routine analytical chemistry sub-group · rac-224-ctr cm9 coll. study 2019 – august 2020 3/72 1....
Post on 29-Aug-2020
2 Views
Preview:
TRANSCRIPT
Routine Analytical Chemistry Sub-Group
Technical Report
2019 Collaborative Study of
CORESTA Monitor 9 (CM9)
for the Determination of Test Piece
Weight, TPM, Water, Nicotine,
NFDPM, Carbon Monoxide and Puff Count Obtained under Mainstream
‘ISO’ and ‘Intense’ Smoking
Regimes
August 2020
Coordinator:
Linda A. Crumpler, Cerulean, USA
Authors:
Guy Jaccard and Donatien Tafin Djoko
Philip Morris International, Switzerland
Table of Contents
1. Introduction ......................................................................................................................... 3
2. Organisation ........................................................................................................................ 3
2.1 Participants .............................................................................................................. 3
2.2 Protocol ................................................................................................................... 4
3. Raw Data ............................................................................................................................. 5
4. Statistical Analysis ............................................................................................................ 18
4.1 Exclusion of outliers .............................................................................................. 18
4.1.1 Numerical outlier technique: Cochran & Grubbs test ............................... 18
4.2 Repeatability and Reproducibility estimation ....................................................... 18
5. Data Representation .......................................................................................................... 20
5.1 ISO 3308 smoking regime ..................................................................................... 21
5.2 ISO Intense 20778 smoking regime ...................................................................... 25
6. Comparison ....................................................................................................................... 28
Comparisons of Linear with Rotary smoking machines for test piece CM9 ........ 28
Comparison with previous studies ........................................................................ 28
7. Conclusion......................................................................................................................... 30
APPENDIX A – List of Participating Laboratories ................................................................. 31
APPENDIX B – Experimental Protocol .................................................................................. 32
APPENDIX C – Departures from Experimental Protocol ....................................................... 33
APPENDIX D – Raw Data Set ................................................................................................ 34
APPENDIX E – IUPAC 1994 Harmonized Statistical Procedure ........................................... 39
APPENDIX F – Linear – Rotary Comparisons ....................................................................... 40
APPENDIX G – Rotary Smoking Machines ........................................................................... 47
APPENDIX H – Linear Smoking Machines ............................................................................ 53
APPENDIX I – Equipment Survey .......................................................................................... 59
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 3/72
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 2019 study was designed:
• to measure mainstream ISO (ISO 3308) and ISO Intense (ISO 20778) smoke yields of
nicotine-free dry particulate matter (NFDPM), nicotine (NIC) and carbon monoxide
(CO) to verify the current monitor test piece CM9
• to determine intra- and inter-laboratory variability for the measured ISO and ISO Intense
smoke yields for the CM9
• to verify the conditioned weight for the CM9
2. Organisation
2.1 Participants
In total 18 laboratories participated in the 2019 study. Appendix A lists the participating
laboratories in alphabetical order. Note: the mix of labs between ISO and Intense differed.
18 laboratories delivered data for ISO mainstream smoke (ISO 3308) for the CM9 test piece
using 25 smoking machines (18 rotary smoking machines and 7 linear smoking machines).
14 laboratories delivered data for ISO Intense mainstream smoke (ISO 20778) for the CM9 test
piece using 17 smoking machines (10 rotary smoking machines and 7 linear smoking
machines).
Table 1 summarises the number and type of smoking machines used.
Table 1: Number of smoking machines
Machine Class ISO (ISO 3308) ISO Intense (ISO 20778)
Linear smoking machines 7 7
LX-20 type 1 1
SM450 type 6 6
Rotary smoking machines 18 10
RM20D type 2 1
RM20H type 7 4
RM200 A type 9 5
Total 25 17
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 4/72
Table 2 summarises the number of datasets for CM 9 provided for the reported parameters.
Table 2: Number of datasets obtained
Physical Parameter
WEIGHT 125
Smoking Parameter ISO (ISO 3308) Intense (ISO 20778)
TPM 125 85
WATER 125 85
NIC 125 85
NFDPM 125 85
CO 125 85
PUFF 125 85
Total individual data obtained 750 510
Total individual data expected 750 510
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 CM9 - 2019 Experimental Protocol” (provided in Appendix B) to analyse the product
CM9 and to report the seven parameters listed in Table 3.
Table 3: Parameters to be reported
Parameter Number of replicates
Unit Code
Conditioned Weight 5 mg/test piece (t.p.) WEIGHT
Total Particulate Matter 5 mg/test piece (t.p.) TPM
Water content (smoke) 5 mg/test piece (t.p.) WATER
Smoke Nicotine 5 mg/test piece (t.p.) NIC
Nicotine Free Dry
Particulate Matter 5 mg/test piece (t.p.) NFDPM
Carbon Monoxide 5 mg/test piece (t.p.) CO
Puff count 5 puff/test piece (t.p.) PUFF
CM9 test pieces should have been smoked under two different mainstream smoking regimes
with a fixed butt length of 33 mm as defined in the following table:
Table 4: Mainstream ISO and Intense smoking regime parameters
Smoking Regime
Puff Volume (mL)
Puff Frequency (s)
Puff Duration (s)
Vent. Blocking (%)
ISO 35 60 2 0
Intense 55 30 2 100
The participants bought the CM9 test piece individually via Borgwaldt KC or Cerulean.
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 5/72
3. Raw data
Table 5 provides the results for the conditioned weight of CM9. Tables 6 to 11 list the results
for the reported parameters for ISO smoking regime (ISO 3308). Tables 12 to 17 list the results
for ISO intense smoking regime (ISO 20778). Basic statistics (mean and standard deviation)
were applied to summarize the raw data for each smoking machine used and parameters
reported for CM 9 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.
Table 5: CM9, WEIGHT mean and standard deviation per laboratory code
Lab Code Machine Mean
(mg/t.p.) SD
(mg/t.p.) CV [%]
Sample size
1 R 948,74 2,49 0,26 5
2 R 938,3 3,95 0,42 5
3A R 940,38 4,13 0,44 5
3B R 943,32 4,01 0,43 5
4 R 943,38 3,52 0,37 5
5A L 948 4,54 0,48 5
5B R 937,2 1,89 0,2 5
6 L 950,16 2,2 0,23 5
7 R 944,2 1,79 0,19 5
8A R 937,42 1,91 0,2 5
8B R 937,98 1,10 0,12 5
9 L 946,98 5,66 0,6 5
10 L 937,18 2,02 0,22 5
11A R 938,4 5,13 0,55 5
11B R 938,2 2,28 0,24 5
12 R 941,88 2,44 0,26 5
13 L 932,66 7,14 0,77 5
14A R 937 1,66 0,18 5
14B R 935,74 1,73 0,18 5
15 R 941,5 4,15 0,44 5
16A R 945,3 1,13 0,12 5
16B R 946,6 2,31 0,24 5
16C R 943,78 1,58 0,17 5
17 L 930,22 9,66 1,04 5
18 L 937,8 9,6 1,02 5
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 6/72
Table 6: CM9. ISO smoking regime. TPM mean and standard deviation per laboratory code
Lab Code Machine
Type Mean
(mg/t.p.) SD
(mg/t.p.) CV [%]
Sample size
1 R 17,22 0,22 1,29 5
2 R 17,04 0,45 2,63 5
3A R 17,08 0,18 1,04 5
3B R 17,57 0,18 1,02 5
4 R 17,1 0,24 1,43 5
5A L 17,56 0,2 1,15 5
5B R 16,72 0,26 1,58 5
6 L 17,46 0,55 3,12 5
7 R 17,03 0,21 1,26 5
8A R 17,35 0,25 1,45 5
8B R 16,73 0,19 1,11 5
9 L 17,25 0,33 1,89 5
10 L 16,85 0,4 2,37 5
11A R 16,66 0,18 1,05 5
11B R 17,05 0,24 1,38 5
12 R 16,62 0,4 2,39 5
13 L 16,86 0,33 1,99 5
14A R 16,56 0,46 2,78 5
14B R 15,77 0,38 2,44 5
15 R 16,85 0,17 1,01 5
16A R 16,78 0,15 0,88 5
16B R 16,9 0,12 0,69 5
16C R 17,03 0,25 1,48 5
17 L 16,97 0,67 3,95 5
18 L 17,53 0,25 1,41 5
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 7/72
Table 7: CM9. ISO smoking regime. Water mean and standard deviation per laboratory code
Lab Code Machine
Type Mean
(mg/t.p.) SD
(mg/t.p.) CV [%]
Sample size
1 R 2,02 0,05 2,71 5
2 R 1,99 0,18 8,87 5
3A R 2,11 0,03 1,34 5
3B R 2,34 0,08 3,49 5
4 R 2,07 0,1 4,72 5
5A L 1,55 0,06 3,87 5
5B R 2,02 0,17 8,24 5
6 L 1,34 0,2 15,02 5
7 R 1,95 0,05 2,55 5
8A R 2,14 0,08 3,78 5
8B R 2,17 0,14 6,68 5
9 L 1,66 0,09 5,69 5
10 L 1,22 0,11 9,02 5
11A R 1,91 0,05 2,38 5
11B R 2,04 0,05 2,39 5
12 R 1,95 0,06 3,2 5
13 L 1,36 0,17 12,42 5
14A R 2 0,13 6,28 5
14B R 1,67 0,16 9,3 5
15 R 2 0,11 5,64 5
16A R 1,73 0,12 6,75 5
16B R 1,84 0,13 6,95 5
16C R 1,83 0,07 3,58 5
17 L 0,97 0,49 50,66 5
18 L 1,78 0,71 39,81 5
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 8/72
Table 8: CM9. ISO smoking regime. Nicotine mean and standard deviation per laboratory code
Lab Code Machine
Type Mean
(mg/t.p.) SD
(mg/t.p.) CV [%]
Sample size
1 R 1,441 0,015 1,01 5
2 R 1,434 0,042 2,943 5
3A R 1,485 0,032 2,147 5
3B R 1,498 0,009 0,589 5
4 R 1,425 0,017 1,218 5
5A L 1,481 0,044 2,977 5
5B R 1,438 0,016 1,096 5
6 L 1,559 0,048 3,092 5
7 R 1,507 0,01 0,659 5
8A R 1,407 0,037 2,636 5
8B R 1,415 0,014 0,977 5
9 L 1,425 0,022 1,54 5
10 L 1,437 0,028 1,915 5
11A R 1,418 0,026 1,825 5
11B R 1,426 0,017 1,173 5
12 R 1,497 0,035 2,333 5
13 L 1,525 0,032 2,087 5
14A R 1,319 0,04 3,041 5
14B R 1,241 0,028 2,22 5
15 R 1,378 0,017 1,198 5
16A R 1,432 0,033 2,293 5
16B R 1,432 0,033 2,282 5
16C R 1,438 0,056 3,919 5
17 L 1,452 0,063 4,316 5
18 L 1,576 0,043 2,729 5
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 9/72
Table 9: CM9. ISO smoking regime. NFDPM mean and standard deviation per laboratory code
Lab Code Machine
Type Mean
(mg/t.p.) SD
(mg/t.p.) CV [%]
Sample size
1 R 13,75 0,2 1,49 5
2 R 13,62 0,27 2 5
3A R 13,49 0,16 1,17 5
3B R 13,73 0,15 1,09 5
4 R 13,6 0,15 1,08 5
5A L 14,52 0,26 1,8 5
5B R 13,26 0,15 1,1 5
6 L 14,56 0,46 3,16 5
7 R 13,56 0,2 1,46 5
8A R 13,8 0,15 1,08 5
8B R 13,15 0,13 0,99 5
9 L 14,16 0,31 2,17 5
10 L 14,19 0,31 2,21 5
11A R 13,32 0,17 1,25 5
11B R 13,59 0,24 1,77 5
12 R 13,18 0,32 2,39 5
13 L 13,98 0,43 3,05 5
14A R 13,24 0,33 2,51 5
14B R 12,85 0,24 1,83 5
15 R 13,47 0,16 1,17 5
16A R 13,61 0,14 1,06 5
16B R 13,63 0,11 0,81 5
16C R 13,76 0,22 1,59 5
17 L 14,55 0,52 3,61 5
18 L 14,17 0,57 4,01 5
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 10/72
Table 10: CM9. ISO smoking regime. CO mean and standard deviation per laboratory code
Lab Code Machine
Type Mean
(mg/t.p.) SD
(mg/t.p.) CV [%]
Sample size
1 R 13,17 0,15 1,11 5
2 R 13,09 0,19 1,49 5
3A R 14,38 0,23 1,6 5
3B R 14,2 0,29 2,06 5
4 R 13,66 0,13 0,98 5
5A L 13,21 0,37 2,79 5
5B R 13,65 0,32 2,34 5
6 L 12,73 0,47 3,68 5
7 R 13,51 0,32 2,35 5
8A R 13,66 0,21 1,53 5
8B R 12,47 0,21 1,68 5
9 L 13,48 0,24 1,8 5
10 L 12,78 0,25 1,92 5
11A R 13,17 0,22 1,69 5
11B R 13,09 0,21 1,63 5
12 R 14,07 0,32 2,25 5
13 L 12,7 0,41 3,26 5
14A R 12,11 0,16 1,35 5
14B R 12,54 0,69 5,53 5
15 R 14,33 0,58 4,05 5
16A R 13,53 0,26 1,93 5
16B R 13,69 0,12 0,89 5
16C R 13,79 0,27 1,97 5
17 L 12,42 0,66 5,3 5
18 L 13,52 0,43 3,16 5
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 11/72
Table 11: CM9. ISO smoking regime. Puff count mean and standard deviation per laboratory code
Lab Code Machine
Type Mean
(mg/t.p.) SD
(mg/t.p.) CV [%]
Sample size
1 R 7,56 0,05 0,72 5
2 R 7,46 0,05 0,73 5
3A R 7,6 0,09 1,17 5
3B R 7,83 0,09 1,13 5
4 R 7,45 0,05 0,61 5
5A L 7,8 0,06 0,74 5
6 L 7,92 0,13 1,58 5
7 R 7,59 0,09 1,13 5
8A R 7,5 0,03 0,33 5
8B R 7,49 0,09 1,26 5
9 L 7,96 0,14 1,78 5
10 L 7,48 0,15 2,02 5
11A R 7,36 0,1 1,38 5
11B R 7,63 0,1 1,32 5
12 R 7,49 0,05 0,69 5
13 L 7,59 0,11 1,41 5
14A R 7,48 0,12 1,58 5
14B R 7,3 0,15 2,03 5
15 R 7,53 0,01 0,18 5
16A R 7,32 0,05 0,68 5
16B R 7,35 0,07 1 5
16C R 7,29 0,06 0,82 5
17 L 7,7 0,1 1,33 5
18 L 7,86 0,08 1,02 5
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 12/72
Table 12: CM9. ISO Intense smoking regime. TPM mean and standard deviation per laboratory code
Lab Code Machine
Type Mean
(mg/t.p.) SD
(mg/t.p.) CV [%]
Sample size
1 R 41,44 0,25 0,6 5
2 R 40,64 0,31 0,77 5
3A R 42,03 0,22 0,53 5
3B R 40,4 0,81 2 5
4 R 41,36 0,39 0,94 5
5A L 44,19 0,38 0,86 5
5B R 39,94 0,39 0,97 5
6 L 44,83 0,77 1,73 5
7 R 40,76 0,69 1,69 5
9 L 46,1 0,7 1,51 5
10 L 44,44 0,54 1,22 5
11A R 40,78 0,16 0,4 5
11B R 41,16 0,48 1,16 5
12 R 38,51 0,71 1,84 5
13 L 44,09 0,5 1,14 5
17 L 47,25 0,88 1,87 5
18 L 46,19 0,82 1,78 5
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 13/72
Table 13: CM9. ISO Intense smoking regime. Water mean and standard deviation per laboratory code
Lab Code Machine
Type Mean
(mg/t.p.) SD
(mg/t.p.) CV [%]
Sample size
1 R 9,53 0,16 1,65 5
2 R 8,68 0,49 5,66 5
3A R 9,44 0,26 2,71 5
3B R 9,94 0,24 2,38 5
4 R 9,97 0,27 2,72 5
5A L 10,83 0,77 7,14 5
5B R 8,57 0,35 4,03 5
6 L 10,91 0,19 1,71 5
7 R 9,02 0,57 6,27 5
9 L 11,7 0,29 2,45 5
10 L 11,15 0,32 2,87 5
11A R 9,74 0,33 3,43 5
11B R 9,81 0,3 3,06 5
12 R 8,4 0,32 3,86 5
13 L 11,25 0,55 4,92 5
17 L 11,72 0,75 6,4 5
18 L 5,77 0,19 3,23 5
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 14/72
Table 14: CM9. ISO Intense smoking regime. Nicotine mean and standard deviation per laboratory code
Lab Code Machine
Type Mean
(mg/t.p.) SD
(mg/t.p.) CV [%]
Sample size
1 R 3,031 0,057 1,869 5
2 R 3,036 0,052 1,723 5
3A R 3,075 0,039 1,266 5
3B R 3,059 0,051 1,678 5
4 R 3,055 0,046 1,518 5
5A L 3,252 0,057 1,758 5
5B R 3,078 0,046 1,509 5
6 L 3,203 0,017 0,536 5
7 R 3,146 0,072 2,303 5
9 L 3,055 0,009 0,304 5
10 L 3,1 0,017 0,555 5
11A R 2,958 0,027 0,923 5
11B R 2,988 0,039 1,299 5
12 R 3,095 0,056 1,808 5
13 L 3,066 0,013 0,417 5
17 L 3,074 0,053 1,73 5
18 L 1,887 0,005 0,263 5
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 15/72
Table 15: CM9. ISO Intense smoking regime. NFDPM mean and standard deviation per laboratory code
Lab Code Machine
Type Mean
(mg/t.p.) SD
(mg/t.p.) CV [%]
Sample size
1 R 28,88 0,17 0,61 5
2 R 28,92 0,3 1,05 5
3A R 29,52 0,28 0,96 5
3B R 27,39 0,64 2,33 5
4 R 28,34 0,22 0,78 5
5A L 30,1 0,74 2,47 5
5B R 28,3 0,32 1,15 5
6 L 30,76 0,67 2,17 5
7 R 28,6 0,31 1,09 5
9 L 31,35 0,41 1,31 5
10 L 30,23 0,51 1,68 5
11A R 28,09 0,4 1,43 5
11B R 28,37 0,56 1,98 5
12 R 27,02 0,45 1,66 5
13 L 29,69 0,95 3,19 5
17 L 32,38 0,99 3,05 5
18 L 38,6 0,79 2,05 5
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 16/72
Table 16: CM9. ISO Intense smoking regime. CO mean and standard deviation per laboratory code
Lab Code Machine
Type Mean
(mg/t.p.) SD
(mg/t.p.) CV [%]
Sample size
1 R 24,75 0,12 0,47 5
2 R 24,41 0,37 1,53 5
3A R 25,41 0,32 1,27 5
3B R 25,68 0,26 1,01 5
4 R 24,93 0,29 1,18 5
5A L 23,33 0,17 0,73 5
5B R 24,49 0,51 2,08 5
6 L 23,48 0,12 0,52 5
7 R 24,57 0,48 1,96 5
9 L 25,48 0,33 1,3 5
10 L 24,43 0,4 1,63 5
11A R 24,84 0,17 0,69 5
11B R 24,32 0,44 1,82 5
12 R 25,27 0,41 1,61 5
13 L 24 0,32 1,33 5
17 L 24,34 0,59 2,44 5
18 L 25,38 0,36 1,42 5
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 17/72
Table 17: CM9. ISO Intense smoking regime. Puff count mean and standard deviation per laboratory code
Lab Code Machine
Type Mean
(mg/t.p.) SD
(mg/t.p.) CV [%]
Sample size
1 R 10,81 0,09 0,83 5
2 R 10,86 0,16 1,43 5
3A R 10,84 0,12 1,1 5
3B R 11,25 0,09 0,81 5
4 R 10,85 0,17 1,61 5
5A L 10,81 0,1 0,94 5
5B R 10,44 0,13 1,29 5
6 L 11,24 0,21 1,85 5
7 R 11,1 0,18 1,59 5
9 L 11,02 0,1 0,94 5
10 L 10,39 0,16 1,53 5
11A R 10,55 0,14 1,3 5
11B R 11,01 0,21 1,86 5
12 R 11,11 0,18 1,6 5
13 L 10,56 0,09 0,83 5
17 L 10,79 0,11 1,06 5
18 L 11,15 0,17 1,55 5
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 18/72
4. Statistical analysis
4.1 Exclusion of outliers
4.1.1 Numerical outlier technique: Cochran & Grubbs test
The statistical evaluation of data for this collaborative study followed the methods provided by
ISO 5725-2[1]. For outlier testing, the Grubbs and Cochran methods were used.
ISO 5725-2 Tests Consistency
Cochran’s – test Within-laboratory variability: Suitable for detecting whether the highest value in a set of laboratory standard deviations is an outlier or not.
Grubbs’ – test Between-laboratory variability: Suitable for detecting whether the highest (or lowest) laboratories averages are outliers or not.
The protocol “Harmonized statistical procedure” defined by IUPAC (International Union of
Pure and Applied Chemistry) has been applied as well. It consists of sequential applications of
the Cochran and Grubbs tests until no further outliers are detected or until a drop of more than
22.2% in the original number of laboratories would occur (see flowchart in Appendix F).
First, the Cochran outlier test is applied, and if an outlying laboratory is identified, then a single
value Grubbs test is performed on the individual values of this outlying laboratory (Individual
Grubbs). If no individual value is identified as outlier, the outlying laboratory is removed. When
an individual value is identified as an outlier, only this value is removed.
Afterwards single-value Grubbs test is applied and outlying laboratories are removed. If no
laboratory is identified as outlier, the pair-value test is applied (two values at the same end).
Remove any laboratory(ies) flagged by these tests, but stop removal if more than 22.2% would
be removed.
The test was performed with both linear and rotary smoking machines together, but also with
rotary, respectively linear smoking machines separately. The results provided in the report for
all smoking machines, respectively with linear or rotary only smoking machines are obtained
after exclusion of the outliers for those respective categories.
Note:
The paired value Grubbs’ test is an extension of the single value Grubbs' test for pairs of
outliers. The use is advised in ISO 5725 to detect pairs of outlier undetectable sequentially by
using single value Grubbs' test.
The outlying laboratories are provided in the Tables 18-23.
4.2 Repeatability and reproducibility estimation
Repeatability and reproducibility limits are calculated for both smoking regimes, each
parameter and for both smoking machine types. The results are summarized in tables 18 to 23,
with all machines grouped, respectively with linear or rotary machines only, both with ISO
(ISO 3308) and intense smoking regimes (ISO 20778), for CM9. Outlying laboratories are
provided in the same tables. The number of laboratories provided in the tables correspond to
the number of laboratories, for which data (totally or at least in part) were taken into account
[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
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 19/72
for the calculation of repeatability and reproducibility parameters, after suppression of outlying
data. The corresponding graphs named “individual values” are given in Part 5 of this report. C
and G/G2 in the Tables 18 to 23 stand for Cochran test and Grubbs test outliers respectively.
Table 18: r&R estimations for CM9 under ISO 3308 smoking regime (all machines)
p n Global Mean
Sr CVr [%]
r SR CVR [%]
R C G/G2 Stragglers Parameter
All
23 5 941,49 3,37 0,36 9,53 5,60 0,59 15,83 17-18 NA 13 CW (mg/t.p.)
25 5 16,98 0,32 1,88 0,9 0,48 2,83 1,36 NA NA 17-14A-14B TPM (mg/t.p)
23 5 1,87 0,11 6,10 0,32 0,3 16,26 0,86 17-18 NA NA Water (mg/t.p)
25 5 1,443 0,033 2,307 0,094 0,076 5,232 0,214 NA NA 14A-14B-18 Nicotine (mg/t.p.)
25 5 13,71 0,28 2,06 0,8 0,52 3,78 1,46 NA NA 18 NFDPM (mg/t.p)
25 5 13,32 0,34 2,59 0,97 0,69 5,17 1,95 NA NA 14B CO (mg/t.p.)
25 5 7,55 0,09 1,22 0,26 0,22 2,86 0,61 NA NA NA Puff.count
Table 19: r&R estimations for CM9 under ISO 3308 smoking regime (rotary machines)
p n Global Mean
Sr CVr [%]
r SR CVR [%]
R C G/G2 Stragglers Parameter
Ro
tary
17 5 16,96 0,26 1,55 0,74 0,36 2,11 1,01 NA 14B NA TPM (mg/t.p.)
18 5 1,99 0,11 5,36 0,3 0,18 9,28 0,52 NA NA NA Water (mg/t.p)
14 5 1,403 0,03 2,173 0,086 0,063 4,48 0,178 NA 7-3B-12-3A NA Nicotine (mg/t.p.)
18 5 13,48 0,2 1,51 0,57 0,32 2,35 0,89 NA NA NA NFDPM (mg/t.p)
16 5 13,45 0,24 1,75 0,67 0,63 4,69 1,79 14B-15 NA NA CO (mg/t.p.)
18 5 7,47 0,08 1,1 0,23 0,16 2,16 0,46 NA NA NA Puff.count
Table 20: r&R estimations for CM9 under ISO 3308 smoking regime (linear machines)
p n Global Mean
Sr CVr [%]
r SR CVR [%]
R C G/G2 Stragglers Parameter
Lin
ea
r
7 5 17,21 0,42 2,43 1,18 0,49 2,84 1,38 NA NA NA TPM (mg/t.p.)
5 5 1,42 0,14 9,6 0,39 0,21 15,06 0,61 18-17 NA NA Water (mg/t.p.)
7 5 1,494 0,042 2,806 0,119 0,071 4,755 0,201 NA NA NA Nicotine (mg/t.p.)
7 5 14,31 0,42 2,96 1,2 0,44 3,11 1,26 NA NA NA NFDPM (mg/t.p.)
7 5 12,98 0,42 3,27 1,2 0,57 4,39 1,61 NA NA NA CO (mg/t.p.)
7 5 7,76 0,11 1,46 0,32 0,21 2,65 0,58 NA NA NA Puff.count
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 20/72
Table 21: r&R estimations for CM9 under ISO Intense 20778 smoking regime (all machines)
p n Global Mean Sr CVr[%] r SR CVR [%] R C G/G2 Stragglers Parameter
All
17 5 42,6 0,58 1,35 1,63 2,6 6,11 7,37 NA NA NA TPM (mg/t.p.)
17 5 9,79 0,42 4,24 1,17 1,53 15,65 4,33 NA NA 18 Water (mg/t.p.)
16 5 3,079 0,045 1,452 0,126 0,083 2,696 0,235 NA 18 5A-6 Nicotine (mg/t.p.)
16 5 29,25 0,55 1,88 1,55 1,53 5,23 4,32 NA 18 NA NFDPM (mg/t.p.)
17 5 24,65 0,36 1,46 1,02 0,75 3,02 2,11 NA NA NA CO (mg/t.p.)
17 5 10,87 0,15 1,35 0,42 0,3 2,73 0,84 NA NA NA Puff.count
Table 22: r&R estimations for CM9 under ISO Intense 20778 smoking regime (rotary machines)
p n Global Mean
Sr CVr [%]
r SR CVR [%]
R C G/G2 Stragglers Parameter
Ro
tary
10 5 40,7 0,49 1,2 1,38 1,06 2,61 3 NA NA NA TPM (mg/t.p.)
10 5 9,31 0,35 3,73 0,98 0,67 7,2 1,9 NA NA NA Water (mg/t.p.)
10 5 3,052 0,05 1,639 0,142 0,07 2,282 0,197 NA NA NA Nicotine (mg/t.p.)
10 5 28,34 0,39 1,38 1,11 0,81 2,86 2,29 NA NA NA NFDPM (mg/t.p.)
10 5 24,87 0,36 1,45 1,02 0,56 2,25 1,58 NA NA NA CO (mg/t.p.)
10 5 10,88 0,15 1,38 0,43 0,28 2,61 0,8 NA NA NA Puff.count
Table 23: r&R estimations for CM9 under ISO Intense 20778 smoking regime (linear machines)
p n Global Mean
Sr CVr [%]
r SR CVR [ %]
R C G/G2 Stragglers Parameter
Lin
ea
r
7 5 45,3 0,68 1,5 1,92 1,36 3 3,85 NA NA NA TPM (mg/t.p.)
6 5 11,26 0,53 4,71 1,5 0,61 5,4 1,72 NA 18 NA Water (mg/t.p.)
6 5 3,125 0,034 1,088 0,096 0,088 2,812 0,249 NA 18 5A Nicotine (mg/t.p.)
6 5 30,75 0,74 2,41 2,09 1,19 3,86 3,35 NA 18 NA NFDPM (mg/t.p.)
7 5 24,35 0,36 1,47 1,01 0,9 3,7 2,55 NA NA NA CO (mg/t.p.)
7 5 10,85 0,14 1,3 0,4 0,33 3,07 0,94 NA NA NA Puff.count
5. Data representation
The following figures show the raw data for CM9 and for all parameters. The plots indicate
mean values with 95 % confidence interval (CI) highlighted in green (for valid participants) or
in red (for participants detected as outlier) for each smoking machine. Laboratories excluded
by outlier statistics are denoted by the name of the test rejecting the laboratory (G for Grubbs,
G2 for double Grubbs and C for Cochran). The confidence limits at 95 % and 99 % for the
difference between the reference value (average of all laboratories) and the average of one
laboratory are plotted in orange and red respectively.
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 21/72
5.1 ISO 3308 smoking regime
Figure 1: CM9 Individual observations of conditioned test piece WEIGHT
Outlier values in red, straggler value in orange
Figure 2: CM9 Individual observations of mainstream ISO 3308 TPM
Straggler values in orange
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 22/72
Figure 3: CM9 Individual observations of mainstream ISO 3308 WATER
Outlier values in red
Figure 4: CM9 Individual observations of mainstream ISO 3308 Nicotine
Stragglers values in orange
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 23/72
Figure 5: CM9 Individual observations of mainstream ISO 3308 NFDPM
Straggler value in orange
Figure 6: CM9 Individual observations of mainstream ISO 3308 CO
Straggler value in orange
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 24/72
Figure 7: CM9 Individual observations of mainstream ISO 3308 PUFF Count
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 25/72
5.2 ISO Intense 20778 smoking regime
Figure 8: CM9 Individual observations of mainstream ISO Intense 20778 TPM
Figure 9: CM9 Individual observations of mainstream ISO Intense 20778 WATER
Straggler value in orange
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 26/72
Figure 10: CM9 Individual observations of mainstream ISO Intense 20778 Nicotine
Outlier value in red, straggler values in orange
Figure 11: CM9 Individual observations of mainstream ISO Intense 20778 NFDPM
Outlier value in red
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 27/72
Figure 12: CM9 Individual observations of mainstream ISO Intense 20778 CO
Outlier value in red
Figure 13: CM9 Individual observations of mainstream ISO Intense 20778 PUFF Count
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 28/72
6. Comparison
Comparisons of linear with rotary smoking machines for test piece CM9
It should be noted that a statistical evaluation of differences in linear and rotary smoking
machine results on the basis of just one product (CM9) could be misleading. Furthermore, a
simplistic differentiation between linear and rotary smoking machines could also be misleading
as both machine types used in this study comprise different models produced by different
manufacturers. Furthermore it has to be noted that each measurement from a rotary machine
represents a single result from a single pad onto which the smoke of twenty (or ten in intense
smoking regime) test pieces is trapped. Linear smoking machines require 4 pads to collect
mainstream TPM from the same number of test pieces and hence each measurement on a linear
machine is the average of 4 results. This has to be taken into account when interpreting
statistical differences in repeatability between machine classes.
Due to the aforementioned reasons a pure statistical comparison is considered to have limited
value.
Graphical comparison of smoke data separated for linear and rotary smoking machines are
available in Appendix F.
Comparison with previous studies
This section compares the results of this study with previous collaborative studies of different
test pieces conducted by the Routine Analytical Sub-Group under the ISO 3308 smoking
regime. It has to be noted that the number of smoking machines, smoking machine types and
participants varies throughout the studies.
Table 24 lists the averages, reproducibility and repeatability limits for the test pieces CM7,
CM8 and CM9 under ISO 3308 smoking regime.
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 29/72
Table 24: Averages, repeatability, reproducibility of CORESTA collaborative studies from 2011
to 2019 for different test pieces under ISO 3308 smoking conditions
ISO 3308 smoking regime
Year 2011 2012 2013 2014 2014 2016 2017 2018 2018 2019
Test piece CM7 CM7 CM7 CM7 CM8 CM8 CM8 CM8 CM9 CM9
Average
TPM (mg/t.p.)
16.37 16.28 16.16 16.15 17.57 17.33 17.37 17.24 16.98 16.98
WATER (mg/t.p.)
1.78 1.75 1.71 1.71 1.84 1.81 1.82 1.79 1.68 1.87
NICOTINE (mg/t.p.)
1.236 1.221 1.221 1.204 1.650 1.657 1.672 1.650 1.48 1.443
NFDPM (mg/t.p.)
13.34 13.29 13.23 13.25 14.06 13.86 13.95 13.81 13.82 13.71
CO (mg/t.p.)
12.93 12.84 12.76 12.83 13.42 13.24 13.21 13.12 13.06 13.32
PUFF (/t.p.)
8.36 8.36 8.32 8.23 7.70 7.72 7.78 7.88 7.76 7.55
Repeatability (r)
TPM (mg/t.p.)
0.93 0.80 0.85 0.87 1.06 1.05 1.07 1.03 0.96 0.90
WATER (mg/t.p.)
0.41 0.41 0.39 0.36 0.39 0.35 0.40 0.43 0.45 0.32
NICOTINE (mg/t.p.)
0.075 0.066 0.076 0.075 0.119 0.093 0.096 0.090 0.095 0.094
NFDPM (mg/t.p.)
0.77 0.78 0.72 0.72 0.82 0.89 0.89 0.90 0.80 0.80
CO (mg/t.p.)
0.95 0.78 0.75 0.79 1.05 0.79 0.97 0.97 1.03 0.97
PUFF (/t.p.)
0.38 0.34 0.31 0.36 0.30 0.39 0.36 0.36 0.35 0.26
Reproducibility (R)
TPM (mg/t.p.)
1.77 1.67 1.61 1.93 1.89 1.95 1.93 1.92 1.56 1.36
WATER (mg/t.p.)
0.97 1.03 0.98 1.01 1.12 1.08 1.15 0.95 0.91 0.86
NICOTINE (mg/t.p.)
0.150 0.143 0.146 0.155 0.197 0.202 0.254 0.17 0.185 0.214
NFDPM (mg/t.p.)
1.88 1.73 1.85 2.16 1.97 1.91 1.86 1.69 1.42 1.46
CO (mg/t.p.)
1.94 1.75 1.61 1.97 2.02 1.52 1.97 1.64 1.79 1.95
PUFF (/t.p.)
0.86 0.93 0.91 0.82 0.75 0.83 1.00 0.87 0.94 0.61
There is no systematic tendency for the mean values of CM9 between 2018 and 2019: some
parameters decrease slightly, but not all, such as nicotine or puff count. Repeatability and
reproducibility figures are quite stable and comparable to those obtained with the other test
pieces. CM9 results are in line with previous test pieces.
Table 25 lists the averages, reproducibility and repeatability limits for the test pieces CM7,
CM8 and CM9 under intense smoking regime.
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 30/72
Table 25: Averages, repeatability, reproducibility of CORESTA collaborative studies from 2013
to 2019 for different test pieces under ISO intense 20778 smoking conditions
ISO Intense 20778 smoking regime
Year 2013 2016 2017 2018 2018 2019
Test piece CM7 CM8 CM8 CM8 CM9 CM9
Average
TPM (mg/t.p.) 41.56 43.08 43.36 42.83 42.84 42.60
WATER (mg/t.p.) 10.33 10.01 10.29 10.27 10.19 9.79
NICOTINE (mg/t.p.) 2.493 3.400 3.425 3.373 3.107 3.079
NFDPM (mg/t.p.) 28.39 29.65 29.65 29.19 29.44 29.25
CO (mg/t.p.) 24.72 24.88 24.86 24.89 24.71 24.65
PUFF (/t.p.) 11.79 11.08 11.12 11.28 10.97 10.87
Repeatability (r)
TPM (mg/t.p.) 2.38 1.96 2.17 2.17 1.79 1.63
WATER (mg/t.p.) 1.23 0.98 1.33 1.18 1.28 1.17
NICOTINE (mg/t.p.) 0.152 0.152 0.161 0.199 0.179 0.126
NFDPM (mg/t.p.) 1.57 1.39 1.30 1.64 1.62 1.55
CO (mg/t.p.) 1.30 1.04 1.24 1.31 1.25 1.02
PUFF (/t.p.) 0.52 0.47 0.43 0.51 0.50 0.42
Reproducibility (R)
TPM (mg/t.p.) 10.53 9.47 7.86 8.72 8.93 7.37
WATER (mg/t.p.) 4.77 3.79 4.18 4.86 3.71 4.33
NICOTINE (mg/t.p.) 0.313 0.508 0.416 0.405 0.275 0.235
NFDPM (mg/t.p.) 5.66 5.03 4.56 4.47 4.72 4.32
CO (mg/t.p.) 3.01 2.00 2.72 2.83 2.46 2.11
PUFF (/t.p.) 1.27 0.92 1.18 1.12 1.10 0.84
The mean values obtained for CM9 in 2019 are lower for all parameters when compared with
the mean values obtained in 2018, but are still very close. The values for repeatability and
reproducibility are generally better in 2019 than in 2018 for almost all parameters. The observed
differences in terms of means, repeatability and reproducibility may be due to a different set of
laboratories in 2018 and 2019.
Table 26 lists the averages, reproducibility and repeatability limits of conditioned weight.
Table 26: Average weight data, repeatability and reproducibility for test pieces CM9
Study CM9 2018 CM9 2019
Weight (mg/t.p.) 943.2 941.49
Repeatability (r) 13.3 9.53
Reproducibility (R) 17.9 15.83
The data obtained in the three collaborative tests for the test piece conditioned weight are quite
stable in terms of average, repeatability and reproducibility.
7. Conclusion
In summary the analytical results for the CM9 test piece lead to the conclusion that they can be
used as monitor test pieces in smoke analysis.
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 31/72
APPENDIX A – List of Participating Laboratories
ASL Analytic Service Laboratory Labstat International Inc.
BAT Germany GmbH Landewyck Tobacco sa
C.I.T. Monte Paz S.A. Liggett Group
Enthalpy Analytical Richmond Papierfabrik Wattens
Imperial Poland Philip Morris Brazil Super Lab
Imperial Tobacco Production Ukraine Prudence Development and Management Corporation
ITG Joure PT HM Sampoerna Tbk
Karelia Tobacco Co. R.J. Reynolds Tobacco Co.
KT&G Reemtsma / Imperial Brands Central Lab Hamburg
Out of the 18 participating laboratories, 4 labs did not perform the intense smoking regime.
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 32/72
APPENDIX B – Experimental Protocol
Adobe Acrobat
Document
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 33/72
APPENDIX C – Departures from Experimental Protocol
No departures from experimental protocol.
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 34/72
APPENDIX D – Raw Data Set
Table 1: Raw data for CM9 – ISO Smoking regime
Lab count
Machine Count
Lab Code
Machine Class
Machine Type
Run No.
Cond. Weight (mg/t.p)
TPM (mg/t.p.)
Water (mg/t.p)
Nicotine (mg/t.p)
NFDPM (mg/t.p)
CO (mg/t.p)
Puff Count
1 1 1 R RM200A
1 949,3 16,84 1,99 1,419 13,43 13,00 7,50
2 949,2 17,39 2,07 1,452 13,87 13,05 7,50
3 950,3 17,35 1,95 1,456 13,94 13,36 7,60
4 950,5 17,30 2,01 1,437 13,85 13,20 7,60
5 944,4 17,20 2,08 1,440 13,68 13,24 7,60
2 2 2 R RM200A
1 933,5 16,78 1,96 1,385 13,44 12,88 7,50
2 944,0 16,60 1,85 1,408 13,34 12,87 7,50
3 937,5 17,43 1,99 1,474 13,97 13,24 7,50
4 936,5 16,79 1,87 1,422 13,50 13,26 7,40
5 940,0 17,61 2,29 1,482 13,84 13,18 7,40
3
3 3A R RM200A
1 937,9 17,36 2,10 1,539 13,72 14,19 7,66
2 947,7 16,96 2,08 1,487 13,39 14,49 7,70
3 939,1 17,05 2,14 1,471 13,44 14,73 7,57
4 938,1 17,13 2,09 1,472 13,56 14,31 7,59
5 939,1 16,91 2,14 1,457 13,32 14,19 7,47
4 3B R RM20D
1 942,3 17,35 2,22 1,491 13,63 13,70 7,98
2 945,2 17,64 2,28 1,499 13,87 14,43 7,82
3 939,3 17,74 2,40 1,507 13,83 14,20 7,74
4 940,5 17,70 2,39 1,507 13,81 14,36 7,81
5 949,3 17,40 2,39 1,488 13,52 14,32 7,82
4 5 4 R RM20H
1 947,5 17,36 2,12 1,433 13,80 13,80 7,44
2 942,6 16,70 1,90 1,401 13,39 13,50 7,40
3 938,6 17,14 2,12 1,448 13,58 13,60 7,41
4 942,1 17,12 2,10 1,419 13,60 13,80 7,50
5 946,1 17,20 2,13 1,425 13,64 13,60 7,49
5
6 5A L SM450
1 951,3 17,29 1,62 1,528 14,14 13,43 7,83
2 943,9 17,48 1,61 1,419 14,46 13,46 7,83
3 942,8 17,54 1,50 1,519 14,52 12,92 7,83
4 953,2 17,63 1,50 1,476 14,65 12,72 7,70
5 948,8 17,84 1,52 1,465 14,85 13,54 7,83
7 5B R RM20H
1 936,7 16,64 1,99 1,410 13,24 13,74 7,10
2 934,7 16,65 2,11 1,441 13,10 13,47 7,33
3 939,5 17,06 2,23 1,446 13,38 14,15 7,35
4 936,5 16,89 2,00 1,449 13,44 13,31 7,22
5 938,6 16,37 1,78 1,442 13,15 13,60 7,33
6 8 6 L SM450
1 949,7 17,93 1,14 1,630 15,16 12,98 7,94
2 949,7 17,68 1,35 1,573 14,75 12,68 7,97
3 953,8 17,83 1,63 1,558 14,64 12,90 8,06
4 947,8 17,25 1,41 1,535 14,31 13,15 7,72
5 949,8 16,60 1,16 1,500 13,94 11,95 7,90
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 35/72
Lab count
Machine Count
Lab Code
Machine Class
Machine Type
Run No.
Cond. Weight (mg/t.p)
TPM (mg/t.p.)
Water (mg/t.p)
Nicotine (mg/t.p)
NFDPM (mg/t.p)
CO (mg/t.p)
Puff Count
7 9 7 R RM200A
1 946,0 17,02 1,95 1,506 13,56 13,80 7,58
2 946,0 17,27 2,03 1,492 13,75 13,75 7,62
3 943,0 17,17 1,91 1,508 13,75 13,36 7,65
4 942,0 16,71 1,91 1,519 13,28 13,03 7,64
5 944,0 16,96 1,97 1,512 13,48 13,60 7,44
8
10 8A R RM200A
1 940,5 17,50 2,17 1,424 13,91 13,65 7,53
2 937,1 17,63 2,21 1,434 13,99 13,85 7,48
3 937,2 17,41 2,19 1,441 13,78 13,83 7,50
4 935,2 17,19 2,11 1,355 13,73 13,65 7,48
5 937,1 17,00 2,01 1,382 13,61 13,33 7,53
11 8B R RM20
1 938,3 16,93 2,12 1,430 13,38 12,40 7,50
2 936,3 16,55 2,04 1,397 13,11 12,83 7,35
3 939,0 16,74 2,21 1,424 13,11 12,31 7,61
4 938,8 16,54 2,07 1,405 13,07 12,35 7,48
5 937,5 16,90 2,40 1,421 13,08 12,45 7,53
9 12 9 L SM450
1 954,9 17,72 1,59 1,459 14,67 13,43 7,93
2 941,0 16,86 1,55 1,405 13,90 13,18 7,78
3 950,3 17,39 1,79 1,407 14,19 13,75 8,08
4 942,8 17,09 1,70 1,431 13,95 13,35 8,13
5 945,9 17,17 1,65 1,422 14,09 13,71 7,90
10 13 10 L SM450
1 935,0 17,33 1,29 1,471 14,56 12,85 7,56
2 940,4 17,10 1,30 1,454 14,34 12,99 7,65
3 937,2 16,78 1,30 1,433 14,04 12,97 7,51
4 937,2 16,79 1,07 1,430 14,29 12,72 7,40
5 936,1 16,27 1,13 1,398 13,74 12,39 7,26
11
14 11A R RM200A
1 933,0 16,56 1,94 1,390 13,23 13,22 7,21
2 944,0 16,95 1,92 1,440 13,59 13,29 7,40
3 933,0 16,68 1,91 1,390 13,38 13,45 7,30
4 942,0 16,51 1,84 1,430 13,24 13,01 7,47
5 940,0 16,58 1,96 1,440 13,18 12,89 7,40
15 11B R RM20H
1 937,0 17,06 2,10 1,440 13,52 12,95 7,72
2 941,0 17,43 1,99 1,440 14,00 13,05 7,71
3 935,0 17,03 2,04 1,430 13,56 13,39 7,61
4 939,0 16,79 1,99 1,420 13,38 12,85 7,64
5 939,0 16,95 2,07 1,400 13,48 13,21 7,47
12 16 12 R RM20H
1 943,5 16,69 1,95 1,490 13,25 14,07 7,53
2 941,7 17,21 2,01 1,545 13,66 14,60 7,52
3 938,9 16,68 1,99 1,518 13,18 13,78 7,40
4 945,0 16,37 1,93 1,457 12,98 13,98 7,50
5 940,3 16,16 1,85 1,475 12,83 13,90 7,50
13 17 13 L SM450
1 927,2 17,28 1,19 1,575 14,52 12,84 7,58
2 936,7 16,83 1,31 1,528 13,99 12,96 7,61
3 931,2 17,03 1,25 1,519 14,26 12,76 7,58
4 925,4 16,37 1,41 1,487 13,47 11,98 7,43
5 942,8 16,81 1,62 1,517 13,67 12,98 7,73
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 36/72
Lab count
Machine Count
Lab Code
Machine Class
Machine Type
Run No.
Cond. Weight (mg/t.p)
TPM (mg/t.p.)
Water (mg/t.p)
Nicotine (mg/t.p)
NFDPM (mg/t.p)
CO (mg/t.p)
Puff Count
14
18 14A R RM20H
1 935,5 16,78 1,94 1,325 13,51 12,00 7,46
2 937,5 17,15 2,20 1,381 13,57 12,00 7,65
3 938,5 16,67 2,01 1,318 13,34 12,10 7,51
4 935,0 16,24 2,00 1,274 12,97 12,04 7,48
5 938,5 15,98 1,86 1,296 12,82 12,39 7,32
19 14B R RM20H
1 935,8 15,40 1,46 1,213 12,72 11,69 7,38
2 934,6 15,92 1,74 1,272 12,91 13,38 7,37
3 938,7 15,90 1,67 1,246 12,99 12,60 7,35
4 934,6 16,26 1,88 1,263 13,12 13,01 7,38
5 935,0 15,35 1,61 1,213 12,52 12,02 7,04
15 20 15 R RM20D
1 941,5 16,95 1,86 1,396 13,69 14,24 7,55
2 936,0 16,61 1,92 1,395 13,30 13,46 7,54
3 945,0 17,03 2,09 1,372 13,57 14,28 7,52
4 939,0 16,75 2,01 1,369 13,37 15,00 7,54
5 946,0 16,92 2,13 1,359 13,43 14,69 7,52
16
21 16A R RM200A
1 945,0 16,53 1,72 1,404 13,41 13,11 7,25
2 943,8 16,78 1,64 1,437 13,70 13,81 7,33
3 945,1 16,92 1,72 1,432 13,76 13,63 7,35
4 945,7 16,85 1,93 1,402 13,52 13,62 7,30
5 946,9 16,81 1,65 1,483 13,68 13,50 7,38
22 16B R RM200A
1 948,9 16,84 1,80 1,398 13,65 13,82 7,30
2 946,6 16,81 1,86 1,418 13,54 13,60 7,40
3 943,6 16,86 1,66 1,422 13,78 13,64 7,27
4 945,1 17,10 2,01 1,435 13,66 13,81 7,33
5 948,8 16,87 1,89 1,485 13,50 13,56 7,45
23 16C R RM400A
1 944,5 16,69 1,77 1,391 13,53 13,61 7,22
2 942,4 17,28 1,79 1,487 14,00 14,23 7,38
3 941,8 17,26 1,85 1,433 13,98 13,77 7,27
4 944,8 16,88 1,93 1,376 13,58 13,53 7,32
5 945,4 17,02 1,79 1,503 13,73 13,80 7,28
17 24 17 L SM450
1 939,8 16,66 1,34 1,430 13,89 11,84 7,61
2 941,5 17,62 1,59 1,421 14,60 11,59 7,80
3 925,7 17,19 0,85 1,514 14,84 12,78 7,74
4 922,5 15,95 0,39 1,375 14,19 12,91 7,58
5 921,6 17,41 0,67 1,519 15,22 13,00 7,79
18 25 18 L LX20
1 945,0 17,33 1,07 1,547 14,71 13,49 7,76
2 926,0 17,23 1,51 1,578 14,14 13,03 7,89
3 950,0 17,65 1,89 1,564 14,20 13,75 7,94
4 934,0 17,60 1,50 1,541 14,56 14,11 7,79
5 934,0 17,84 2,94 1,648 13,25 13,22 7,92
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 37/72
Table 2: Raw data for CM9 – Intense Smoking regime
Lab count
Machine Count
Lab Code
Machine Class
Machine Type
Run No.
TPM (mg/t.p.)
Water (mg/t.p)
Nicotin (mg/t.p)
NFDPM (mg/t.p)
CO (mg/t.p)
Puff Count
1 1 1 R RM200A
1 41,69 9,77 3,003 28,91 24,78 10,80
2 41,71 9,54 3,116 29,05 24,82 10,70
3 41,19 9,54 3,061 28,59 24,54 10,90
4 41,39 9,44 2,976 28,97 24,77 10,90
5 41,22 9,35 3,001 28,86 24,82 10,75
2 2 2 R RM200A
1 40,51 8,36 2,995 29,16 24,17 10,90
2 40,16 8,30 2,980 28,89 24,13 10,75
3 40,82 8,87 3,046 28,90 24,97 11,10
4 40,74 8,41 3,113 29,22 24,17 10,70
5 40,96 9,46 3,046 28,45 24,63 10,85
3
3 3A R RM200A
1 41,71 9,38 3,129 29,20 25,56 10,79
2 42,00 9,26 3,102 29,63 25,66 10,96
3 41,96 9,47 3,035 29,45 25,10 10,98
4 42,21 9,22 3,052 29,94 25,02 10,78
5 42,27 9,86 3,058 29,36 25,70 10,71
4 3B R RM20D
1 39,61 9,79 3,005 26,81 25,69 11,22
2 39,98 9,65 3,048 27,28 25,24 11,19
3 41,26 9,96 3,124 28,17 25,92 11,14
4 39,85 10,06 3,018 26,77 25,79 11,36
5 41,28 10,26 3,099 27,92 25,77 11,32
4 5 4 R RM20H
1 41,19 9,61 3,064 28,52 25,34 11,00
2 41,36 10,16 3,044 28,15 24,60 10,60
3 41,41 10,10 2,995 28,31 24,75 10,97
4 41,95 10,22 3,124 28,60 25,10 10,94
5 40,89 9,75 3,049 28,10 24,85 10,73
5
6 5A L SM450
1 44,34 9,81 3,240 31,28 23,07 10,73
2 44,29 10,77 3,170 30,35 23,44 10,94
3 43,55 10,46 3,240 29,85 23,27 10,73
4 44,20 11,27 3,320 29,61 23,39 10,90
5 44,55 11,84 3,290 29,43 23,50 10,75
7 5B R RM20H
1 40,14 8,42 3,000 28,72 24,97 10,48
2 39,55 8,39 3,080 28,09 23,97 10,41
3 40,30 8,61 3,120 28,57 24,99 10,58
4 40,23 9,15 3,105 27,98 24,56 10,52
5 39,50 8,28 3,085 28,14 23,96 10,23
6 8 6 L SM450
1 45,60 11,19 3,230 31,18 23,43 11,21
2 44,35 10,95 3,196 30,24 23,53 11,18
3 43,95 10,83 3,195 29,99 23,51 11,11
4 45,68 10,91 3,210 31,62 23,64 11,60
5 44,56 10,68 3,186 30,75 23,31 11,09
7 9 7 R RM200A
1 41,68 9,36 3,226 29,10 25,39 10,98
2 41,07 9,56 3,162 28,35 24,46 11,12
3 40,31 8,72 3,113 28,48 24,48 11,15
4 39,90 8,18 3,040 28,68 24,13 10,89
5 40,86 9,30 3,191 28,37 24,37 11,35
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 38/72
Lab count
Machine Count
Lab Code
Machine Class
Machine Type
Run No.
TPM (mg/t.p.)
Water (mg/t.p)
Nicotin (mg/t.p)
NFDPM (mg/t.p)
CO (mg/t.p)
Puff Count
8 10 9 L SM450
1 45,54 11,48 3,069 30,99 25,28 11,04
2 45,66 11,48 3,051 31,14 25,26 10,91
3 45,91 11,65 3,050 31,21 26,00 11,18
4 46,12 11,69 3,045 31,38 25,24 10,96
5 47,28 12,18 3,058 32,04 25,62 10,99
9 11 10 L SM450
1 44,55 10,82 3,117 30,61 24,52 10,37
2 44,38 11,04 3,110 30,29 24,78 10,20
3 43,67 10,97 3,097 29,66 23,77 10,56
4 45,19 11,31 3,102 30,82 24,69 10,55
5 44,42 11,63 3,072 29,77 24,38 10,29
10
12 11A R RM200A
1 40,65 10,16 2,915 27,58 24,66 10,43
2 41,01 9,44 2,965 28,61 24,76 10,45
3 40,71 9,39 2,950 28,37 24,73 10,64
4 40,64 9,71 2,985 27,95 25,06 10,47
5 40,90 9,98 2,975 27,95 24,98 10,74
13 11B R RM20H
1 41,25 9,35 3,030 28,87 24,39 10,77
2 41,14 10,17 2,950 28,02 24,08 11,03
3 41,80 9,89 3,030 28,89 24,44 11,09
4 40,46 9,90 2,965 27,59 23,75 10,85
5 41,17 9,74 2,965 28,46 24,94 11,29
11 14 12 R RM20H
1 38,18 8,57 3,055 26,56 24,70 11,26
2 38,44 8,19 3,116 27,14 25,51 11,22
3 38,65 8,27 3,064 27,31 25,10 11,24
4 37,69 8,10 3,055 26,54 25,29 10,98
5 39,61 8,89 3,184 27,53 25,77 10,87
12 15 13 L SM450
1 43,72 11,43 3,088 29,20 23,95 10,57
2 43,50 12,14 3,058 28,33 23,46 10,43
3 44,28 10,94 3,061 30,12 24,26 10,51
4 44,79 10,85 3,067 30,78 24,16 10,63
5 44,18 10,87 3,057 30,03 24,15 10,64
13 16 17 L SM450
1 46,63 12,30 3,159 31,17 23,31 10,64
2 46,96 11,96 3,084 31,98 24,77 10,78
3 46,40 11,06 3,065 32,16 24,38 10,86
4 48,55 12,49 3,026 32,80 24,59 10,93
5 47,73 10,81 3,034 33,81 24,66 10,72
14 17 18 L LX20
1 45,28 5,56 1,890 37,83 25,42 10,96
2 46,49 6,00 1,880 38,56 25,63 11,21
3 47,15 5,80 1,885 39,43 25,77 11,40
4 46,64 5,60 1,886 39,37 24,84 11,17
5 45,38 5,88 1,893 37,80 25,26 11,02
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 39/72
APPENDIX E – IUPAC 1994 Harmonized Statistical Procedure
IUPAC 1994 HARMONIZED STATISTICAL PROCEDURE
SCREEN OUT NON
VALID DATA
START OF LOOP
CALCULATE PRECISION
MEASURES
(C)
COCHRAN
OUTLYING LAB?
(G)
SINGLE
GRUBBS
OUTLIER?
(G2)
PAIRED
GRUBBS
OUTLIER?
END REPORT
ORIGINAL & LAST
COMPUTED
PRECISION
MEASURES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 2/9
DROP INDIVIDUAL VALUE
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 2/9
ANY LABS
DROPPED IN
THIS LOOP
YES
YES
YES
YES
NO
NO
NO
NO
(Gi)SINGLE GRUBBS
OUTLIER ON INDIVIDUAL VALUES
OF COCHRAN OUTLYING
LAB?
YES
DROP LAB UNLESS OVERALL
FRACTION OF LABS DROPPED
WOULD EXCEED 2/9
NO
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 40/72
APPENDIX F – Linear – Rotary Comparisons
In all figures, the black line corresponds to the spread for r, while the red bar corresponds to the
spread for R
Figure 1: CM9 under ISO 3308 smoking regime – r and R values (conditioned weight)
Figure 2: CM9 under ISO 3308 smoking regimes – r and R values (TPM)
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 41/72
Figure 3: CM9 under ISO 3308 smoking regimes – r and R values (Water)
Figure 4: CM9 under ISO 3308 smoking regime – r and R values (Nicotine)
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 42/72
Figure 5: CM9 under ISO 3308 smoking regimes – r and R values (NFDPM)
Figure 6: CM9 under ISO 3308 smoking regime – r and R values (CO)
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 43/72
Figure 7: CM9 under ISO 3308 smoking regime – r and R values (puff count)
Figure 8: CM9 under ISO intense 20778 smoking regimes – r and R values (TPM)
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 44/72
Figure 9: CM9 under ISO intense 20778 smoking regimes – r and R values (Water)
Figure 10: CM9 under ISO intense 20778 smoking regime – r and R values (Nicotine)
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 45/72
Figure 11: CM9 under ISO intense 20778 smoking regimes – r and R values (NFDPM)
Figure 12: CM9 under ISO intense 20778 smoking regime – r and R values (CO)
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 46/72
Figure 13: CM9 under ISO intense 20778 smoking regime – r and R values (puff count)
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 47/72
APPENDIX G – Rotary Smoking Machines
1. ISO 3308 smoking regime
Figure 1: CM9 Individual observations of mainstream ISO 3308 TPM
Outlier value in red
Figure 2: CM9 Individual observations of mainstream ISO 3308 WATER
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 48/72
Figure 3: CM9 Individual observations of mainstream ISO 3308 Nicotine
Outlier values in red, straggler values in orange
Figure 4: CM9 Individual observations of mainstream ISO 3308 NFDPM
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 49/72
Figure 5: CM9 Individual observations of mainstream ISO 3308 CO
Outlier values in red
Figure 6: CM9 Individual observations of mainstream ISO 3308 PUFF Count
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 50/72
2. Intense ISO 20778 smoking regime
Figure 7: CM9 Individual observations of mainstream ISO Intense 20778 TPM
Figure 8: CM9 Individual observations of mainstream ISO Intense 20778 WATER
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 51/72
Figure 9: CM9 Individual observations of mainstream “Intense” Nicotine
Figure 10: CM9 Individual observations of mainstream ISO Intense 20778 NFDPM
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 52/72
Figure 11: CM9 Individual observations of mainstream ISO Intense 20778 CO
Figure 12: CM9 Individual observations of mainstream ISO Intense 20778 PUFF Count
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 53/72
APPENDIX H – Linear Smoking Machines
1. ISO Smoking regime
Figure 1: CM9 Individual observations of mainstream ISO 3308 TPM
Figure 2: CM9 Individual observations of mainstream ISO 3308 WATER
Outlier values in red
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 54/72
Figure 3: CM9 Individual observations of mainstream ISO 3308 Nicotine
Figure 4: CM9 Individual observations of mainstream ISO 3308 NFDPM
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 55/72
Figure 5: CM9 Individual observations of mainstream ISO 3308 CO
Straggler value in orange, outlier values in red
Figure 6: CM9 Individual observations of mainstream ISO 3308 PUFF Count
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 56/72
2. ISO Intense 20778 smoking regime
Figure 7: CM9 Individual observations of mainstream ISO Intense 20778 TPM
Figure 8: CM9 Individual observations of mainstream ISO Intense 20778 WATER
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 57/72
Figure 9: CM9 Individual observations of mainstream ISO Intense 20778 Nicotine
Outlier value in red
Figure 10: CM9 Individual observations of mainstream ISO Intense 20778 NFDPM
Outlier value in red
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 58/72
Figure 11: CM9 Individual observations of mainstream ISO Intense 20778 CO
Figure 12: CM9 Individual observations of mainstream ISO Intense 20778 PUFF Count
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 59/72
APPENDIX I – Equipment Survey
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph Model/Manufacturer/Column/ Internal Standards
Airlflow Meter Model/Manufacturer
NDIR analyser Model/Manufacturer
1 RM200A2/ Borgwaldt KC Agilent 7890A
Nic Column: Length: 30 m i.d.: 320 µm
Film Thickness: 0.25 µm
Stationary Phase: HP-Innowax
Nicotine I.S. n- Heptadecane
Anemometer Type Schiltknecht
Siemens Water Column:
Length 15m i.d.: 320µm
Film thickness: 20µm
Stationary Phase: HP-PLOT/Q
Water I.S. Ethanol
2 RM200A / Borgwaldt KC Agilent 7890
(Nic) HP 6890 (Water)
Nic Column: Length: 30 m i.d.: 320 µm
Film Thickness: Stationary Phase:
DB-ALC 1
Nicotine I.S. n-Heptadecane
Anemometer Type Schiltknecht
Borgwaldt KC Water Column:
Length: 6 ft. i.d.: 2 mm
Film Thickness: Stationary Phase:
Porapak Q
Water I.S. Ethanol
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 60/72
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph Model/Manufacturer/Column/ Internal Standards
Airlflow Meter Model/Manufacturer
NDIR analyser Model/Manufacturer
3A RM200A2 / Borgwaldt KC Agilent 7890B
Nic Column: 1.8 x 2.0 mm INNO
Steel packed column
7.5% Carbowax / 2% KOH, 80/100
Chromosorb-WAW
Nicotine I.S. n-Heptadecane
Anemometer Type g.440.4s-180 Schiltknecht
Borgwaldt KC
Water Column: 3.60 m x 2.0 m
INNO-Steel packed column
60/90 Hayesep-Q,
Water I.S. Methanol
3B RM20D / Borgwaldt Agilent 7890B
Nic Column: 1.8 x 2.0 mm INNO Steel packed column7.5%
Carbowax / 2% KOH, 80/100
Chromosorb-WAW
Nicotine I.S. n- Heptadecane
Anemometer Schiltknecht
Siemens
Water Column: 3.60 m x 2.0 m
INNO-Steel packed column
60/90 Hayesep-Q,
Water I.S. Methanol
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 61/72
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph Model/Manufacturer/Column/ Internal Standards
Airlflow Meter Model/Manufacturer
NDIR analyser Model/Manufacturer
4 RM20H / Borgwaldt KC Agilent 7890N
Nic Column: Length: 80/100 8ft
i.d.: 2.0mm Film thickness:1/8
In Stationary Phase: 10% CW-20M 2% KOH Chr-WAW
Nicotine I.S. n-Heptadecane
Anemometer Schiltknecht
CO/CO2 Analyser C24 Borgwaldt KC
Water Column: Length: 80/100 6ft
i.d.: 2.1 mm Film thickness:1/8
in. Stationary Phase:
Porapak Q
Water I.S. Ethanol
5A SM450 / Cerulean Agilent 7890A
Nic Column: Length: 15m i.d.: 0.32mm
Film Thickness: 0.25µm
Stationary Phase: polyethylene glycol
(PEG)
Nicotine I.S. Carvone
Anemometer Type ThermoAir2 model
VPS 103 / Schiltknecht
COA205 / Ceulean Water Column: Length: 30m i.d.: 0.32 mm
Film thickness: 20µm
Stationary Phase: Polystyrene-
divinylbenzene
Water I.S. Ethanol
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 62/72
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph Model/Manufacturer/Column/ Internal Standards
Airlflow Meter Model/Manufacturer
NDIR analyser Model/Manufacturer
5B RM20H / Borgwaldt KC Agilent 7890A
Nic Column: Length: 15m i.d.: 0.32mm
Film Thickness: 0.25µm
Stationary Phase: polyethylene glycol
(PEG)
Nicotine I.S. Carvone
Anemometer Type ThermoAir3 with RS232 interface /
Schiltknecht
CO-Analyser 80744870 / Borgwaldt
KC Water Column: Length: 30m i.d.: 0.32 mm
Film thickness: 20µm
Stationary Phase: Polystyrene-
divinylbenzene
Water I.S. Ethanol
6 SM450 / Cerulean 7890 / Agilent
Nic Column:Length: 5 mi.d.: 0.18
mmFilm thickness: 0.3 µmStationary Phase: DBWAX
WTR
Nicotine I.S.n-Heptadecane
ThermoAir2 / Schiltknecht
COA205 / Cerulean
Water Column: Length: 6 ft packed
i.d.: 2.1 mm Stationary Phase: 80/100 Porapak Q
Water I.S. 200 Proof
Ethy1 Alcohol
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 63/72
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph Model/Manufacturer/Column/ Internal Standards
Airlflow Meter Model/Manufacturer
NDIR analyser Model/Manufacturer
7 RM200A / Borgwaldt KC 6890 / HP
Nic Column: Length: 30 m i.d.: 0.32 mm
Film thicknessL 0.25 µm
Stationary Phase: Optima Wax
Nicotine I.S. n-Heptadecane
Anemometer Type / Schiltknecht
Sibench / Siemens Water Column: Length: 15 m i.d.: 0.320 mm
Film thickness: 20.0 µm
Stationary Phase: HP-PlotQ
Water I.S. Methanol
8A RM200A / Borgwaldt KC
6890 N / Agilent (Nic)
7890 / Agilent (Water)
Nic Column: Length: 30 m i.d.: 0.32mm
Film Thickness: 0.25µm
Stationary Phase: HP-INNOWAX
Nicotine I.S. n-Heptadecane
G.440.3S / Schiltknecht
C24 / Borgwaldt KC Water Column: Length: 30 m i.d.: 0.320 mm
Film Thickness: 20 µm
Stationary Phase: HP-PLOT/Q
Water I.S. Ethanol
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 64/72
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph Model/Manufacturer/Column/ Internal Standards
Airlflow Meter Model/Manufacturer
NDIR analyser Model/Manufacturer
8B RM20H / Borgwaldt KC
6890 N / Agilent (Nic)
7890 / Agilent (Water)
Nic Column: Length: 30 m i.d.: 0.32mm
Film Thickness: 0.25µm
Stationary Phase: HP-INNOWAX
Nicotine I.S. n-Heptadecane
G.440.3s-113 / Schiltknecht
C24 / Borgwaldt KC Water Column: Length: 30 m i.d.: 0.320 mm
Film Thickness: 20 µm
Stationary Phase: HP-PLOT/Q
Water I.S. Ethanol
9 SM450 / Cerulean
GC2010plus-FID / Shimadzu
(Nic)GC2010-TCD / Shimadzu
)Water)
Nic Column: Length: 10 mi.d.: 0.18
mmFilm thickness: 0,18 µmStationary Phase: ZB=wax
plus Phenomenex
Nicotine I.S.n-Heptadecane
ThermoAir3 / Schiltknecht
COA205 / Cerulean Water Column: Length: 12.5 m i.d.: 0.53 mm
Film thickness: 20 µm
Stationary Phase: Poraplot Q-HT
Agilent
Water I.S. Ethanol
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 65/72
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph Model/Manufacturer/Column/ Internal Standards
Airlflow Meter Model/Manufacturer
NDIR analyser Model/Manufacturer
10 SM450 / Cerulean Agilent 6890
Nic Column: 6' x 1/8" OD,
stainless steel Stationary Phase:7%
Carbowax-20M, 2% KOH and 3% OS-
138 on Chromosorb 80/100 mesh
Nicotine I.S. n-Heptadecane
1 COA205 / Cerulean
Water Column: 10' x 1/8" OD, stainless steel
Porapak WS 80/100 mesh
Water I.S. Ethanol
11A RM200A / Borgwaldt KC Agilent 7890A
Nic Column: Length: 2 mi.d.: 1/8"Film Thickness: 2.1 mmStationary Phase: 10%
CarboWax 20M 2% KOH
Nicotine I.S.n-Heptadecane
g.440.3s-116 / Schiltknecht
80744870 / Borgwaldt KC
Water Column: Length: 2 m
i.d.: 1/8" Stationary Phase: Porapak Q 80-200
mesh
Water I.S. Ethanol
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 66/72
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph Model/Manufacturer/Column/ Internal Standards
Airlflow Meter Model/Manufacturer
NDIR analyser Model/Manufacturer
11B RM20H / Borgwaldt KC Agilent 7890A
Nic Column: Length: 2 m
i.d.: 1/8" Film Thickness: 2.1
mm Stationary Phase: 10% CarboWax 20M 2% KOH
Nicotine I.S. n-Heptadecane
g.440.3s-116 / Schiltknecht
70740050 / Borgwaldt KC
Water Column: Length: 2 m
i.d.: 1/8" Stationary Phase: Porapak Q 80-200
mesh
Water I.S. Ethanol
12 RM20H / Borgwaldt KC Agilent 7890B
No informtion provided
Nicotine I.S. n-Heptadecane
ThermoAir3 /Schiltknecht
CO-Analysr / Borgwaldt KC
No informtion provided
Water I.S. Ethanol
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 67/72
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph Model/Manufacturer/Column/ Internal Standards
Airlflow Meter Model/Manufacturer
NDIR analyser Model/Manufacturer
13 SM450 / Cerulean Agilent 6890
Nicotine Column:Stainless
Steel, 1/8" O.D.7% Carbowas 20M, 2% KOH, 3% OS-138 on Chromosorb W-HP, 80/100 mesh
Nicotine I.S.n-Heptadecane
ThermoAir2 /Schiltknecht
COA205 / Cerulean
Water Column: Stainless Steel, 1/8"
O.D. Porapak QS, 80/100
mesh
Water I.S. Ethanol
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 68/72
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph Model/Manufacturer/Column/ Internal Standards
Airlflow Meter Model/Manufacturer
NDIR analyser Model/Manufacturer
14A RM20H / Borgwaldt KC Agilent 7890B
Nic Column: Length: 5 m
i.d.: Film Thickness:
Stationary Phase: DB-WAXETR
Nicotine I.S. C-17
Schiltknecht g.440.3s-113
Built in RM20H Water Column: Length: 25 m
i.d.: Film Thickness:
Stationary Phase: PoraPLOT Q
Ethanol
14B RM20H / Borgwaldt KC Agilent 7890B
Nic Column: Length: 5 m
i.d.: Film Thickness:
Stationary Phase: DB-WAXETR
Nicotine I.S. C-17
Schiltknecht Model G.440.3s-113
Built in RM20H Water Column: Length: 25 m
i.d.: Film Thickness:
Stationary Phase: PoraPLOT Q
Water I.S. Ethanol
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 69/72
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph Model/Manufacturer/Column/ Internal Standards
Airlflow Meter Model/Manufacturer
NDIR analyser Model/Manufacturer
15 RM20D / Borgwaldt KC HP 6890
Agilent 7890A
Nicotine Column: Stainless Steel,
1/8" O.D. 7% Carbowas 20M, 2% KOH, 3% OS-
138 on Chromosorb W-HP, 80/100
mesh
Nicotine I.S. n-
Heptadecane
Schiltknecht ThermoAir3
odel G.440.3s-113
CO/CO2 - C24 Analyser/ Borgwaldt
KC Water Column: Length: 30m i.d.: 0.320mm
Film Thickness: 20µm
Stationary Phase: HP-PLOT/Q
Water I.S. Ethanol
15 RM20D_1&2 / Borgwaldt KC HP 6890Agilent
7890A
Nic Column: Length: 6' stainless
steel packedi.d.: not givenFilm
thickness: Stationary Phase:
Supelco 10% Carbowax 20M /
Chromosorb WAW
Nicotine I.S.n-heptadecane
SchiltknechtAir flow meter Thermo Air
Borgwaldt KC CO/CO2 -C24 Analyser
Water Column: Length: 6'7 x 1/8"
O.D. stainless steel i.d.: not given
Film Thickness: Stationary Phase: Supelco Haye Sep
Q
Water I.S. Methanol
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 70/72
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph Model/Manufacturer/Column/ Internal Standards
Airlflow Meter Model/Manufacturer
NDIR analyser Model/Manufacturer
16A RM200A / Borgwaldt Agilent 7890B
Nic Column: Length: 5 m i.d.: 0.2 mm
Film thickness: 0.40 µm
Stationary Phase: DB-Waxetr 128-
7323 Agilent
Nicotine I.S. n-heptadecane
g.440.3s-181 / Schiltknecht
CO Analyser / Borgwaldt KC Water Column:
Stainless Steel Packed
Length: 2 m i.d.: 2 mm
Film Thickness: Stationary Phase:
PorapakQS 80/100 mesh
Water I.S. Ethanol
16B RM200A / Borgwaldt Agilent 7890B
Nic Column: Length: 5 mi.d.: 0.2 mmFilm thickness: 0.40 µmStationary Phase: DB-Waxetr 128-7323 Agilent
Nicotine I.S.n-heptadecane
g.440.3s-181 / Schiltknecht
CO Analyser / Borgwaldt KC
Water Column: Stainless Steel
Packed Length: 2 m i.d.: 2 mm
Film Thickness: Stationary Phase:
PorapakQS 80/100 mesh
Water I.S. Ethanol
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 71/72
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph Model/Manufacturer/Column/ Internal Standards
Airlflow Meter Model/Manufacturer
NDIR analyser Model/Manufacturer
16C RM200A / Borgwaldt Agilent 7890B
Nic Column: Length: 5 m i.d.: 0.2 mm
Film thickness: 0.40 µm
Stationary Phase: DB-Waxetr 128-
7323 Agilent
Nicotine I.S. n-heptadecane
g.440.3s-181 / Schiltknecht
CO Analyser / Borgwaldt KC Water Column:
Stainless Steel Packed
Length: 2 m i.d.: 2 mm
Film Thickness: Stationary Phase:
PorapakQS 80/100 mesh
Water I.S. Ethanol
17 SM450 / Cerulean HP 5890, 6890 &
7890
Nic Column: Length: 6' X 1/8"
i.d.: Film thickness:
Stationary Phase: 16% Aoiezon L + 2
% KOH + 2 % Carbowax 20M
80/100
Nicotine I.S. Anethole
ThermoAir2 / Schiltknecht
COA / Cerulean
Water Column: Length: 6' X 1/8"
i.d.: Film Thickness:
Stationary Phase: PorapakQ 80/100
mesh
Water I.S. Methanol
RAC-224-CTR CM9 Coll. Study 2019 – August 2020 72/72
Lab Code
Smoking Machine Model Manufacturer
Gas Chromatograph Model/Manufacturer/Column/ Internal Standards
Airlflow Meter Model/Manufacturer
NDIR analyser Model/Manufacturer
18 LX20 / Borgwaldt Agilent 7890A
Nic Column: Length: 30 m
i.d.: 0.320 Film thickness: 0.25 Stationary Phase:
Carbowax/20M
Nicotine I.S. n-
Heptadecane
ThermoAir6 / Schiltknecht
CX25 / Borgwaldt Water Column: Length: 15 m
i.d.: 0.320 Film Thickness: 20 Stationary Phase:
HP Plot/Q
Water I.S. Ethanol
Page 1 of 12
Routine Analytical Chemistry Sub-Group
Collaborative Study
ANNUAL STUDY OF THE CORESTA MONITOR
TEST PIECE CM9 2019
EXPERIMENTAL PROTOCOL
Linda A. Crumpler, Cerulean, USA
6 June 2019
Page 2 of 12
Foreword
This CORESTA protocol describes the elements that the Standards Task Force has identified
as important for describing elements of an experimental protocol for a collaborative study or
a proficiency study as defined below (Horwitz 862):
• Collaborative study
“A collaborative study is an interlaboratory study in which each laboratory uses the
defined method of analysis to analyse identical portions of homogeneous materials to
assess the performance characteristics obtained for that method of analysis.”
CORESTA recognizes that collaborative studies require considerable effort and
should be conducted only on methods that have received adequate prior testing.
• Proficiency Study
“A proficiency study is an interlaboratory study consisting of one or more assays-
conducted by a group of laboratories on one or more identical materials, by whatever
method is in use in each laboratory, for the purpose of comparing the results of each
laboratory with those of other laboratories, with the objective of evaluating or
improving performance.”
Proficiency studies often serve as pre-work for selecting a method for a full
collaborative study.
Page 3 of 12
Table of Contents
Foreword ..........................................................................................................................................2
1. Introduction ...........................................................................................................................4
2. Objectives .............................................................................................................................4
3. Study Coordinator(s) .............................................................................................................4
4. Normative References ...........................................................................................................4
5. Methods ................................................................................................................................5
6. Target Variables and Data Reporting ....................................................................................8
7. Study Time Table ................................................................................................................10
8. Data Submission .................................................................................................................10
9. Explanation of Minimum Statistics to be Applied for a Collaborative Study .....................10
Bibliography .................................................................................................................................11
Appendix A – Système International (SI) Units and their Symbols ...............................................12
Page 4 of 12
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 CM9.
2. Objectives
This year’s study will have expanded objectives that include smoking the monitor test piece
under both ISO and a specified intense smoking regime. The study objectives are:
• To measure mainstream smoke yields of nicotine-free dry particulate matter
(NFDPM), nicotine and carbon monoxide (CO) when smoked under ISO and a
specified intense smoking regime
• To establish the conditioned weight of CM8 prior to smoking
• To determine intra- and inter-laboratory variability for the measured smoke yields and
to continue this comparison over time
• To obtain statistical information about possible differences in smoke yields from
different smoking machines
3. Study Coordinator(s) Linda A. Crumpler
Linda.crumpler@cerulean.com
Phone: +1 336-778-9282 Mobile: +1 804-274-0085
4. Normative References
The relevant Standards for ISO, Intense smoking and statistical analyses are:
Definitions and standard conditions ISO 3308
Conditioning ISO 3402
TPM / NFDPM ISO 4387
Carbon monoxide ISO 8454
Nicotine ISO 10315
Water (GC) ISO 10362-1
Statistical Analysis ISO 5725-2
Ventilation zone blocking, puffing parameters, and number of test pieces smoked
*Health Canada Method T-115 paragraph 16.1
Tar and Nicotine and
CO T-115e4.pdf
*Note: T-115 has been removed from the Health Canada website and therefore is embedded
here.
Page 5 of 12
5. Methods
5.1. General Guidance
As a general guide, experiments conducted under each puffing regime should be conducted
according to ISO standard requirements. Exceptions to this guiding principle include the
puffing parameters applied for intense smoking regime, the vent blocking applied, the
number of cigarettes smoked per sample and the butt length for smoking. The study (the
smoking results) and the daily use of the monitor are based on a fixed butt length of 33
mm forCM9.
Please note that any operating conditions (a) not specified in the above ISO standards, or
regarded as optional, (b) not specified in the intense method documents provided as
guidelines and (c) any circumstances that may have influenced test results should be noted in
the test report.
Puffing parameter and vent blocking specifications for each puffing regime are summarized
in Table 1. Note: Although the CORESTA Monitor Test Pieces are unventilated it is advised
to follow the Health Canada procedures exactly and tape the filter ventilation zone.
Table 1: Smoking Regime Specifications
Smoking Regime
Puff Volume
(mL)
Puff Frequency*
(s)
Puff Duration
(s)
Vent Blocking
(%) Description
1 35 ± 0.3 60 ± 0.5 2 ± 0.02 0 ISO
2 55 ±0.5 30 ± 1.0 2 ± 0.02 100 Intense
5.2. Test Specimen(s) CM9 test piece.
5.3. Sampling
Each participating laboratory is responsible for procuring their own supply of CM9 through
the normal channels (Borgwaldt KC or Cerulean). The smoking plans will use 200 test
pieces for each rotary smoking machine or 220 test pieces for each linear smoking machine
included in the study. A composite of all packs should be prepared for conditioning
according to ISO 8243:2006. If a substantial period of time is expected to occur between
the times when the test pieces are smoked with the different smoking regimes, then two
separate composite samples should be prepared, one for each smoking regime.
5.4. Ventilation Zone Blocking for Intense Smoking
The blocking of the filter ventilation zone will be achieved by wrapping a single layer of
invisible tape, 19.0 mm wide or equivalent, around the complete circumference of the filter and
tipping paper of the test articles.
5.5. Butt Marking
Page 6 of 12
For the purpose of this study the CM9 test pieces will be butt marked to a fixed butt length of
33 mm.
5.6. Conditioning
The composite samples shall be conditioned for at least 48 hours but no more than 10 days
under the following conditions:
Temperature: 22 ± 1°C Relative humidity: 60 ± 3%
Temperature and relative humidity of the conditioning enclosure (chamber or room) shall be
checked and recorded for every smoking run.
Test cigarettes to be smoked for the determination of NFDPM, nicotine and CO should be
selected at random from the conditioned cigarettes.
Any test pieces with visible defects shall be discarded.
5.7. Test Piece Weight
The test articles will be weighed for ISO smoking only since the ventilation zone blocking tape
applied for intense smoking may vary between laboratories. The weight of the test piece after
conditioning is to be determined by weighing all test pieces to be smoked just before they are
placed at the smoking machine. The result is reported as the mean weight of the 20 test pieces
for linear or rotary smoking machine at ISO puffing parameters.
5.8. Smoking Machine
Where smoking laboratories have more than one type of smoking machine (i.e. linear and rotary
variants) they are encouraged to include as many types in the study as possible.
5.9. Smoking Plans
The smoking plans will incorporate one product (CM9), shown as M in the smoking plans.
These plans are designed to smoke the CM9 in all ports for each puffing regime, spread over a
number of days. If possible, each participating laboratory should use only one operator (for
each smoking machine type) throughout the course of the study.
For ISO smoking, one test result is defined as the mean yield obtained from smoking 20 test
pieces in a single smoking machine run, therefore from a rotary machine it is the result from one
run smoking 20 test pieces and from a linear machine it is the average of four ports, smoking five
test pieces per port. This is repeated on five separate days resulting in 100 test pieces being
smoked (Tables 2-3).
For Intense smoking, the number of test pieces smoked per filter pad is reduced to avoid
overloading the pad. As a consequence, the number of smoking runs/ports has to be increased
so that the same nominal numbers of test pieces are smoked. Thus, a test result from a rotary
machine is the mean of two runs, each of 10 test pieces, and from a linear machine it is the
average of eight ports, smoking three test pieces per port (Tables 4-5).
Page 7 of 12
Note that the side seam of the test pieces should be positioned at random and not in a fixed
position since it has been observed that some laboratory staff habitually place cigarettes in a
particular orientation. Ports not occupied by the test pieces are left blank, which may be
assigned to any other cigarette that is to be smoked by the laboratory, or the ports may be left
empty.
Table 2: Smoking Plan for 20-port Linear Machines for ISO smoking (5 test pieces per
pad)
Port number
Day
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20
1 M M M M
2 M M M M
3 M M M M
4 M M M M
5 M M M M
Table 3: Smoking Plan for 20-port Rotary Machines for ISO smoking (20 test pieces per
pad)
Day Run Test
Piece
1 1 M
2 2 M
3 3 M
4 4 M
5 5 M
Page 8 of 12
Table 4: Smoking Plan for 20-port Linear Machines for Intense smoking (3 test
pieces per pad)
Day
Ru
n Port number
1 2 3 4 5 6 7 8 9 10
11
12
13
14
15
16
17
18
19
20
1 6 M M M M
7 M M M M
2 8 M M M M
9 M M M M
3 10 M M M M
11 M M M M
4 12 M M M M
13 M M M M
5 14 M M M M
15 M M M M
Table 5: Smoking Plan for 20-port Rotary Machines for Intense smoking (10 test pieces
per pad)
Day Run Test Piece
1 6 M
7 M
2 8 M
9 M
3 10 M
11 M
4 12 M
13 M
5 14 M
15 M
6. Target Variables and Data Reporting
The variables to be reported fall into two categories: those which will form the basis of the
statistical evaluation of the data and those that are ancillary to the test.
The variables to be reported for statistical analysis are:
• Mean weight of the Monitor after conditioning (just prior to smoking)
• Mean puff number per test piece
• Mean TPM per test piece
• 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:
Page 9 of 12
• 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:
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 ###.#
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.
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 ##.##
Page 10 of 12
7. Study Time Table
The smoking should be performed during June and July 2019. Strict adherence to the
timeline is very important for the data to be compiled for an initial assessment at the next
Sub-Group meeting in October, 2018 . Data not received by August 19, 2019 will be
excluded from the formal statistical analysis. Please review your data carefully before
submitting as the statistical analysis is very labor intensive.
The statistical analysis of the results will follow as closely as possible the recommendations
of ISO 5725.
Should any questions arise please contact the study coordinator, Linda Crumpler.
All results must be sent via e-mail to:
Linda A. Crumpler linda.crumpler@cerulean.com
8. Data Submission
All results must be sent via e-mail to:
Linda A. Crumpler linda.crumpler@cerulean.com
9. Explanation of Minimum Statistics to be Applied for a Collaborative
Study At a minimum Repeatability and Reproducibility estimation will be applied.
Page 11 of 12
Bibliography
Chem, Pure Appl. QUALITY ASSURANCE SCHEMES THE INTERNATIONAL
HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL
CHEMISTRY LABORATORIES (n.d.): n. pag. Web.
Council of Science Editors. 8th ed. N.p.: Council of Science Editors, n.d. Print.
Form and Style for ASTM Standards. West Conshohocken, PA: ASTM INTERNATIONAL,
2015. Print.
Horwitz, William. "Protocol for the Design, Conduct and Interpretation of Collaborative
Studies." Pure and Applied Chemistry 60.6 (1988): 855-64. ShareGate. International Union
of Pure and Applied Chemistry, De Gruyter, Jan. 1988. Web. 30 July 2015.
ISO 5725 Standard And Reference Laboratories Error.pdf. "ISO 5252." ISO 5725 Standard
And Reference Laboratories Error (n.d.): n. pag. Web.
"IUPAC 2006 IUPAC, Pure and Applied Chemistry 78, 145–196"" N.p., n.d. Web. 25 Aug.
2015.
"Numbers, Units, Mathematicial Expressions, and Statistics." Scientific Style and Format;
The CSE Manual for Authors Editors, and Publishers. 8th ed. Chicago: The University of
Chicago, 2014. 157-91. Print.
Page 12 of 12
Appendix A – Système International (SI) Units and their Symbols
SI base units
Base Quantity Name Symbol
Length meter m Mass kilogram Kg
Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd
SI derived units
Derived Quantity Name Symbol Equivalent SI Units
Frequency hertz Hz s-1
Force newton N m·kg·s-2
Pressure pascal Pa N/m
2
Energy joule J N·m Power watt W J/s
Electric charge coulomb C s·A Electric potential volt V W/A Electric resistance ohm Ω V/A
Celsius temperature Degrees Celsius °C K*
*Unit degree Celsius is equal in magnitude to unit kelvin
SI prefixes
Factor Name Symbol Numerical value
1012 tera T 1 000 000 000 000
109 giga G 1 000 000 000
106 mega M 1 000 000
103 kilo k 1 000
102 hecto h 100
101 deka da 10
10-1 deci d 0.1
10-2 centi c 0.01
10-3 milli m 0.001
10-4 micro µ 0.000 001
10-6 nano n 0.000 000 001
10-7 pico p 0.000 000 000 001
top related