1、BS ISO 9197:2016 Paper, board and pulps Determination of water-soluble chlorides BSI Standards Publication WB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06BS ISO 9197:2016 BRITISH STANDARD National foreword This British Standard is the UK implementation of ISO 9197:2016. It supersedes BS ISO
2、 9197:2006 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee PAI/11, Methods of test for paper, board and pulps. A list of organizations represented on this committee can be obtained on request to its secretary. This publication does not purport to incl
3、ude all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2016. Published by BSI Standards Limited 2016 ISBN 978 0 580 90639 8 ICS 85.040; 85.060 Compliance with a British Standard cannot confer immunity from legal obligation
4、s. This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 August 2016. Amendments/corrigenda issued since publication Date T e x t a f f e c t e dBS ISO 9197:2016 ISO 2016 Paper, board and pulps Determination of water-soluble chlorides Papier, ca
5、rton et ptes Dtermination des chlorures solubles dans leau INTERNATIONAL STANDARD ISO 9197 Third edition 2016-08-15 Reference number ISO 9197:2016(E)BS ISO 9197:2016ISO 9197:2016(E)ii ISO 2016 All rights reserved COPYRIGHT PROTECTED DOCUMENT ISO 2016, Published in Switzerland All rights reserved. Un
6、less otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the
7、 address below or ISOs member body in the country of the requester. ISO copyright office Ch. de Blandonnet 8 CP 401 CH-1214 Vernier, Geneva, Switzerland Tel. +41 22 749 01 11 Fax +41 22 749 09 47 copyrightiso.org www.iso.orgBS ISO 9197:2016ISO 9197:2016(E)Foreword iv 1 Scope . 1 2 Normative referenc
8、es 1 3 T erms and definitions . 1 4 Principle 1 5 Reagents 1 6 Apparatus . 2 7 Sampling and preparation of sample 2 8 Procedure. 2 9 Expression of results 3 10 Test report . 3 Annex A (informative) Precision . 5 Annex B (informative) Laboratory manuals . 6 Bibliography 7 ISO 2016 All rights reserved
9、 iii Contents PageBS ISO 9197:2016ISO 9197:2016(E) Foreword ISO (the International Organization for 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. Eac
10、h 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 and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the Internation
11、al Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different
12、 types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives). Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall no
13、t be held responsible for identifying any or all such patent rights. Details of any patent rights identified during the development of the document will be in the Introduction and/or on the ISO list of patent declarations received (see www.iso.org/patents). Any trade name used in this document is in
14、formation given for the convenience of users and does not constitute an endorsement. For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) se
15、e the following URL: Foreword - Supplementary information The committee responsible for this document is ISO/TC 6, Paper, board and pulps. This third edition cancels and replaces the second edition (ISO 9197:2006), of which it constitutes a minor revision. The changes compared to the previous editio
16、n are as follows: the text in 5.4 on the preparation of nitric acid has been corrected; the precision statement has been moved to Annex A.iv ISO 2016 All rights reservedBS ISO 9197:2016INTERNATIONAL ST ANDARD ISO 9197:2016(E) Paper, board and pulps Determination of water-soluble chlorides 1 Scope Th
17、is International 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 20 mg of chloride ion per kilogram of dry sample. 2 Normative references The following documents, in whole or in part, are norm
18、atively referenced in this document and are indispensable for its application. 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 qualit
19、y ISO 287, Paper and board Determination of moisture content of a lot Oven-drying method ISO 638, Paper, board and pulps Determination of dry matter content Oven-drying method ISO 7213, Pulps Sampling for testing 3 T erms a nd definiti ons For the purposes of this document, the following terms and d
20、efinitions apply. 3.1 water soluble chlorides amount of chloride ion that is extracted with cold water and determined under the conditions specified 4 Principle Pieces of the sample under test are extracted with water at room temperature in a disintegrator. The resulting suspension is filtered and a
21、n aliquot is used for determination of the chloride ion content by ion chromatography. 5 Reagents During the analysis, use only reagents of recognized analytical quality and only water as specified in 5.1. 5.1 Distilled or demineralized water, conductivity less than 0,2 mS/m. 5.2 Chloride stock solu
22、tion, c(Cl) = 1 000 mg/l. Dry a portion of potassium chloride, (KCI), at 140 C. Transfer 210,2 mg thereof to a 100 ml volumetric flask, dissolve the KCI and dilute to the mark with water (5.1). Commercially available standard solutions may be used. 5.3 Chloride matching solution. Dilute the chloride
23、 stock solution (5.2) to a mass fraction of chloride ion of, for example, c(Cl) = 10 mg/l. Do not use chloride matching solutions that are more than one week old. ISO 2016 All rights reserved 1BS ISO 9197:2016ISO 9197:2016(E) 5.4 Nitric acid, c(HNO 3 ) = 1,3 mol/l. Add with caution 82 ml of concentr
24、ated nitric acid, c(HNO 3 ) = 15,8 mol/l (about 70 % HNO 3 ), to 500 ml of water (5.1) and dilute to 1 l. 5.5 Additional solutions, as specified in the instructions for the ion chromatograph. 6 Apparatus Glassware and other apparatus used for this analysis shall be scrupulously clean. Soak all glass
25、ware for 5 min to 10 min 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. 6.1 Wet disintegrator, a high-speed mixer, capable of disintegrating the sample completely with minimum damage to the fi
26、bres. 6.2 Ion chromatograph, having a pump, an injector loop of known volume, a column system suitable for the determination of chlorides and a conductivity detector. 6.3 Syringe, Class A, of capacity 5 ml and having a prefilter of about 0,2 m pore width. 6.4 Tea-strainer or similar device, of stain
27、less steel, for removing fibres from a suspension. 7 Sampling 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. If the test is made on another type of sample, report the source of the sample and, if possible, the sam
28、pling 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 circumstances in each case. For sampling from lots of pulp, paper or board, the instructions in ISO 7213 or ISO 1
29、86, 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 handling the sample and the test pieces prepared from it. The laboratory where the analysis is made shall be
30、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 or chlorine dioxide as a bleaching agent. Keep specimens protected, wrapped in aluminium foil or in pl
31、astic 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 paper and board) or in ISO 638 (for pulps). 8 Procedure Carry out the procedure in duplicate. A blank t
32、est shall also be carried out in parallel with the entire determination. Weigh, to the nearest 0,01 g, a test piece, generally of between 2 g and 5 g. 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
33、ion of the extract is within the optimum range of the ion chromatograph.2 ISO 2016 All rights reservedBS ISO 9197:2016ISO 9197:2016(E) Transfer the weighed test piece to the disintegrator (6.1) and add 250 ml 2 ml of water (5.1) at 23 C 2 C. Disintegrate the test piece until it is completely disinte
34、grated, but no longer. After disintegration, soak the test piece for about 1 h while stirring gently to ensure complete extraction of chloride. Immediately after stopping the gentle stirring, withdraw a portion of the suspension, using the syringe (6.3). If this operation is hampered by the presence
35、 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 from suspended material. Since the operation of the ion chromatograph (6.2) depends on its design, no detailed instructions may be given here. Op
36、erate the apparatus as instructed by the manufacturer (see also Annex A). For calibration, prepare from the chloride matching solution (5.3) a series of five calibration solutions, covering about one decade of concentrations, for example, from 1 mg/l to 10 mg/l. Run the calibration solutions and the
37、 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 concentrations. The five points for the calibration solutions should fall on a straight line. If they fail to do so, repeat the cal
38、ibration with another set of calibration solutions, covering a higher or lower concentration range, as relevant. Check the calibration several times daily and whenever a new set of calibration solutions is used. 9 Expression of results Read the chloride ion concentration of the sample solution from
39、the calibration graph. Calculate the mass fraction of chloride ion in the sample from Formula (1): ,(1) wherew Cl is the mass fraction of chloride ion, in milligrams per kilogram, in the sample; Cl is the chloride ion concentration, in milligrams per litre, of the filtered sample solution; Cl,0 is t
40、he chloride ion concentration, in milligrams per litre, of the blank solution;V is the volume of water (5.1) used: the volume specified is 250 ml;m is the mass, in grams, of sample taken;X is the mass fraction of dry matter, expressed as a percentage, in the sample. Calculate the mean of the duplica
41、tes and report results below 20 mg/kg as “less than 20 mg/kg”, and results of 20 mg/kg or more to the nearest 10 mg/kg. 10 Test report The report shall include the following information: a) a reference to this International Standard, ISO 9197:2016; b) the date and place of testing; c) the complete i
42、dentification of the sample tested; ISO 2016 All rights reserved 3BS ISO 9197:2016ISO 9197:2016(E) 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.4 ISO 2016
43、All rights reservedBS ISO 9197:2016ISO 9197:2016(E) Annex A (informative) Precision A.1 General The following results were obtained in an interlaboratory trial conducted by the Scandinavian Pulp, Paper and Board Testing Committee. The repeatability and reproducibility limits reported are estimates o
44、f the maximum difference which should be expected in 19 of 20 instances, when comparing two test results for material similar to those described under similar test conditions. These estimates may not be valid for different materials or different test conditions. NOTE Repeatability and reproducibilit
45、y limits are calculated by multiplying the repeatability and reproducibility standard deviations by 2,77, where 2,77 = 1,96 2. A.2 Repeatability Data not available. A.3 Reproducibility Nine laboratories analysed four samples as specified in this International Standard. Each sample was analysed in du
46、plicate. The mean mass fraction of chloride ion and the standard deviation (between laboratories) were calculated according to ISO/TR 24498. The results are given in Table A.1. Table A.1 Sample Mean mass fraction of chloride ion Reproducibility standard deviation C o e f f i c ie n t of variation Re
47、producibility limit mg/kg mg/kg s R CoV,R % R mg/kg Machine-glazed (MG) paper from bleached kraft pulp (14,6) a (3,6) 24,7 10,0 Birch bleached kraft pulp 27,1 6,6 24,4 18,3 Copy paper 1 297 25 8,4 69,2 Copy paper 2 1 240 76 6,1 211 aThe value is under the lower limit of determination. ISO 2016 All r
48、ights reserved 5BS ISO 9197:2016ISO 9197:2016(E) Annex B (informative) 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 s
49、ame principle, but differ in details. It is a principle of standardization 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 of equipment. In practice, this means that the course of the analysis cannot be described in this International Standard in s
