A GC System
Nic Column: Packed column - CARBOWAX 10% + 2% KOH
Nicotine I.S. n-heptadecane
435-2 Testo Cerulean COA205
CTR-RAC_2012 CM7 Collaborative Study 72 of 73 May 2013
Water Column: Packed column - PORAPAK QS 80 - 100
Water I.S. Ethanol
40 SM450 Agilent 6890 N Nic Column: Packed column - CARBOWAX 10% + 2% KOH
Nicotine I.S.Anethole
VPS102/ Schlitknecht Cerulean COA205
Water Column: 27m x 0.53mm fused silica containing Poraplot Q
Water I.S. Ethanol
41 SM450 Agilent 6890 Nic Column: DB WAX - 30 m x 0.32 mm x 0.25 mm
Nicotine I.S. Anethole
Schiltknecht Thermoair 2
Cerulean COA205
Water Column: HP-PLOT Q - 30 m x 0.53 mm x 40 mm
Water I.S. Ethanol
42A RM200A GC 7890A/Agilent Technologies
Nic Column: Packed, Carbowax-20M 2% KOH
Nicotine I.S. Decaheptane
g.440.3s-116 / Schiltknecht,
Model No. 80744870 / Borgwaldt-KC
Water Column: Packed, Porapak Q
Water I.S. Ethanol
42B RM20H GC 7890A/Agilent Technologies
Nic Column: Packed, Carbowax-20M 2% KOH
Nicotine I.S. Decaheptane
g.440.3s-116 / Schiltknecht,
Model No. 80744870 / Borgwaldt-KC
Water Column: Packed, Porapak Q
Water I.S. Ethanol
43 RM 200 Model 1998 Note: No airstraightener or modification kit
GC HP 6890 Model 1996
Nic Column: Capillary Column HP-INNOWAX
Nicotine I.S. Quinaldine
Anemometer RM 200 Art n° 80714730
Analyzer CO RM 200
Water Column: Packed Column Porapak
Water I.S. Methanol
44 SM450 GC2010-TCD/ SHIMADZU (water analysis) GC14B-FID/
Nic Column: Polyethyleneglycol 20 M + KOH 10% + 2% Chromosorb W80/100 AW-
Nicotine I.S. n-heptadecane
Schiltknecht Thermoair 2
Cerulean COA205
CTR-RAC_2012 CM7 Collaborative Study 73 of 73 May 2013
SHIMADZU (nicotine analysis)
DMCS Shimadzu 2.0 m x 3.0 mm
Water Column: Porapak Q 80/100 Shimadzu 2.0 m x 3.0 mm
Water I.S. Ethanol
46 SM450 HP-5890 Nic Column: Supelco 80/100 Porapak R 1/8 in x 2.1 mm
Nicotine I.S. n-heptadecane
Schiltknecht - 1 Air flow meter
Cerulean
Water Column: Alltech EC-Wax 30m x 0.53mm x 1.2 mm
Water I.S. Ethanol
47 Borgwaldt LX-20 Perkin Elmer, Clarus 680
Nic Column: P&E Elite WAX: 30 m (25 m) x 0.53 mm ID, 1.0 um film
Nicotine I.S. n-heptadecane
Borgwaldt KC AirFlow Module
Borgwaldt KC Non-Dispersive Infrared Absorption (NDIR) Gas Analyzer, Model C25 Water Column:
Agilent CP PoraPLOT Q: 13 m (10 m), 0.53 mm ID, 20 um film
Water I.S. Ethanol