1、December 2016 English price group 9No 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).ICS 65.160!%s“2590280www.din.deDIN I
2、SO 10315Cigarettes Determination of nicotine in smoke condensates Gaschromatographic method (ISO 10315:2013, corrected version 20141101),English translation of DIN ISO 10315:2016-12Zigaretten Nikotinbestimmung in Rauchkondensaten Gaschromatographisches Verfahren (ISO 10315:2013, korrigierte Fassung
3、20141101),Englische bersetzung von DIN ISO 10315:2016-12Cigarettes Dosage de la nicotine dans les condensats de fume Mthode par chromatographie en phase gazeuse (ISO 10315:2013, version corrige 20141101),Traduction anglaise de DIN ISO 10315:2016-12SupersedesDIN ISO 10315:200012www.beuth.deDocument c
4、omprises 12 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.11.16 A comma is used as the decimal marker. Contents PageNational foreword 3Introduction .51 Scope 62 Normative references . 63 Principle . 64 Reagents . 65 Apparatus
5、 76 Procedure 76.1 Test portion . 76.2 Setting up the apparatus86.3 Calibration of the gas chromatograph .86.4 Determination 87 Expression of results . 88 Repeatability and reproducibility . 89 Alternative gas-chromatographic procedures and analysis precautions . 99.1 General 99.2 Alternative column
6、s . 99.3 Injection systems 109.4 Alternative internal standards 1010 Test report . 10Annex A (informative) Use of this method with the gas-chromatographic determination of water 11Bibliography 12DIN ISO 10315:2016-12 2National Annex NA (informative) Bibliography. 4National foreword This document (IS
7、O 10315:2013) has been prepared by Technical Committee ISO/TC 126 “Tobacco and tobacco products” (Secretariat: DIN, Germany). The responsible German body involved in its preparation was DIN-Normenausschuss Lebensmittel und landwirtschaftliche Produkte (DIN Standards Committee Food and Agricultural P
8、roducts), Working Committee NA 057-04-01 AA Tabak und Tabakerzeugnisse. Consultation on the gas-chromatographic method of determining nicotine in smoke condensates was adopted in 1986 as part of the work programme of the Technical Committee ISO/TC 126 “Tobacco and tobacco products” (Secretariat: DIN
9、, Germany). After the revision of the second edition, the third edition of ISO 10315 was published in 2013. This edition was corrected in 2014 and published as a consolidated version. The consolidated version continues to have 2013 as the year of publication. Working Committee NA 057-04-01 AA Tabak
10、und Tabakerzeugnisse of the DIN-Normenausschuss Lebensmittel und landwirtschaftliche Produkte (DIN Standards Committee Food and Agricultural Products) decided to adapt DIN ISO 10315:2000 to the third edition of ISO 10315, published in 2013, taking into account the corrected version published in 2014
11、. The Working Committee made its decision in particular from the point of view of a necessary harmonization of the international and national standards in the field of smoke analysis. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights
12、. 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 4387 DIN ISO 4387 ISO 8243 DIN ISO 8243 ISO 10362-1 DIN ISO 1
13、0362-1 ISO 13276 DIN ISO 13276 Amendments This standard differs from DIN ISO 10315:2000-12 as follows: a) a statement has been added to the Introduction that no machine smoking regime can represent all human smoking behaviour. The technical substance of the standard has not been changed. b) a warnin
14、g notice has been added; c) in the first paragraph, the last sentence has been included as NOTE 1; d) in Clause 4, CAS numbers have been given; e) 4.6 has been revised with regard to the purity of the nicotine or nicotine salicylate; f) in 9.2.2 and Annex A, NOTES have been added; g) the standard ha
15、s been brought in line with the current rules of presentation. Previous editions DIN ISO 10315: 1992-07, 2000-12 DIN ISO 10315:2016-12 3 National Annex NA (informative) Bibliography DIN ISO 3308, Routine analytical cigarette-smoking machine Definitions and standard conditions DIN ISO 3402, Tobacco a
16、nd tobacco products Atmosphere for conditioning and testing DIN ISO 4387, Cigarettes Determination of total and nicotine-free dry particulate matter using a routine analytical smoking machine DIN ISO 8243, Cigarettes Sampling DIN ISO 10362-1, Cigarettes Determination of water in smoke condensates Pa
17、rt 1: Gas-chromatographic method DIN ISO 13276, Tobacco and tobacco products Determination of nicotine purity Gravimetric method using tungstosilicic acid DIN ISO 10315:2016-12 4 IntroductionThis International Standard may be considered as part of a set produced by ISO/TC 126 which describes the det
18、ermination of total and nicotine-free dry particulate matter (NFDPM) in cigarette smoke condensates. The set comprises:ISO 3308, ISO 3402, ISO 4387, ISO 8243, ISO 10315, and ISO 10362-1.A related International Standard, ISO 3400, determines total alkaloids, whereas this International Standard determ
19、ines only nicotine by virtue of the gas-chromatographic separation. Occasionally, differences can occur because of minor amounts of alkaloids other than nicotine in some types of tobacco.Annex A provides information about the use of this method in conjunction with or simultaneously with the gas-chro
20、matographic method of water determination specified in ISO 10362-1.A bibliography is provided.No machine smoking regime can represent all human smoking behaviour: it is recommended that cigarettes also be tested under conditions of a different intensity of machine smoking than those specified in thi
21、s International Standard; machine smoking testing is useful to characterize cigarette emissions for design and regulatory purposes, but communication of machine measurements to smokers can result in misunderstandings about differences in exposure and risk across brands; smoke emission data from mach
22、ine 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 between products in machine measurements as differences in exposure or risk is a misuse of testing using ISO stan
23、dards.Cigarettes Determination of nicotine in smoke condensates Gas-chromatographic methodDIN ISO 10315:2016-12 5 WARNING The use of this International Standard can involve hazardous materials, operations, and equipment. This International Standard does not purport to address all the safety problems
24、 associated with its use. It is the responsibility of the user of this International Standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.1 ScopeThis International Standard specifies a method for the gas-chromatographic
25、determination of nicotine in cigarette smoke condensates. The smoking of cigarettes and the collection of mainstream smoke are normally carried out in accordance with ISO 4387.NOTE 1 The method specified in this International Standard is also applicable to the determination of nicotine in cigarette
26、smoke condensates obtained by non-standard smoking.NOTE 2 In countries not in a position to use the gas-chromatographic method, reference should be made to ISO 3400 for the determination of total nicotine alkaloids. In such cases, values obtained using the method described in ISO 3400 may be used wi
27、th the addition of a note in the expression of results.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest e
28、dition of the referenced document (including any amendments) applies.ISO 4387, Cigarettes Determination of total and nicotine-free dry particulate matter using a routine analytical smoking machine3 PrincipleThe smoke condensate from the mainstream smoke is dissolved in a solvent containing an intern
29、al standard. The nicotine content of an aliquot of the solution is determined by gas chromatography, and the nicotine content of the whole of the smoke condensate is calculated.4 ReagentsUse only reagents of recognized analytical reagent grade.4.1 Carrier gas: helium (CAS: 7440-59-7) or nitrogen (CA
30、S: 7727-37-9) of high purity (at least 99,999 %).4.2 Auxiliary gases: hydrogen (CAS: 1333-74-0) of high purity (at least 99,999 %) and air for the flame ionization detector.4.3 Propan-2-ol (CAS: 67-63-0), with maximum water content of 1,0 mg/ml.DIN ISO 10315:2016-12 6 4.4 Internal standard: n-heptad
31、ecane (CAS: 629-78-7) or quinaldine (CAS: 91-63-4) of purity not less than 99 %.Carvone (CAS: 99-49-0), n-octadecane (CAS: 593-45-3), or other appropriate internal standards may be used after assessment of their purity and determination that the internal standard does not co-elute with other compone
32、nts in the smoke extract. The peak area of the internal standard on samples should be monitored for consistency. In cases where inconsistencies are found, analysis of an extraction of a smoke sample without the internal standard in the extraction solution should be performed to confirm the absence o
33、f a peak in the smoke extract eluting at the same time as the internal standard (see Clause 9).4.5 Extraction solvent: propan-2-ol (4.3) containing an appropriate concentration of internal standard (4.4); this is normally in the range of 0,2 mg/ml to 0,5 mg/ml.Solvent not stored in a temperature-con
34、trolled laboratory shall be allowed to equilibrate to (22 2) C before use.4.6 Reference substance: nicotine (CAS: 54-11-5) of known purity not less than 98 %.Store this at between 0 C and 4 C and exclude light.Nicotine salicylate (CAS: 29790-52-1) of known purity not less than 98 % may also be used.
35、NOTE The purity of the nicotine or nicotine salicylate may be verified in accordance with ISO 13276 or by any other validated method.4.7 Calibration solutionsDissolve the nicotine (4.6) in the solvent (4.5) to produce a series of at least four calibration solutions with concentrations that cover the
36、 range expected to be found in the test portion (usually 0,02 mg/ml to 2,0 mg/ml). Store these solutions at between 0 C and 4 C and exclude light.Solvent and solutions stored at low temperatures shall be allowed to equilibrate to (22 2) C before use.5 ApparatusUsual laboratory apparatus and, in part
37、icular, the following items.5.1 Gas-chromatograph, equipped with a flame ionization detector, recorder, and integrator or other suitable data handling instrument (see Clause 9).5.2 Column, of internal diameter between 2 mm and 4 mm and preferably of length 1,5 m to 2 m.The column is preferably made
38、of glass, but other materials such as deactivated stainless steel or nickel may be used. Stationary phase: 10 % poly(ethylene glycol) (PEG) 20 000 plus 2 % potassium hydroxide on an acid-washed silanized support material, 150 m (100 mesh) to 190 m (80 mesh) (see also Clause 9).6 Procedure6.1 Test po
39、rtionPrepare the test portion by dissolving the smoke condensate obtained by the machine smoking of a known number of cigarettes in a fixed volume of the solvent (4.5) of 20 ml for 44 mm discs, or 50 ml for 92 mm discs, ensuring that the disc is fully covered. The volume may be adjusted to give a co
40、ncentration of nicotine appropriate for the calibration graph (see 6.3) provided that there is adequate volume for effective extraction of the smoke condensate. Analysis should be performed as soon as possible, but if storage is inevitable then store the sample at between 0 C and 4 C and exclude lig
41、ht. For standard smoking, refer to ISO 4387.DIN ISO 10315:2016-12 7 6.2 Setting up the apparatusSet up the apparatus and operate the gas chromatograph (5.1) in accordance with the manufacturers instructions. Ensure that the peaks for solvent, internal standard, nicotine, and other smoke component pe
42、aks, especially neophytadiene (which can appear on the tail of the nicotine peak under certain circumstances), are well resolved (see also Clause 9).Suitable operating conditions are as follows: column temperature, 170 C (isothermal); injection temperature, 250 C; detector temperature, 250 C; carrie
43、r gas, helium, or nitrogen at a flow rate of about 30 ml/min; injection volume, 2 l.Using the above conditions, the analysis time is about 6 min to 8 min (see also Clause 9).6.3 Calibration of the gas chromatographInject an aliquot (2 l) of each of the calibration solutions (4.7) into the gas chroma
44、tograph. Record the peak areas (or heights) of the nicotine and internal standard (4.4). Carry out the determination at least twice.Calculate the ratio of the nicotine peak to the internal standard peak from the peak area (or height) data for each of the calibration solutions. Plot the graph of the
45、nicotine concentrations in accordance with the area ratios, and calculate a linear regression equation (concentration of nicotine according to the area ratios) from these data. The graph should be linear and the regression line should pass through the origin. Use the slope of the regression equation
46、.Perform this full calibration procedure daily. In addition, inject an aliquot of an intermediate concentration standard after every 20 sample determinations. If the calculated concentration for this solution differs by more than 3 % from the original value, repeat the full calibration procedure.6.4
47、 DeterminationInject aliquots (2 l) of the test portion (see 6.1) into the gas chromatograph. Calculate the ratio of the nicotine peak/internal standard peak from the peak area (or height) data.Carry out two determinations on the same test portion (see 6.1).Calculate the mean value of the ratio from
48、 the two determinations.Where results are obtained from a number of separate channels of smoking and where an auto-sampler is used, a single aliquot portion from the smoke traps is considered adequate.7 Expression of resultsCalculate the concentration of nicotine in the test portion using the graph or linear regression equation prepared in 6.3. Fro
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