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1、BRITISH STANDARD BS 5202-12: 1991 ISO 10315: 1991 Incorporating Amendment No. 1 Methods for Chemical analysis of tobacco and tobacco products Part 12: Determination of nicotine in smoke condensate of cigarettes (gas-chromatographic method) Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 14:36
2、:31 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5202-12:1991 This British Standard, having been prepared under the direction of the Agriculture and Food Standards Policy Committee, was published under the authority of the Standards Board and comes into effect on 29 November 1991 BSI 09-1999 The fo
3、llowing BSI references relate to the work on this standard: Committee reference AFC/11 Draft for comment 90/53732 DC ISBN 0 580 20283 6 Committees responsible for this British Standard The preparation of this British Standard was entrusted by the Agriculture and Food Standards Policy Committee (AFC/
4、-) to Technical Committee AFC/11, upon which the following bodies were represented: Department of Trade and Industry (Laboratory of the Government Chemist) Tobacco Advisory Council Amendments issued since publication Amd. No.DateComments 7155July 1992Indicated by a sideline in the margin Licensed Co
5、py: sheffieldun sheffieldun, na, Mon Dec 04 14:36:31 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5202-12:1991 BSI 09-1999i Contents Page Committees responsibleInside front cover National forewordii Introduction1 1Scope1 2Normative references1 3Principle1 4Reagents1 5Apparatus2 6Procedure2 7Express
6、ion of results2 8Repeatability and reproducibility2 9Test report3 Annex A (informative) Use of this method in conjunction, or simultaneously with the gas-chromatographic determination of water4 Annex B (informative) Bibliography4 Table 13 Publication(s) referred toInside back cover Licensed Copy: sh
7、effieldun sheffieldun, na, Mon Dec 04 14:36:31 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5202-12:1991 ii BSI 09-1999 National foreword This Part of BS 5202 has been prepared under the direction of the Agriculture and Food Standards Policy Committee. It is identical with ISO 10315:1991 “Cigarette
8、s Determination of nicotine in smoke condensates Gas-chromatographic method”, published by the International Organization for Standardization (ISO), and in the preparation of which the United Kingdom played a full part. Additional information. In 6.1 of the international text, to remove ambiguity, t
9、he words “to obtain the concentration of nicotine adjusted to the calibration graph” should be interpreted as “to give a concentration of nicotine appropriate for the calibration graph”. In 6.4 of the international text, the injection of more than one aliquot portion of the test portion (6.1) is imp
10、lied. In the UK, where results are obtained from at least four separate channels of smoking and where an autosampler is used, a single aliquot portion from the smoke traps is considered adequate. When ISO 4387:1991 “Cigarettes Determination of total and nicotine-free dry particulate matter using a r
11、outine analytical smoking machine”, referred to in 6.1, and ISO 10362-1:1991 “Cigarettes Determination of water in smoke condensates Part 1: Gas-chromatographic method”, referred to in Annex A, are published, it is intended to publish them as dual-numbered British Standards. NOTEOther International
12、Standards are referred to in the introduction. These references are for information only. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not o
13、f itself confer immunity from legal obligations. Cross-references International Standard Corresponding British Standard ISO 3400:1989BS 5202 Methods for chemical analysis of tobacco and tobacco products Part 7:1990 Determination of alkaloids in smoke condensate of cigarettes (spectrometric method) (
14、Identical) Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, pages 1 to 4, an inside back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table o
15、n the inside front cover. Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 14:36:31 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5202-12:1991 BSI 09-19991 Introduction This International Standard may be considered as part of a set produced by ISO/TC 126 which describes the determination of to
16、tal and nicotine-free dry particulate matter (NFDPM) in cigarette smoke condensate. The set comprises ISO 3308:1991, Routine analytical cigarette-smoking machine Definitions and standard conditions1). ISO 3402:1991, Tobacco and tobacco products Atmosphere for conditioning and testing1). ISO 4387:199
17、1, Cigarettes Determination of total and nicotine-free dry particulate matter using a routine analytical smoking machine1). ISO 8243:1991, Cigarettes Sampling1). ISO 10315:1991, Cigarettes Determination of nicotine in smoke condensates Gas-chromatographic method. ISO 10362-1:1991, Cigarettes Determi
18、nation of water in smoke condensates Part 1: Gas-chromatographic method. Annex A provides information about the use of this method in conjunction with or simultaneously with the gas-chromatographic method of water determination, ISO 10362-1. Annex B refers to ISO 3400, which determines total alkaloi
19、ds, whereas ISO 10315 determines 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. 1 Scope This International Standard specifies a method for the gas-chromatographic d
20、etermination of nicotine in cigarette smoke condensates. The smoking of cigarettes and collection of mainstream smoke are normally carried out in accordance with ISO 4387. However, the method is also applicable to the determination of nicotine in cigarette smoke condensates obtained by non-standard
21、smoking. NOTE 1In the countries that are 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 with an additional note in the e
22、xpression of results. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to ag
23、reements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 4387:1991, Cigarettes Determination of total an
24、d nicotine-free dry particulate matter using a routine analytical smoking machine1). ISO 8243:1991, Cigarettes Sampling1). 3 Principle Dissolution of the smoke condensate from the mainstream smoke in a solvent. Determination of the nicotine content of an aliquot of the solution by gas chromatography
25、 and calculation of the nicotine content of the whole of the smoke condensate. 4 Reagents All reagents shall be of recognized analytical reagent grade. 4.1 Carrier gas Helium or nitrogen. 4.2 Auxillary gases Air and hydrogen of high purity for the flame ionization detector. 4.3 Propan-2-ol Maximum w
26、ater content: 1,0 mg per cm3. 4.4 Internal standard n-Heptadecane or quinaldine (of purity at least 99 %). 4.5 Extraction solvent Propan-2-ol (4.3) containing 0,5 g per litre of internal standard (4.4). 4.6 Reference substance Nicotine (of purity at least 98 %). Store at 0 C to + 4 C and exclude lig
27、ht. 4.7 Calibration solutions Dissolve the nicotine (4.6) in the solvent (4.5) to produce a series of at least four calibration solutions whose concentrations cover the range expected to be found in the test portion (usually 0,02 mg per cm3 to 2,0 mg per cm3). Store these solutions at 0 C to + 4 C a
28、nd exclude light. 1) To be published. Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 14:36:31 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5202-12:1991 2 BSI 09-1999 5 Apparatus Usual laboratory apparatus and the following items: 5.1 Gas-chromatograph, equipped with flame ionization detecto
29、r and recorder or integrator. 5.2 Column, of internal diameter between 2 mm and 4 mm and preferably of length 1,5 m to 2 m. Stationary phase: 10 % PEG 20 000 plus 2 % potassium hydroxide on an acid washed silanized support material, 80 mesh to 100 mesh. NOTE 2The column is preferably made of glass b
30、ut other materials such as deactivated stainless steel or nickel may be used. Alternative stationary phases, such as 2 % Versamid 9002) plus 1 % potassium hydroxide or lower loadings of PEG 20 000 with or without potassium hydroxide, may be used. If alternative stationary phases are used it is neces
31、sary to ensure that the peak due to nicotine is well resolved from peaks due to other smoke components, the internal standard and the solvent. NOTE 3Other columns have been proposed and are being studied by CORESTA. 6 Procedure 6.1 Test portion Prepare the test portion by dissolving the smoke conden
32、sate obtained by the machine smoking of a known number of cigarettes in 20 cm3 for 44 mm disc or 50 cm3 for 92 mm disc of the solvent (4.5) to obtain the concentration of nicotine adjusted to the calibration graph (6.3). Analysis should be performed as soon as possible but if storage is inevitable t
33、hen store the sample at 0 C to 4 C and exclude light. For standard smoking refer to ISO 4387. 6.2 Setting up the apparatus Set up the apparatus and operate the gas chromatograph, recorder or integrator and autosampler (if one is used) in accordance with the manufacturers instructions. Ensure that th
34、e peaks for solvent, internal standard, nicotine and other smoke component peaks, especially neophytadiene, are well resolved. Suitable operating conditions are Column temperature: 170 C (isothermal) Injection temperature: 250 C Detector temperature: 250 C Carrier gas: Helium or nitrogen at a flow r
35、ate of about 30 cm3per min Injection volume: 24l Using the above conditions the analysis time is about 6 min to 8 min. 6.3 Calibration of the gas chromatograph Inject an aliquot (2 4l) of each of the calibration solutions (4.7) into the gas chromatograph. Record the peak areas (or heights) of the ni
36、cotine and internal standard. 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 nicotine concentrations according to the area ratios or ca
37、lculate 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. Perform this full calibration procedure daily. In addition, inje
38、ct 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 Determination Inject aliquots (2 4l) of the test portion (6.1)
39、into the gas chromatograph. Calculate the ratio of the nicotine peak to the internal standard peak from the peak area (or height) data. Carry out two determinations on the same test portion (6.1). Calculate the mean value of the ratio from the two determinations. 7 Expression of results Calculate th
40、e concentration of nicotine in the test portion using the graph or linear regression equation prepared in 6.3. From the concentration of nicotine in the test portion calculate the amount of nicotine in the smoke condensate. Deduce the amount in the cigarettes smoked. Express the test results in mill
41、igrams per cigarette for each channel to the nearest 0,01 mg and the average per cigarette to the nearest 0,1 mg. 8 Repeatability and reproducibility A major international collaborative study, involving 30 laboratories and 6 samples conducted in 1990 showed that when cigarettes are smoked in accorda
42、nce with ISO 4387, and the resulting smoke solutions are analysed by this method the following values for repeatability (r) and reproducibility (R) are obtained. 2) Trade name. Versamid 900 is an example of a suitable product available commercially. This information is given for the convenience of u
43、sers of this International Standard and does not constitute an endorsement by ISO of this product. Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 14:36:31 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5202-12:1991 BSI 09-19993 The difference between two single results found on matched cigare
44、tte samples by one operator using the same apparatus within the shortest feasible time interval will exceed the repeatability value (r) on average not more than once in 20 cases in the normal and correct operation of the method. Single results on matched cigarette samples reported by two laboratorie
45、s will differ by more than the reproducibility value (R) on average not more than once in 20 cases in the normal and correct operation of the method. Data analysis gave the estimates as summarized in Table 1. Table 1 For the purpose of calculating r and R, one test result was defined as the mean yie
46、ld obtained from smoking 20 cigarettes in a single run. For further details of the interaction of r and R with other factors, see CORESTA Report 91/1. The subject of tolerances due to sampling is dealt with in ISO 8243. 9 Test report The test report shall give the yield of nicotine per cigarette smo
47、ked and the method used, and include all conditions which may affect the result (e.g. atmospheric pressure during smoking). It shall also give all details necessary for the identification of the cigarettes smoked. Mean yield of nicotine mg Repeatability conditions r Reproducibility conditions R 0,09
48、1 0,179 0,326 0,673 0,835 1,412 0,040 0,046 0,050 0,077 0,079 0,107 0,069 0,069 0,076 0,109 0,142 0,195 Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 14:36:31 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5202-12:1991 4 BSI 09-1999 Annex A (informative) Use of this method in conjunction, or
49、 simultaneously with the gas-chromatographic determination of water This method can be used in conjunction with the gas-chromatographic method of water determination in smoke condensates, specified in ISO 10362-1. This may be done by a) the addition of an appropriate quantity of the internal standard prescribed for the water determination in the solvent described in 4.5; b) the use, preferably of helium, as the carrier gas; c) an injection of an aliquot of the smoke condensate solution on to a column for water analysis, which is