1、January 2011 Translation by DIN-Sprachendienst.English price group 13No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).IC
2、S 65.160!$ll“1739173www.din.deDDIN ISO 4387Cigarettes Determination of total and nicotine-free dry particulate matter using aroutine analytical smoking machine (ISO 4387:2000 + Amd.1:2008)English translation of DIN ISO 4387:2011-01Zigaretten Bestimmung des Rohkondensats und des nikotinfreien Trocken
3、kondensats unterVerwendung einer Zigaretten-Abrauchmaschine fr Routineanalysen (ISO 4387:2000 +Amd.1:2008)Englische bersetzung von DIN ISO 4387:2011-01Cigarettes Dtermination de la matire particulaire totale et de la matire particulaire anhydre etexempte de nicotine au moyen dune machine fumer analy
4、tique de routine(ISO 4387:2000 + Amd.1:2008)Traduction anglaise de DIN ISO 4387:2011-01SupersedesDIN ISO 4387:2000-12www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.2204.11 DIN ISO 4387:2011-01 2 A comma is used as the decimal mark
5、er. Contents Page National foreword 3 National Annex NA (informative) Bibliography.4 Introduction .5 1 Scope 6 2 Normative references 6 3 Terms, definitions and abbreviated terms .6 4 Principle7 5 Apparatus 8 6 Sampling.8 7 Determination of total particulate matter .8 7.1 Preparation of the cigarett
6、es for smoking .8 7.2 Marking the butt length 10 7.3 Selection of cigarettes 10 7.4 Conditioning.10 7.5 Preliminary tests before smoking 11 7.6 Smoking and collection of particulate matter.11 7.7 Determination of total particulate matter .13 7.8 Calculation of total particulate matter 13 7.9 Treatme
7、nt of total particulate matter 13 8 Test report .14 9 Repeatability and reproducibility .16 Annex A (informative) Smoking plans.17 Bibliography 22 DIN ISO 4387:2011-01 National foreword This standard has been prepared by Technical Committee ISO/TC 126 “Tobacco and tobacco products” (Secretariat: DIN
8、, Germany). The responsible German body involved in its preparation was the Normenausschuss Lebensmittel und landwirtschaftliche Produkte (Food and Agricultural Products Standards Committee), Working Committee NA 057-04-01 AA Tabak und Tabakerzeugnisse. The standardization of the determination of th
9、e total particulate matter in cigarettes using a routine analytical smoking machine was included in the work programme of Technical Committee ISO/TC 126 during its constituent meeting in Berlin in 1968. After revision of the second edition of the International Standard ISO 4387, the third edition wa
10、s published in 2000. In 2008 an Amendment was published in which it was explained that no machine smoking regime can represent all human smoking behaviours. The DIN Working Committee decided to incorporate the 2008 Amendment to ISO 4387 into DIN ISO 4387, which had been published in 2000. The Workin
11、g Committee came to this decision in consideration of the necessary harmonization of international and national standards on smoking analysis. Amendments are indicated by a vertical line in the left margin next to the text. Attention is drawn to the possibility that some of the elements of this docu
12、ment may be the subject of patent rights. DIN shall not be held responsible for identifying any or all such patent rights. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 3308 DIN ISO 3308 ISO 3402 DIN ISO 3402 ISO 8243 DIN ISO 8243 ISO
13、 10315 DIN ISO 10315 ISO 10362-1 DIN ISO 10362-1 Amendments This standard differs from DIN ISO 4387:2000-12 as follows: a) ISO 4387:2000/Amd.1:2008, stating that no machine smoking regime can represent all human smoking behaviours, has been incorporated in the Introduction. The technical substance o
14、f the standard has not been changed. Previous editions DIN 10240-2: 1982-02 DIN 10240-3: 1978-04 DIN ISO 4387: 1992-07; 2000-12 3 DIN ISO 4387:2011-01 National Annex NA (informative) Bibliography DIN ISO 3308, Routine analytical cigarette-smoking machine Definitions and standard conditions DIN ISO 3
15、402, Tobacco and tobacco products Atmosphere for conditioning and testing DIN ISO 8243, Cigarettes Sampling DIN ISO 10315, Cigarettes Determination of nicotine in smoke condensates Gas-chromatographic method DIN ISO 10362-1, Cigarettes Determination of water in smoke condensates Part 1: Gas-chroma-t
16、ographic method 4 IntroductionCigarettes are manufactured to close tolerances using strict quality control procedures. However, all theconstituents involved in the manufacture are derived from natural products (tobacco, cigarette paper, tipping, etc.)and this results in a final product which is intr
17、insically variable. The complexity does not finish here because thecigarette is converted during smoking to cigarette smoke.Cigarette smoke is a complex mixture consisting of many individual chemical constituents. These compounds existas gases, vapours and condensed aerosol particles. Additionally,
18、various ageing processes, together withdiffusional and intersolubility effects, start occurring immediately after the formation of the smoke which furthercomplicate its composition.The quantitative measurement of nicotine-free dry particulate matter (NFDPM, sometime referred to as “tar“) is,therefor
19、e, dependent on its arbitrary definition.From the time that scientists have attempted to determine a value for NFDPM, many different methods have beenused. However, experience has shown some procedures to be more reliable and, with these factors in mind, during1988 and 1989, collaborative studies by
20、 Task Forces composed of members of the Cooperation Centre forScientific Research Relative to Tobacco (CORESTA) Smoke and Technology groups have been made on therepeatability and reproducibility of the determination of total and dry particulate matter from cigarettes.The studies show that improvemen
21、ts in repeatability and reproducibility result when some restrictions are placed onthe wide variety of methods and practices permitted by existing standard methods. Thus, this InternationalStandard, and the others which together form a complete set for the sampling, conditioning and determination of
22、nicotine, water and particulate matter from cigarettes, have been produced after much cooperation andcollaborative experimentation by many laboratories in many countries.CORESTA first published an International Standard for the machine smoking of cigarettes in 1968, and since thattime many improveme
23、nts in equipment as well as in procedure have been suggested.This International Standard incorporates these improvements and consequently represents the state of the art onthis subject and provides one set of procedures accepted as reference methods.This method is a machine method and allows cigaret
24、tes to be smoked using a strictly controlled set of parameters.Thus, it enables the NFDPM and nicotine from cigarettes, when smoked by this procedure, to be compared andranked on the basis of machine yield.No machine smoking regime can represent all human smoking behaviours: it is recommended that c
25、igarettes also be tested under conditions of a different intensity of machine smoking than those specified in this International Standard; machine smoking testing is useful to characterize cigarette emissions for design and regulatory purposes, but communication of machine measurements to smokers ca
26、n result in misunderstandings about differences in exposure and risk across brands; smoke emission data from machine measurements may be used as inputs for product hazard assessment, but they are not intended to be nor are they valid as measures of human exposure or risks. Communicating differences
27、between products in machine measurements as differences in exposure or risk is a misuse of testing using ISO standards. Cigarettes Determination of total and nicotine-free dryparticulate matter using a routine analytical smoking machine5 DIN ISO 4387:2011-01 1 ScopeThis International Standard specif
28、ies methods for the determination of total particulate matter and for thesubsequent determination of nicotine-free dry particulate matter present in the smoke from cigarettes generatedand collected using a routine analytical smoking machine.2 Normative referencesThe following normative documents con
29、tain provisions which, through reference in this text, constitute provisions ofthis International Standard. For dated references, subsequent amendments to, or revisions of, any of thesepublications do not apply. However, parties to agreements based on this International Standard are encouraged toinv
30、estigate the possibility of applying the most recent editions of the normative documents indicated below. Forundated references, the latest edition of the normative document referred to applies. Members of ISO and IECmaintain registers of currently valid International Standards.ISO 2971, Cigarettes
31、and filter rods Determination of nominal diameter Method using a laser beam measuringapparatus.ISO 3308:2000, Routine analytical cigarette-smoking machine Definitions and standard conditions.ISO 3402, Tobacco and tobacco products Atmosphere for conditioning and testing.ISO 6488-1, Tobacco Determinat
32、ion of water content Part 1: Karl Fischer method.ISO 6565, Tobacco and tobacco products Draw resistance of cigarettes and pressure drop of filter rods Standard conditions and measurement.ISO 8243, Cigarettes Sampling.ISO 10315, Cigarettes Determination of nicotine in smoke condensates Gas-chromatogr
33、aphic method.ISO 10362-1, Cigarettes Determination of water in smoke condensates Part 1: Gas-chromatographic method.ISO 16055, Tobacco and tobacco products Monitor test piece Requirements and application.3 Terms, definitions and abbreviated termsFor the purposes of this International Standard, the f
34、ollowing terms, definitions and abbreviated terms apply.3.1total particulate mattercrude smoke condensateTPMthat portion of the mainstream smoke which is trapped in the smoke trap, expressed as milligrams per cigarette6 DIN ISO 4387:2011-01 3.2dry particulate matterdry smoke condensateDPMtotal parti
35、culate matter after deduction of its water content, expressed as milligrams per cigarette3.3nicotine-free dry particulate matternicotine-free dry smoke condensateNFDPMdry particulate matter after deduction of its nicotine content, expressed as milligrams per cigarette3.4smoking processuse of a smoki
36、ng machine to smoke cigarettes from lighting to final puff3.5smoking runspecific smoking process to produce such smoke from a sample of cigarettes as is necessary for the determinationof the smoke components3.6laboratory samplesample intended for laboratory inspection or testing and which is represe
37、ntative of the gross sample or the sub-period sample3.7test samplecigarettes for test taken at random from the laboratory sample and which are representative of each of theincrements making up the laboratory sample3.8conditioning samplecigarettes selected from the test sample for conditioning prior
38、to tests3.9test portiongroup of cigarettes prepared for a single determination and which is a random sample from the test sample orconditioned sample, as appropriate3.10monitor test piececigarette taken from a batch specially fabricated under controlled manufacturing conditionsNOTE The cigarettes of
39、 such a batch show the greatest possible homogeneity with regard to their physical and chemicalcharacteristics.4PrincipleThe test cigarettes are sampled then conditioned. The test cigarettes are smoked on an automatic smokingmachine with simultaneous collection of total particulate matter in a glass
40、 fibre filter trap. If used, the consistency ofthe laboratory smoking process and subsequent analytical procedures are controlled by using monitor test piecesspecified in ISO 16055. The mass of the total particulate matter so collected is determined gravimetrically. The totalparticulate matter is ex
41、tracted from the trap for determination of the water and nicotine contents by gaschromatography.7 DIN ISO 4387:2011-01 NOTE In the countries that are not in a position to use gas-chromatographic methods, reference should be made toISO 3400 for the determination of total nicotine alkaloids, and the d
42、etermination of water in smoke condensate should beperformed by the method described in ISO 10362-2. In such cases, values obtained for nicotine and water in smoke condensatemay be used with the addition of a note made in the expression of the result.5 ApparatusNormal laboratory apparatus and, in pa
43、rticular, the following items.5.1 Routine analytical cigarette-smoking machine, complying with the requirements of ISO 3308.5.2 Soap bubble flow meter, graduated at 35 ml to an accuracy of Gb1 0,2 ml and with a resolution of 0,1 ml.5.3 Apparatus for the determination of puff duration and frequency.5
44、.4 Analytical balance, suitable for measuring to the nearest 0,1 mg.The weighing of filter pad holders may be affected by static electricity, necessitating the use of an antistatic device.5.5 Conditioning enclosure, carefully maintained under the conditions specified in ISO 3402.5.6 Length-measuring
45、 device, suitable for measuring to the nearest 0,5 mm.5.7 Device for the determination of diameter, in accordance with ISO 2971.If such apparatus is not available, the diameter may be determined from the circumference by slitting the cigarettelongitudinally, removing and flattening the paper then me
46、asuring its width.5.8 Smoke trap sealing device, end caps made from a non-hygroscopic and chemically inert material.5.9 Gloves, made of cotton, or the non-talc surgical type.6 SamplingA laboratory sample (3.6) shall be taken by a sampling scheme such as one of those given in ISO 8243.This sample wil
47、l normally contain cigarettes taken from different parts of the population. Make up the test sample(3.7) required for the test by randomly selecting cigarettes from the different parts of the population represented inthe laboratory sample.7 Determination of total particulate matter7.1 Preparation of
48、 the cigarettes for smoking7.1.1 GeneralIf N cigarettes of a given type are to be smoked, C Gb4 N cigarettes shall be prepared from Q cigarettes forconditioning and butt marking.The symbols used in this clause are as follows:N is the number of cigarettes of a given type to be smoked, resulting from
49、sampling at one point in time orfrom a sub-period sample;8 DIN ISO 4387:2011-01 C is a multiplying factor, of value greater than 1, to allow for loss due to damage or selection proceduresbetween initial sampling and smoking;Q is the total number of cigarettes available (laboratory sample, see 3.6);n is the number of replicate determinations of total particulate matter;q is the number of cigarettes smoked into the same trap;P is the total number of packets of cigarettes available.NOTE The multiplier C is usually at least 1,2
