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1、Reference number ISO 10362-1:1999(E) ISO 1999 INTERNATIONAL STANDARD ISO 10362-1 Second edition 1999-12-15 Cigarettes Determination of water in smoke condensates Part 1: Gas-chromatographic method Cigarettes Dosage de leau dans les condensats de fume Partie 1: Mthode par chromatographie en phase gaz
2、euse Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 09:13:27 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 10362-1:1999(E) PDF disclaimer This PDF file may contai
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5、eters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below. ISO 1999 All rights reserved. Unless otherwis
6、e 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 ISO at the address below or ISOs member body in the country of the requester. ISO copyright of
7、fice Case postale 56 ? CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 734 10 79 E-mail copyrightiso.ch Web www.iso.ch Printed in Switzerland ii ISO 1999 All rights reserved Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/998075
8、5100 Not for Resale, 04/23/2007 09:13:27 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 10362-1:1999(E) ISO 1999 All rights reservediii Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member
9、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 organizations, governmental
10、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 ISO/IEC Directive
11、s, Part 3. 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 member bodies casting a vote. Attention is drawn to the possibility that some of the element
12、s of this part of ISO 10362 may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 10362-1 was prepared by Technical Committee ISO/TC 126,Tobacco and tobacco products. This second edition cancels and replaces t
13、he first edition (ISO 10362-1:1991), which has been editorially revised. ISO 10362 consists of the following parts, under the general titleCigarettes Determination of water in smoke condensates: ?Part 1: Gas-chromatographic method ?Part 2: Karl Fischer method Annex A of this part of ISO 10362 is for
14、 information only. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 09:13:27 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 10362-1:1999(E) iv ISO 1999 All rights re
15、served Introduction This part of ISO 10362 may be considered as part of a set produced by ISO/TC 126 which describes the determination of total and nicotine-free dry particulate matter (NFDPM) in cigarette smoke condensate. The set comprises: ISO 3308, ISO 3402, ISO 4387, ISO 8243, ISO 10315 and ISO
16、 10362-1. Annex A provides information about the use of this method in conjunction or simultaneously with the gas-chromato- graphic method of nicotine determination described in ISO 10315. A bibliography is provided. Copyright International Organization for Standardization Provided by IHS under lice
17、nse with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 09:13:27 MDTNo reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARDISO 10362-1:1999(E) ISO 1999 All rights reserved1 Cigarettes Determination of water in smoke condensates Part 1: Gas-chromato
18、graphic method 1Scope This part of ISO 10362 specifies a method for the gas-chromatographic determination of water 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 of this part of IS
19、O 10362 is applicable to the determination of water in smoke condensates obtained by non-standard smoking. NOTEIn countries not in a position to use the gas-chromatographic method, the determination of water in smoke condensates should be performed by a Karl Fischer method (ISO 10362-2). In such cas
20、es, values obtained for water in smoke condensate may be used with the addition of a note made in the expression of the results. 2Normative reference The following normative document contains provisions which, through reference in this text, constitute provisions of this part of ISO 10362. For dated
21、 references, subsequent amendments to, or revisions of, this publication do not apply. However, parties to agreements based on this part of ISO 10362 are encouraged to investigate the possibility of applying the most recent edition of the normative document indicated below. For undated references, t
22、he latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 4387,Cigarettes Determination of total and nicotine-free dry particulate matter using a routine analytical smoking machine. 3Principle The smoke
23、condensate from the mainstream smoke is dissolved in a solvent containing an internal standard. The water content of an aliquot of the solution is determined by gas chromatography, and the water content of the whole of the smoke condensate is calculated. 4Reagents Use only reagents of recognized ana
24、lytical reagent grade. 4.1Carrier gas: helium or nitrogen (see note in 6.2). 4.2Propan-2-ol, with maximum water content of 1,0 mg/ml. 4.3Internal standard: ethanol, or methanol (of purity at least 99 %). 4.4Extraction solvent: propan-2-ol (4.2) containing an appropriate concentration of internal sta
25、ndard (4.3), normally 5 ml/l. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 09:13:27 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 10362-1:1999(E) 2 ISO 1999 All
26、 rights reserved Solvent not stored in a temperature-controlled laboratory shall be allowed to equilibrate to (22 ? 2) ?C before use. 4.5Reference substance: distilled water or deionized water. 4.6Calibration solutions Prepare a series of at least four calibration solutions whose concentrations of a
27、dded water cover the range expected to 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 co
28、ntainer shall be fitted with a water trap and all solutions shall be kept sealed. The solvent shall be stirred continuously to ensure the homogeneity of the water concentration in the solvent. The calibration solutions shall be made up using an extraction solvent from the same batch used in 6.1. It
29、is recommended that the calibration solutions be made up at least each week. 5Apparatus Usual laboratory apparatus and, in particular, the following items. 5.1Gas-chromatograph, equipped with a thermal conductivity detector, recorder and integrator or other suitable data-handling equipment. Glasswar
30、e and septa for vials should be stored in a desiccator until use. 5.2Column, of internal diameter between 2 mm and 4 mm and preferably of length 1,5 m to 2 m. Stationary phase: Porapak Q1)150 ?m (100 mesh) to 190 ?m (80 mesh). The column is preferably made of deactivated stainless steel but other ma
31、terials such as glass or nickel may be used. Alternative stationary phases, such as Porapak QS1)or Chromosorb 1021), may be used. 5.3Dispensing system, preferably automated, capable of delivering the required volume of solvent (4.4). The dispensing system should be flushed prior to use by dispensing
32、 a volume of solvent of at least 50 ml which will then be rejected. 6Procedure 6.1Test portion Prepare 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 (4.4) of 20 ml for 44 mm discs or 50 ml for 92 m
33、m discs, ensuring that the disc is fully covered. The volume may be adjusted to give a concentration of water appropriate for the calibration graph (see 6.3) provided that there is an adequate volume for effective extraction of the smoke condensate. For standard smoking, see ISO 4387. 1)Porapak Q, P
34、orapak QS and Chromosorb 102 are trade names of examples of suitable products available commercially. This information is given for the convenience of users of this part of ISO 10362 and does not constitute an endorsement by ISO of these products. Copyright International Organization for Standardiza
35、tion Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 09:13:27 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 10362-1:1999(E) ISO 1999 All rights reserved3 6.2Setting up the apparatus Set up the apparatus and operate the g
36、as 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 about 4 min. Condition the system just prior to use by injecting a 2 ?l aliquot of the extraction solvent as a prime
37、r. Suitable operating conditions are as follows: ?column temperature: 170 ?C (isothermal); ?injection temperature: 250 ?C; ?detector temperature: 250 ?C; ?carrier gas: helium at a flow rate of about 30 ml/min; ?injection volume: 2 l. NOTENitrogen may also be used as an alternative carrier gas if the
38、 detector sensitivity is sufficiently high. 6.3Calibration of the gas chromatograph Inject an aliquot (2 ?l) of each of the calibration solutions (4.6) into the gas chromatograph. Record the peak areas (or heights) of the water and internal standard (4.3). Carry out the determination at least twice.
39、 Calculate the ratio of the water peak to the internal standard peak from the peak area (or height) data for each of the calibration solutions including the solvent blank. Plot the graph of the concentrations of added water in accordance with the area ratios or calculate a linear regression equation
40、 from these data. Use the linear regression equation. 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 5 % from the orig
41、inal value, repeat the full calibration procedure. NOTEThe 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. 6.4Blank test Due to the absorption of water by smoke traps and s
42、olvent, 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 the same manner as that used for smoke collection. Place them near the smoking machine during smoking and extract an
43、d analyse them together with the smoke samples. 6.5Determination Inject aliquots (2 l) of the test portion from the smoke traps (see 6.1) and blank traps (see 6.4). Calculate the ratio of the water peak/internal standard peak from the peak area (or height) data. Carry out the determination at least
44、twice under identical conditions. Calculate the mean value of the ratio from the replicate determinations. NOTEWhere results are obtained from a number of separate channels of smoking and where an autosampler is used, a single aliquot portion from the smoke traps is considered adequate. Copyright In
45、ternational Organization for Standardization Provided by IHS under license with ISO Licensee=Aramco HQ/9980755100 Not for Resale, 04/23/2007 09:13:27 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 10362-1:1999(E) 4 ISO 1999 All rights reserved 7Expression of results Ca
46、lculate the water concentration of the smoke trap and blank trap extracts using the graph or linear regression equation prepared in 6.3. The water content of the smoke, mW, in milligrams per cigarette, is given by the equation: ES WBWS W V q m? ? ? ? where ?WSis the concentration of water in the sam
47、ple smoke trap, in milligrams per millilitre; ?WBis the concentration of water in the blank smoke trap, in milligrams per millilitre; qis the number of cigarettes smoked through each smoke trap; VESis the volume of extraction solvent in which the contents of the smoke trap were dissolved. Express th
48、e test results in milligrams per cigarette for each channel to the nearest 0,01 mg, and the average per cigarette to the nearest 0,1 mg. 8Repeatability and reproducibility A major international collaborative study involving 30 laboratories and 6 samples, conducted in 1990, showed that when cigarettes are smoked in accordance with ISO 4387 and the resulting smoke solutions are analysed by this method, the following values for the repeatability limits (r) and the reproducibility limits (R) are obtained. The difference between two singl