1、-XO7UDQVODWLRQE,16SUDFKHQGLHQVW(QJOLVKSULFHJURXS1RSDUWRIWKLVWUDQVODWLRQPDEHUHSURGXFHGZLWKRXWSULRUSHUPLVVLRQRI,1HXWVFKHV,QVWLWXWIU1RUPXQJH9%HUOLQ%HXWK9HUODJ*PE+%HUOLQ*HUPDQKDVWKHHFOXVLYHULJKWRIVDOHIRU*HUPDQ6WDQGDUGV ,11RUPHQ , machine smoking testing is useful to characterize cigarette emissions for
2、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 machine measurements may be used as inputs for product hazard assessment, but they are not intended to b
3、e 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 standards. Cigarettes Determination of water in smoke condensates Part 1: Gas-chromatographic method 1 S
4、copeThis part of ISO 10362 specifies a method for the gas-chromatographic determination of water in cigarette smokecondensates. The smoking of cigarettes and collection of mainstream smoke are normally carried out in accordancewith ISO 4387. However, the method of this part of ISO 10362 is applicabl
5、e to the determination of water in smokecondensates obtained by non-standard smoking.NOTE In countries not in a position to use the gas-chromatographic method, the determination of water in smokecondensates should be performed by a Karl Fischer method (ISO 10362-2). In such cases, values obtained fo
6、r water in smokecondensate may be used with the addition of a note made in the expression of the results.2 Normative referenceThe following normative document contains provisions which, through reference in this text, constitute provisions ofthis part of ISO 10362. For dated references, subsequent a
7、mendments to, or revisions of, this publication do notapply. However, parties to agreements based on this part of ISO 10362 are encouraged to investigate the possibilityof applying the most recent edition of the normative document indicated below. For undated references, the latestedition of the nor
8、mative document referred to applies. Members of ISO and IEC maintain registers of currently validInternational Standards.ISO 4387, Cigarettes Determination of total and nicotine-free dry particulate matter using a routine analyticalsmoking machine.3PrincipleThe smoke condensate from the mainstream s
9、moke is dissolved in a solvent containing an internal standard. Thewater content of an aliquot of the solution is determined by gas chromatography, and the water content of the whole ofthe smoke condensate is calculated.4 ReagentsUse only reagents of recognized analytical reagent grade.4.1 Carrier g
10、as: helium or nitrogen (see note in 6.2).4.2 Propan-2-ol, with maximum water content of 1,0 mg/ml.4.3 Internal standard: ethanol, or methanol (of purity at least 99 %).4.4 Extraction solvent: propan-2-ol (4.2) containing an appropriate concentration of internal standard (4.3),normally 5 ml/l.Solvent
11、 not stored in a temperature-controlled laboratory shall be allowed to equilibrate to (22 Gb1 2) Gb0C before use.DIN ISO 10362-1:2013-074.5 Reference substance: distilled water or deionized water.4.6 Calibration solutionsPrepare a series of at least four calibration solutions whose concentrations of
12、 added water cover the range expectedto be found in the test portion (usually up to 4 mg/ml) by adding weighed amounts of water (4.5) to the solvent (4.4).One of these calibration solutions shall be the solvent with no added water (solvent blank).To prevent water being absorbed, the bulk solvent con
13、tainer shall be fitted with a water trap and all solutions shall bekept sealed. The solvent shall be stirred continuously to ensure the homogeneity of the water concentration in thesolvent. The calibration solutions shall be made up using an extraction solvent from the same batch used in 6.1.It is r
14、ecommended that the calibration solutions be made up at least each week.5 ApparatusUsual laboratory apparatus and, in particular, the following items.5.1 Gas-chromatograph, equipped with a thermal conductivity detector, recorder and integrator or othersuitable data-handling equipment.Glassware and s
15、epta for vials should be stored in a desiccator until use.5.2 Column, of internal diameter between 2 mm and 4 mm and preferably of length 1,5 m to 2 m.Stationary phase: Porapak Q1)150 G6dm (100 mesh) to 190 G6dm(80mesh).The column is preferably made of deactivated stainless steel but other materials
16、 such as glass or nickel may beused. Alternative stationary phases, such as Porapak QS1)or Chromosorb 1021), may be used.5.3 Dispensing system, preferably automated, capable of delivering the required volume of solvent (4.4).The dispensing system should be flushed prior to use by dispensing a volume
17、 of solvent of at least 50 ml which willthen be rejected.6 Procedure6.1 Test portionPrepare the test portion by dissolving the smoke condensate obtained by the machine smoking of a known number ofcigarettes in a fixed volume of the solvent (4.4) of 20 ml for 44 mm discs or 50 ml for 92 mm discs, ens
18、uring that thedisc is fully covered. The volume may be adjusted to give a concentration of water appropriate for the calibrationgraph (see 6.3) provided that there is an adequate volume for effective extraction of the smoke condensate. Forstandard smoking, see ISO 4387.1) Porapak Q, Porapak QS and C
19、hromosorb 102 are trade names of examples of suitable products available commercially. Thisinformation is given for the convenience of users of this part of ISO 10362 and does not constitute an endorsement by ISO of theseproducts.7DIN ISO 10362-1:2013-076.2 Setting up the apparatusSet up the apparat
20、us and operate the gas chromatograph (5.1) in accordance with the manufacturers instructions.Ensure that the peaks for water, the internal standard and solvent are well resolved, the analysis time being about4 min. Condition the system just prior to use by injecting a 2 G6dl aliquot of the extractio
21、n solvent as a primer.Suitable operating conditions are as follows:Gbe column temperature: 170 Gb0C (isothermal);Gbe injection temperature: 250 Gb0C;Gbe detector temperature: 250 Gb0C;Gbe carrier gas: helium at a flow rate of about 30 ml/min;Gbe injection volume: 2 l.NOTE Nitrogen may also be used a
22、s an alternative carrier gas if the detector sensitivity is sufficiently high.6.3 Calibration of the gas chromatographInject an aliquot (2 G6dl) of each of the calibration solutions (4.6) into the gas chromatograph. Record the peak areas (orheights) of the water and internal standard (4.3). Carry ou
23、t the determination at least twice.Calculate the ratio of the water peak to the internal standard peak from the peak area (or height) data for each of thecalibration solutions including the solvent blank. Plot the graph of the concentrations of added water in accordancewith the area ratios or calcul
24、ate a linear regression equation from these data. Use the linear regression equation.Perform this full calibration procedure daily. In addition, inject an aliquot of an intermediate concentration standardafter every 20 sample determinations. If the calculated concentration for this solution differs
25、by more than 5 % fromthe original value, repeat the full calibration procedure.NOTE The regression line does not pass through zero due to water present in the extraction solvent.If the water content of the solvent exceeds 1,0 mg/ml, the batch should be rejected.6.4 Blank testDue to the absorption of
26、 water by smoke traps and solvent, it is necessary to determine a value for the sample blank.Prepare sample blanks by treating additional smoke traps including filters (at least 2 per 100 cigarettes smoked) in thesame manner as that used for smoke collection. Place them near the smoking machine duri
27、ng smoking and extractand analyse them together with the smoke samples.6.5 DeterminationInject aliquots (2 l) of the test portion from the smoke traps (see 6.1) and blank traps (see 6.4). Calculate the ratio ofthe water peak/internal standard peak from the peak area (or height) data.Carry out the de
28、termination at least twice under identical conditions. Calculate the mean value of the ratio from thereplicate determinations.NOTE Where results are obtained from a number of separate channels of smoking and where an autosampler is used, asingle aliquot portion from the smoke traps is considered ade
29、quate.DIN ISO 10362-1:2013-077 Expression of resultsCalculate the water concentration of the smoke trap and blank trap extracts using the graph or linear regressionequation prepared in 6.3.The water content of the smoke, mW, in milligrams per cigarette, is given by the equation:ESWBWSWVqm Gd7G2dG3dG
30、72G72whereG72WSis the concentration of water in the sample smoke trap, in milligrams per millilitre;G72WBis the concentration of water in the blank smoke trap, in milligrams per millilitre;q is the number of cigarettes smoked through each smoke trap;VESis the volume of extraction solvent in which th
31、e contents of the smoke trap were dissolved.Express the test results in milligrams per cigarette for each channel to the nearest 0,01 mg, and the average percigarette to the nearest 0,1 mg.8 Repeatability and reproducibilityA major international collaborative study involving 30 laboratories and 6 sa
32、mples, conducted in 1990, showed thatwhen cigarettes are smoked in accordance with ISO 4387 and the resulting smoke solutions are analysed by thismethod, the following values for the repeatability limits (r) and the reproducibility limits (R) are obtained.The difference between two single results fo
33、und on matched cigarette samples by one operator using the sameapparatus within the shortest feasible time interval will exceed the repeatability limit (r) on average not more than oncein 20 cases in the normal and correct operation of the method.Single results on matched cigarette samples reported
34、by two laboratories will differ by more than the reproducibilitylimit (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 Estimates given by data analysisMean value Repeatability limit Repro
35、ducibility limitmWrRmg per cigarette mg per cigarette mg per cigarette0,083 0,154 0,2410,153 0,228 0,3530,338 0,272 0,3810,962 0,407 0,7341,595 0,561 0,9353,187 0,908 1,6809DIN ISO 10362-1:2013-07For the purpose of calculating r and R, one test result was defined as the mean yield obtained from smok
36、ing20 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 reportThe test report shall give the water content per cigarette smoked and the method used, and s
37、hall include allconditions which may affect the result (e.g. atmospheric test conditions during smoking). It shall also give all detailsnecessary for the identification of the cigarettes smoked.DIN ISO 10362-1:2013-07Annex A(informative)Use of this method in conjunction with the method of nicotine d
38、eterminationThis method can be used in conjunction with the method for the gas-chromatographic determination of nicotine insmoke condensates specified in ISO 10315. This may be carried out as follows:Gbe addition of an appropriate quantity of the internal standard specified for the nicotine determin
39、ation in thesolvent described in 4.4;Gbe injection of an aliquot of the smoke condensate solution onto a column for nicotine analysis, which isconnected to a flame ionization detector, as well as onto the water column and detector described in thismethod.A simultaneous automated analysis of nicotine
40、 and water may be achieved by using a splitting system or an auto-sampler with two injection positions. When determining nicotine and water from the same sample sequentially, thewater determination is performed first to prevent absorption of water by the sample affecting the final result.11DIN ISO 1
41、0362-1:2013-07Bibliography1 ISO 3308, Routine analytical cigarette-smoking machine Definitions and standard conditions.2 ISO 3402, Tobacco and tobacco products Atmosphere for conditioning and testing.3 ISO 8243, Cigarettes Sampling.4 ISO 10315, Cigarettes Determination of nicotine in smoke condensates Gas-chromatographic method.5 ISO 10362-2, Cigarettes Determination of water in smoke condensates Part 2: Karl Fischer method.6 CORESTA Report 91/1, Internal Bulletin of Cooperation of the centre for scientific research relative to tobacco,1991-1, ISSN 0525-6240.DIN ISO 10362-1:2013-07
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