Routine Analytical Chemistry Sub-Group · RAC-224-CTR CM9 Coll. Study 2019 – August 2020 3/72 1....

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


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.


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


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


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


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


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


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


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


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


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


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


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


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


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


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


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 [%]


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.)


Table 20: r&R estimations for CM9 under ISO 3308 smoking regime (linear machines)

p n Global Mean

Sr CVr [%]

r SR CVR [%]


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.)



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.)


Table 22: r&R estimations for CM9 under ISO Intense 20778 smoking regime (rotary machines)

p n Global Mean

Sr CVr [%]

r SR CVR [%]


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.)


Table 23: r&R estimations for CM9 under ISO Intense 20778 smoking regime (linear machines)

p n Global Mean

Sr CVr [%]

r SR CVR [ %]


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.)


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.


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


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


Figure 5: CM9 Individual observations of mainstream ISO 3308 NFDPM

Straggler value in orange

Figure 6: CM9 Individual observations of mainstream ISO 3308 CO



Figure 7: CM9 Individual observations of mainstream ISO 3308 PUFF Count


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



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


Figure 12: CM9 Individual observations of mainstream ISO Intense 20778 CO


Figure 13: CM9 Individual observations of mainstream ISO Intense 20778 PUFF Count


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.


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.


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.


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.


APPENDIX B – Experimental Protocol

Adobe Acrobat

Document


APPENDIX C – Departures from Experimental Protocol

No departures from experimental protocol.


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


Lab count

Machine Count

Lab Code

Machine Class

Machine Type

Run No.


TPM (mg/t.p.)

Water (mg/t.p)

Nicotine (mg/t.p)

NFDPM (mg/t.p)

CO (mg/t.p)

Puff Count

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


Lab count

Machine Count

Lab Code

Machine Class

Machine Type

Run No.


TPM (mg/t.p.)

Water (mg/t.p)

Nicotine (mg/t.p)

NFDPM (mg/t.p)

CO (mg/t.p)

Puff Count

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


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


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


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



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



WOULD EXCEED 2/9

NO


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)


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)


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)


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)


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)


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)


Figure 13: CM9 under ISO intense 20778 smoking regime – r and R values (puff count)


APPENDIX G – Rotary Smoking Machines

1. ISO 3308 smoking regime






Outlier values in red, straggler values in orange



2. Intense ISO 20778 smoking regime




Figure 9: CM9 Individual observations of mainstream “Intense” Nicotine



APPENDIX H – Linear Smoking Machines

1. ISO Smoking regime






Straggler value in orange, outlier values in red



2. ISO Intense 20778 smoking regime




Figure 9: CM9 Individual observations of mainstream ISO Intense 20778 Nicotine





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


Porapak Q

Water I.S. Ethanol


Lab Code





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


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


Lab Code





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


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


Stationary Phase: Polystyrene-

divinylbenzene

Water I.S. Ethanol


Lab Code





5B RM20H / Borgwaldt KC Agilent 7890A

Nic Column: Length: 15m i.d.: 0.32mm


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


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


Lab Code





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


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


Stationary Phase: HP-INNOWAX


G.440.3S / Schiltknecht

C24 / Borgwaldt KC Water Column: Length: 30 m i.d.: 0.320 mm

Film Thickness: 20 µm


Water I.S. Ethanol


Lab Code





8B RM20H / Borgwaldt KC

6890 N / Agilent (Nic)

7890 / Agilent (Water)

Nic Column: Length: 30 m i.d.: 0.32mm


Stationary Phase: HP-INNOWAX


G.440.3s-113 / Schiltknecht

C24 / Borgwaldt KC Water Column: Length: 30 m i.d.: 0.320 mm

Film Thickness: 20 µm


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



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


Lab Code





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


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


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


Lab Code





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



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


ThermoAir3 /Schiltknecht

CO-Analysr / Borgwaldt KC

No informtion provided

Water I.S. Ethanol


Lab Code





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


ThermoAir2 /Schiltknecht

COA205 / Cerulean

Water Column: Stainless Steel, 1/8"

O.D. Porapak QS, 80/100

mesh

Water I.S. Ethanol


Lab Code





14A RM20H / Borgwaldt KC Agilent 7890B


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


Stationary Phase: PoraPLOT Q

Ethanol

14B RM20H / Borgwaldt KC Agilent 7890B



Stationary Phase: DB-WAXETR

Nicotine I.S. C-17

Schiltknecht Model G.440.3s-113

Built in RM20H Water Column: Length: 25 m


Stationary Phase: PoraPLOT Q

Water I.S. Ethanol


Lab Code





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


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


Lab Code





16A RM200A / Borgwaldt Agilent 7890B



Stationary Phase: DB-Waxetr 128-

7323 Agilent

Nicotine I.S. n-heptadecane


CO Analyser / Borgwaldt KC Water Column:

Stainless Steel Packed

Length: 2 m i.d.: 2 mm


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


CO Analyser / Borgwaldt KC

Water Column: Stainless Steel

Packed Length: 2 m i.d.: 2 mm



Water I.S. Ethanol


Lab Code





16C RM200A / Borgwaldt Agilent 7890B



Stationary Phase: DB-Waxetr 128-

7323 Agilent

Nicotine I.S. n-heptadecane


CO Analyser / Borgwaldt KC Water Column:

Stainless Steel Packed

Length: 2 m i.d.: 2 mm



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


COA / Cerulean

Water Column: Length: 6' X 1/8"


Stationary Phase: PorapakQ 80/100

mesh

Water I.S. Methanol


Lab Code





18 LX20 / Borgwaldt Agilent 7890A


i.d.: 0.320 Film thickness: 0.25 Stationary Phase:

Carbowax/20M

Nicotine I.S. n-

Heptadecane


CX25 / Borgwaldt Water Column: Length: 15 m

i.d.: 0.320 Film Thickness: 20 Stationary Phase:

HP Plot/Q

Water I.S. Ethanol

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

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Foreword

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

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

a proficiency study as defined below (Horwitz 862):

• Collaborative study

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

defined method of analysis to analyse identical portions of homogeneous materials to

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

CORESTA recognizes that collaborative studies require considerable effort and

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

• Proficiency Study

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

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

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

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

improving performance.”

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

collaborative study.

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

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1. Introduction

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

organize the annual testing of the CORESTA Monitor test piece. This year the study will

include 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

[email protected]

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.

mailto:[email protected]

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5. Methods

5.1. General Guidance

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

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

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

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

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

mm 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

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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).

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

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

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

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

empty.

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

pad)

Port number

Day

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

1 M M M M

2 M M M M

3 M M M M

4 M M M M

5 M M M M

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

pad)

Day Run Test

Piece

1 1 M

2 2 M

3 3 M

4 4 M

5 5 M

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

pieces per pad)

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:

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• 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 ##.##

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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 [email protected]

8. Data Submission

All results must be sent via e-mail to:

Linda A. Crumpler [email protected]

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

Study At a minimum Repeatability and Reproducibility estimation will be applied.



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Bibliography

Chem, Pure Appl. QUALITY ASSURANCE SCHEMES THE INTERNATIONAL

HARMONIZED PROTOCOL FOR THE PROFICIENCY TESTING OF ANALYTICAL

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

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

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

2015. Print.

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

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

of Pure and Applied Chemistry, De Gruyter, Jan. 1988. Web. 30 July 2015.

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

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

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

2015.

"Numbers, Units, Mathematicial Expressions, and Statistics." Scientific Style and Format;

The CSE Manual for Authors Editors, and Publishers. 8th ed. Chicago: The University of

Chicago, 2014. 157-91. Print.

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

SI base units

Base Quantity Name Symbol

Length meter m Mass kilogram Kg

Time second s Electric current ampere A Temperature kelvin K Amount of substance mole mol Luminous intensity Candela cd

SI derived units

Derived Quantity Name Symbol Equivalent SI Units

Frequency hertz Hz s-1

Force newton N m·kg·s-2

Pressure pascal Pa N/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

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