1、 Reference number ISO/TR 22305:2006(E) ISO 2006TECHNICAL REPORT ISO/TR 22305 First edition 2006-06-01 Cigarettes Measurement of nicotine- free dry particulate matter, nicotine, water and carbon monoxide in cigarette smoke Analysis of data from collaborative studies reporting relationships between re
2、peatability, reproducibility and tolerances Cigarettes Dtermination de la matire particulaire anhydre et exempte de nicotine, de la nicotine, de leau et du monoxyde de carbone dans la fume de cigarette Analyse des donnes provenant dtudes collectives et traitant des relations entre la rptabilit, la r
3、eproductibilit et les tolrances ISO/TR 22305:2006(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and installed on the comput
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6、entral Secretariat at the address given below. ISO 2006 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either IS
7、O at the address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2006 All rights reservedISO/TR 22305:2006(E) ISO 200
8、6 All rights reserved iii Contents Page Foreword iv Introduction v 1 Scope1 2 Statistical functions for repeatability (r), reproducibility (R) of yield measurements and compliance tolerances for declared smoke constituent yields 1 2.1 Statistical functions for repeatability (r) and reproducibility (
9、R) 1 2.2 A statistical model for compliance tolerances .2 3 Sources of data3 3.1 International collaborative studies 3 3.2 UK Department of Health Cigarette Survey data 4 4 Comparison of 2003 CORESTA Collaborative Study data with those previously reported.4 4.1 General4 4.2 Comparison of repeatabili
10、ty r 20values from CCS-03 with other collaborative studies.4 4.3 Comparison of reproducibility R 20values from CCS-03 with other collaborative studies 5 4.3.1 General5 4.3.2 Relationship between reproducibility R 20and smoke constituent yield .5 4.4 Comparison of R 100reproducibility values from col
11、laborative studies with measurement tolerances estimated from the UK Department of Health Cigarette Survey data .5 5 Review of information relevant to setting a compliance tolerance for carbon monoxide.6 5.1 General6 5.2 Compliance data for current tolerances6 5.3 Confidence intervals associated wit
12、h yield measurements6 5.4 Statistical models 7 5.5 Prediction of a tolerance for CO from the relative variability in their reproducibility values8 6 Conclusions .8 7 Recommendations.8 Annex A (informative) Background considerations on the choice of sampling procedures 31 Annex B (informative) The de
13、termination of carbon monoxide in cigarette smoke Problems in the evaluation of results .33 Annex C (informative) Proposals from the UK Tobacco Manufacturers Association for a practicable tolerance for verifying cigarette packet declarations of carbon monoxide (March, 2002)41 Annex D (informative) A
14、nalysis of bias measurements from the UK Department of Health Cigarette Survey 59 Annex E (informative) ASIA COLLABORATIVE STUDY #11 2002/2003 .71 Annex F (informative) 2003 CORESTA Collaborative Study Report CORESTA study for the estimation of the repeatability and reproducibility of the measuremen
15、t of nicotine-free particulate matter, nicotine and CO in smoke using the ISO smoking methods, September 2003 .86 Bibliography 146 ISO/TR 22305:2006(E) iv ISO 2006 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bod
16、ies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organization
17、s, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the I
18、SO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the
19、 member bodies casting a vote. In exceptional circumstances, when a technical committee has collected data of a different kind from that which is normally published as an International Standard (“state of the art”, for example), it may decide by a simple majority vote of its participating members to
20、 publish a Technical Report. A Technical Report is entirely informative in nature and does not have to be reviewed until the data it provides are considered to be no longer valid or useful. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
21、rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO/TR 22305 was prepared by Technical Committee ISO/TC 126, Tobacco and tobacco products. ISO/TR 22305:2006(E) ISO 2006 All rights reserved v Introduction 0.1 Summary The purpose of this Technical Report is to
22、review the smoke yield data provided to Working Group ISO/TC 126/WG 8 “Confidence intervals for the determination of carbon monoxide” and to use it as the basis for proposing a tolerance for checks of declared carbon monoxide yields. There are many laboratories around the world routinely measuring t
23、he nicotine-free dry particulate matter (NFDPM), nicotine and carbon monoxide yield of cigarette brands. They can, in general, be divided into two types: those run by cigarette manufacturers for quality monitoring and those run or contracted by regulators to check the yield information provided by m
24、anufacturers. These laboratories need to assess their performance against others to ensure the reliability of their measurements. Their wide geographical spread limits such assessments on a national basis, so that international collaborative studies provide the most practical means and generate data
25、 sets on a regular basis. In addition to allowing individual laboratories to rank their measurements relative to others, the studies also establish confidence intervals (CIs) for the repeatability (r 20 ) 1)of the measurements in a single laboratory and reproducibility (R 20 ) 2)in different laborat
26、ories. The reported r and R values from each study have been used in isolation but when combined, as in this report, provide a means of assessing if newly reported values are outside the expected range. The values from the latest 2003 CORESTA study are compared in this way and found to be within the
27、 previously reported range of values but at the lower end. There is no hard evidence, therefore, that the harmonization work on smoking machines has reduced the variability in CO yield measurements, but the data have been shown to be as good as the best previously reported. For this reason, and beca
28、use it was a large study including all current designs of smoking machine, it provides the most appropriate data for estimating compliance tolerances. The measurement CIs represented by r 20and R 20provide a starting point for estimating the tolerances 3)relevant to compliance checks on the yield in
29、formation provided by manufacturers. They need to be combined with additional information on testing 4)and reporting as well as the inherent variability in the product associated with routine cigarette manufacturing. The statistical model given in this report is designed to incorporate all the relev
30、ant information to estimate compliance tolerances. The model is based upon the within and between laboratory standard deviations for tests of 100 cigarettes, together with additional terms to account for rounding the declared values and to include the product variability. A weakness in the model app
31、roach stems from the lack of data for estimating the terms relating to product variability, the only source of data being the UK Department of Health Survey, which is not specifically designed to provide such data. For this reason the model has been used in this report without including the product
32、terms and the calculated tolerance values R 100+rndg 5)compared with those from an alternative indirect prediction. Obviously, the R 1 00+rndgvalues are lower than the true compliance tolerance since they do not include the product terms. The simplest indirect way of predicting a CO tolerance is fro
33、m the measurement variability relative to NFDPM, for which an accepted tolerance exists. The ratio of the R 100+rndgvalues calculated from the CORESTA 2003 Study data was used for this purpose. 1) Based on tests of 20 cigarettes. 2) Based on tests of 20 cigarettes. 3) ISO 8243 has always included to
34、lerances for NFDPM and nicotine but an interim CO tolerance was added in 2003 whilst ISO/TC 126/WG 8 considered a permanent value. 4) See ISO 4387 and ISO 8243. 5) Based on tests of 100 cigarettes with allowance for rounding the declared value. ISO/TR 22305:2006(E) vi ISO 2006 All rights reservedISO
35、 8243 provides procedures, and tolerances 6) , for sampling both over a period of time, which is recommended, and at one point in time. Tolerances derived from both the statistical model and ratio methods for over a period of time sampling are summarized below. Parameter evaluated Carbon monoxide to
36、lerance R 100+rndg20 % with a minimum of 1,5 mg or 25 % with a minimum of 1 mg R 100+rndgratio (CO/NFDPM) 22 % with a minimum of 1,5 mg It is recommended that the compliance tolerance for CO be set at 20 % for over a period of time sampling, and 25 % for at one point in time sampling, with a minimum
37、 value of 1,5 mg. This recommendation implies a corresponding amendment of ISO 8243. It is further recommended that the tolerances and minimum values are reviewed when compliance rates are established from regulatory checks. It is possible that such data may only become available in the UK and may t
38、ake two or three years to assemble. 0.2 General Information Methods of measurement specified in ISO Standards require estimates of repeatability (r) and reproducibility (R). These are normally derived from a collaborative study conforming to the guidelines in ISO 5725-11and ISO 5725-22involving as m
39、any laboratories as possible. There is a particular problem in obtaining estimates when the measurement results in the destruction of the product sample, for example, cigarettes or fuel for internal combustion engines. If laboratories are measuring the physical dimensions of, say, metal nuts and the
40、ir bolts, measurements can be made on the same items by one operator within a laboratory (repeatability) and by different operators in many laboratories (reproducibility). In this example it is always the same set of nuts and bolts which is measured throughout the experiment. For cigarette smoke con
41、stituent determinations, the situation is entirely different. The cigarettes, once sampled and smoked, produce a set of smoke constituent estimates, each of which is perfectly valid (provided that the standard methods have been followed) but which cannot be repeated or confirmed. The only possible c
42、heck between data is to compare them with an accepted range of yield measurements. A series of ISO Standards exists to condition the cigarettes3 , to specify the smoking machine4for routine analytical smoking5and to measure smoke nicotine6 , smoke water7 8and smoke carbon monoxide (CO)9 . Variation
43、in the final yield of smoke constituent arises from all these procedures but also from manufacture of the product (see Annex A) and from the methods of sampling. These factors require the use of special procedures in collaborative tests on cigarette products. Product variability is minimized by the
44、testing of matched samples, usually taken from a single small batch production, in each participating laboratory. The samples, therefore, do not include the normal product variability and are not representative of any individual brand. The r and R values from collaborative studies are thus essential
45、ly estimates of measurement variability on near identical samples. They cannot be used directly as a tolerance for compliance checks of cigarette brands where other sources of variability must be taken into account. 6) The over a period of time tolerances are 15 % for NFDPM and nicotine, and 20 % fo
46、r CO. The tolerances when sampling at one point in time are increased to 20 % for NFDPM and nicotine and 25 % for CO. In both cases, a minimum value of 1 mg applies to NFDPM and CO and 0,1 mg nicotine. ISO/TR 22305:2006(E) ISO 2006 All rights reserved vii 0.3 Sampling a population of cigarettes manu
47、factured for sale ISO 824310specifies methods for sampling a population of cigarettes manufactured for sale. It also includes the expected tolerances when cigarettes brands are so sampled and when smoke components are measured using the standards detailed above. Increasing international interest and
48、 in particular the EU Directive 2001/37/EC requiring the declaration of CO yield on cigarette packs showed that revision of this standard was urgent. ISO/TC 126 therefore decided in 2003 to set up a working group WG 8 with the task of first making a revision to add a tolerance for CO to the 1991 edi
49、tion of the standard, and then to continue to revise and if possible, simplify the text of the standard. The first task was accomplished and ISO 8243 was published in 2003 as a minor revision. The tolerance for CO was included on the basis of existing studies showing the need for a higher tolerance than for NFDPM. However, further collaborative studies were conducted concurrently and the purpose of this Technical Report is to record the data from these studies and to compare them with other sources of d
