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1、INTERNATIONAL STANDARD ISO 9197 Second edition 2006-04-15 Reference number ISO 9197:2006(E) ISO 2006 Paper, board and pulps Determination of water-soluble chlorides Papier, carton et ptes Dtermination des chlorures solubles dans leau ISO 9197:2006(E) ii ISO 2006 All rights reserved PDF disclaimer Th
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5、erved. Unless otherwise 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 reque
6、ster. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland -,-,- ISO 9197:2006(E) ISO 2006 All rights reserved iii Contents Page 1Scope 1 2Normative references 1 3Terms and definitions 1 4
7、Principle 1 5Reagents . 1 6Apparatus . 2 7Sampling and preparation of sample . 2 8Procedure . 2 9Expression of results 3 10Precision . 4 11Test report 4 Annex A (informative) Laboratory manuals . 5 -,-,- ISO 9197:2006(E) iv ISO 2006 All rights reserved Foreword ISO (the International Organization fo
8、r Standardization) is a worldwide federation of national standards bodies (ISO member 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
9、 right to be represented on that committee. International organizations, governmental 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. Internati
10、onal Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication
11、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 elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights.
12、ISO 9197 was prepared by Technical Committee ISO/TC 6, Paper, board and pulps. This second edition cancels and replaces the first edition (ISO 9197:1998), of which it constitutes a minor revision. A new sentence was added at the beginning of the fifth paragraph of Clause 8, which states: “After disi
13、ntegration, soak the sample for about 1 h while stirring gently to ensure complete extraction of chloride.” There were some minor editorial changes. INTERNATIONAL STANDARDISO 9197:2006(E) ISO 2006 All rights reserved 1 Paper, board and pulps Determination of water-soluble chlorides 1Scope This Inter
14、national Standard specifies a method for the determination of water-soluble chlorides in all types of paper, board and pulp. The lower limit of the determination is of chloride ion per kilogram of dry sample. 2Normative references The following referenced documents are indispensable for the applicat
15、ion of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 186, Paper and board Sampling to determine average quality ISO 287, Paper and board Determination of moisture cont
16、ent Oven-drying method ISO 638, Pulps Determination of dry matter content ISO 7213:1981, Pulps Sampling for testing 3Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 water-soluble chlorides paper, board and pulp amount of chloride ion that is ex
17、tracted with cold water and determined under the conditions specified 4Principle Pieces of the sample under test are extracted with water at room temperature in a disintegrator. The resulting suspension is filtered and an aliquot is used for determination of the chloride ion content by ion chromatog
18、raphy. 5Reagents During the analysis, use only reagents of recognized analytical quality and only water as specified in 5.1. 5.1Distilled or demineralized water, conductivity less than . 5.2Chloride stock solution, . Dry a portion of potassium chloride, (KCI), at . Transfer thereof to a volumetric f
19、lask, dissolve the KCI and dilute to the mark with water (5.1). Commercially available standard solutions may be used. 20 mg 0,2 mS/m c(Cl)=1 000 mg/l 140 C 210,2 mg100 ml -,-,- ISO 9197:2006(E) 2 ISO 2006 All rights reserved 5.3Chloride matching solution. Dilute the chloride stock solution (5.2) to
20、 a mass fraction of chloride ion of, for example, . Do not use chloride matching solutions that are more than 1 week old. 5.4Nitric acid, . Add with caution of concentrated nitric acid, (about HNO3), to of water (5.1) and dilute to 1 litre. 5.5Additional solutions, as specified in the instructions f
21、or the ion chromatograph. 6Apparatus Glassware and other apparatus used for this analysis shall be scrupulously clean. Soak all glassware for to in the nitric acid (5.4) and then rinse thoroughly with water (5.1). Clean, in water, forceps, scissors and the disintegrator used for sample preparation.
22、6.1Wet disintegrator, a high-speed mixer, capable of disintegrating the sample completely with minimum damage to the fibres. 6.2Ion chromatograph, having a pump, an injector loop of known volume, a column system suitable for the determination of chlorides and a conductivity detector. 6.3Syringe, Cla
23、ss A, of capacity and having a prefilter of about pore width. 6.4Tea-strainer or similar device, of stainless steel, for removing fibres from a suspension. 7Sampling and preparation of sample If the test is being made to evaluate a pulp lot, the sample shall be selected in accordance with ISO 7213.
24、If the test is made on another type of sample, report the source of the sample and, if possible, the sampling procedure used. From the sample received, select specimens so that they are representative of the whole sample. The procedure to be followed when sampling depends on the particular circumsta
25、nces in each case. For sampling from lots of pulp, paper or board, the instructions in ISO 7213 or ISO 186, as relevant, are recommended. Since the amount of chlorides in the sample can be very low, take care not to contaminate it during sampling. Wear clean protective gloves at all times when handl
26、ing the sample and the test pieces prepared from it. The laboratory where the analysis is made shall be free from dust and fumes from chlorine-containing substances, such as hydrochloric acid or chlorinated solvents. Particular care should be taken in mill-site laboratories if the mill uses chlorine
27、 or chlorine dioxide as a bleaching agent. Keep specimens protected, wrapped in aluminium foil or in plastic bags, until required for analysis. Analyse specimens as soon as possible after sampling. Determine the dry matter content on a separate specimen using the procedure specified in ISO 287 (for
28、paper and board) or in ISO 638 (for pulps). 8Procedure Carry out the procedure in duplicate. A blank test shall also be carried out in parallel with the entire determination. c(Cl)=10 mg/l c(HNO3) =1,3 mol/l 90 mlc(HNO3) =14 mol/l65 %500 ml 5 min 10 min 5 ml0,2m -,-,- ISO 9197:2006(E) ISO 2006 All r
29、ights reserved 3 Weigh, to the nearest , a test piece, generally of between and . Split thick board and pulp sheets into thinner pieces to facilitate soaking. Select the size of the test piece so that the mass fraction of chloride ion of the extract is within the optimum range of the ion chromatogra
30、ph. Transfer the weighed test piece to the disintegrator (6.1) and add of water (5.1) at . Disintegrate the test piece until it is completely disintegrated, but no longer. After disintegration, soak the test piece for about while stirring gently to ensure complete extraction of chloride. Immediately
31、 after stopping the gentle stirring, withdraw a portion of the suspension, using the syringe (6.3). If this operation is hampered by the presence of fibres or fibre bundles, use the tea-strainer or similar device (6.4) to remove fibrous material. It is essential that the test-piece solution be free
32、from suspended material. Since the operation of the ion chromatograph (6.2) depends on its design, no detailed instructions may be given here. Operate the apparatus as instructed by the manufacturer. See also Annex A. For calibration, prepare from the chloride matching solution (5.3) a series of fiv
33、e calibration solutions, covering about one decade of concentrations, for example, from to . Run the calibration solutions and the test-piece solution on the chromatograph as instructed by the manufacturer of the apparatus. Plot the readings for the calibration solutions against their chloride ion c
34、oncentrations. The five points for the calibration solutions should fall on a straight line. If they fail to do so, repeat the calibration with another set of calibration solutions, covering a higher or lower concentration range, as relevant. Check the calibration several times daily and whenever a
35、new set of calibration solutions are used. 9Expression of results Read the chloride ion concentration of the sample solution from the calibration graph. Calculate the mass fraction of chloride ion in the sample from the expression where is the mass fraction of chloride ion, in milligrams per kilogra
36、m, in the sample; is the chloride ion concentration, in milligrams per litre, of the filtered sample solution; is the chloride ion concentration, in milligrams per litre, of the blank solution; is the volume of water (5.1) used: the volume specified is ; is the mass, in grams, of sample taken; is th
37、e mass fraction of dry matter, expressed as a percentage, in the sample. Calculate the mean of the duplicates and report results below as “less than ”, and results of or more to the nearest . 0,01 g2 g5 g 250 ml2 ml23 C 2 C 1 h 1 mg/l10 mg/l wCl= 100V (Cl Cl,0) mX wCl Cl Cl,0 V250 ml m X 20 mg/kg20
38、mg/kg 20 mg/kg10 mg/kg ISO 9197:2006(E) 4 ISO 2006 All rights reserved 10Precision The following results were obtained in an interlaboratory trial conducted by the Scandinavian Pulp, Paper and Board Testing Committee. Nine laboratories analysed four samples as specified in this International Standar
39、d. Each sample was analysed in duplicate. The mean mass fraction of chloride ion and the standard deviation (between laboratories) were calculated. The results are given in Table 1. 11Test report The report shall include the following information: a)reference to this International Standard; b)date a
40、nd place of testing; c)complete identification of the sample tested; d)the result, expressed as indicated in Clause 9; e)any departure from the procedure described in this International Standard or any other circumstances which can have affected the result. Table 1 Sample Mean mass fraction of chlor
41、ide ion Standard deviation mg/kgmg/kg Machine-glazed (MG) paper from bleached kraft pulp(14,6a)(3,6) Bleached kraft pulp from birch27,16,6 Copy paper 129725 Copy paper 21 24076 a The value is under the lower limit of determination. -,-,- ISO 9197:2006(E) ISO 2006 All rights reserved 5 Annex A (infor
42、mative) Laboratory manuals The procedure specified in this International Standard relies upon instruments of considerable complexity. Several manufacturers have introduced such instruments to the world market. They are all based on the same principle, but differ in details. It is a principle of stan
43、dardization not to specify the use of equipment produced by a particular manufacturer. The reason for this is not only that a standardization body should be neutral with respect to the competition between companies, but also to avoid specifications that will unnecessarily prevent further development
44、 of equipment. In practice, this means that the course of the analysis cannot be described in this International Standard in such detail that it can be used as a laboratory bench manual. For the performance of the analysis, a number of informational details have to be taken from the manufacturers manual or to be established locally in preliminary tests. Examples are settings of liquid flow, temperatures, power, waiting times. -,-,- ISO 9197:2006(E) ICS 85.040; 85.060 Price based on 5 pages ISO 2006 All rights reserved