1、Pulp, paper and board Determination of total chlorine and organically bound chlorineBS ISO 11480:2017BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06 ISO 2017Pulp, paper and board Determination of total chlorine and organically bound chlorinePtes, papier et carton Do
2、sage du chlore total et du chlore li aux matires organiquesINTERNATIONAL STANDARDISO11480Second edition2017-05Reference numberISO 11480:2017(E)National forewordThis British Standard is the UK implementation of ISO 11480:2017. It supersedes BS ISO 11480:1997, which is withdrawn.The UK participation i
3、n 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 include all the necessary provisions of a contract. Users a
4、re responsible for its correct application. The British Standards Institution 2017 Published by BSI Standards Limited 2017ISBN 978 0 580 90641 1ICS 85.060; 85.040Compliance with a British Standard cannot confer immunity from legal obligations. This British Standard was published under the authority
5、of the Standards Policy and Strategy Committee on 30 June 2017.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STANDARDBS ISO 11480:2017 ISO 2017Pulp, paper and board Determination of total chlorine and organically bound chlorinePtes, papier et carton Dosage du chlore total e
6、t du chlore li aux matires organiquesINTERNATIONAL STANDARDISO11480Second edition2017-05Reference numberISO 11480:2017(E)BS ISO 11480:2017ISO 11480:2017(E)ii ISO 2017 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2017, Published in SwitzerlandAll rights reserved. Unless otherwise specified, no
7、 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 address below or ISOs membe
8、r body in the country of the requester.ISO copyright officeCh. de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgBS ISO 11480:2017ISO 11480:2017(E)ii ISO 2017 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2017, Publish
9、ed in SwitzerlandAll rights reserved. Unless 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
10、 can be requested from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCh. de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgISO 11480:2017(E)Foreword ivIntroduction v1
11、 Scope . 12 Normative references 13 Terms and definitions . 14 Microcoulometric method 14.1 Principle 14.2 Chemicals and reagents . 24.3 Precautions 24.4 Apparatus 24.5 Pretreatment of the sample . 34.6 Extraction with acid nitrate solution . 44.7 Combustion 44.8 Blanks 54.9 Checks . 54.10 Calculati
12、on 54.11 Interference from bromine compounds 55 Schniger method . 65.1 Principle 65.2 Chemicals and reagents . 65.3 Precautions 75.4 Apparatus 75.5 Sampling and sample preparation . 75.6 Extraction with acid nitrate solution . 85.7 Combustion 85.8 Ion chromatographic determination 85.9 Blanks 95.10
13、Calculation 96 Test report . 9Annex A (informative) Precision (Microcoulometric method) 11Annex B (informative) Precision (Schniger method) 13Annex C (informative) Laboratory manuals 15Bibliography .16 ISO 2017 All rights reserved iiiContents PageBS ISO 11480:2017ISO 11480:2017(E)ForewordISO (the In
14、ternational 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. Each member body interested in a subject for which a technical committee h
15、as 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 International Electrotechnical Commission (IEC) on all matters of electrotechnical
16、 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 types of ISO documents should be noted. This document was drafted in ac
17、cordance 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 not be held responsible for identifying any or all such patent rights. D
18、etails 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 information given for the convenience of users and does not constitute
19、 an endorsement.For an explanation on the voluntary nature of standards, the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the f
20、ollowing URL: www .iso .org/ iso/ foreword .html.This document was prepared by Technical Committee ISO/TC 6, Paper, board and pulps.This second edition cancels and replaces the first edition (ISO 11480:1997), which has been technically revised to include the option of using the Schniger combustion m
21、ethod combined with ion chromatography.iv ISO 2017 All rights reservedBS ISO 11480:2017ISO 11480:2017(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normal
22、ly 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 and non-governmental, in liaison with ISO, also take part in the
23、 work. ISO collaborates closely with the International 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 d
24、ifferent approval criteria needed for the different 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 docum
25、ent may be the subject of patent rights. ISO shall not 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 .o
26、rg/ patents).Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the voluntary nature of standards, the meaning of ISO specific terms and expressions related to conformity assessment, as well as informati
27、on about ISOs adherence to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: www .iso .org/ iso/ foreword .html.This document was prepared by Technical Committee ISO/TC 6, Paper, board and pulps.This second edition cancels and replaces the
28、first edition (ISO 11480:1997), which has been technically revised to include the option of using the Schniger combustion method combined with ion chromatography.iv ISO 2017 All rights reserved ISO 11480:2017(E)IntroductionThis document specifies two procedures for the determination of total and org
29、anically bound chlorine in pulp, paper and board. The microcoulometric method (Clause 4) is based on combustion in a heated tube followed by microcoulometric titration. The Schniger method (Clause 5) is based on the so-called Schniger combustion followed by ion chromatography.The choice of procedure
30、 depends on the availability of the apparatus and on the risk of interference by bromine compounds in the sample. In the microcoulometric method, the result does not strictly represent the chlorine content since it includes part of any bromine present in the sample. This procedure should thus be avo
31、ided if there is a risk that the sample has a high bromine content.More work is involved in the Schniger method than in the microcoulometric method. However, since the end determination is performed by ion chromatography, the result is unambiguously chlorine. The Schniger method also requires a larg
32、er sample. Consequently, the result is more representative. On the other hand, the microcoulometric method is faster and several replicate determinations can be performed in a short time. ISO 2017 All rights reserved vBS ISO 11480:2017BS ISO 11480:2017Pulp, paper and board Determination of total chl
33、orine and organically bound chlorine1 ScopeThis document specifies two alternative procedures for the determination of total and organically bound chlorine in pulp, paper and board. It is applicable to all types of pulp, paper and board. The lower limit of the determination is about 20 mg/kg.2 Norma
34、tive referencesThe following documents are referred to in the text in such a way that some or all of their content constitutes requirements of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any ame
35、ndments) applies.ISO 287, Paper and board Determination of moisture content of a lot Oven-drying methodISO 638, Paper, board and pulps Determination of dry matter content Oven-drying method3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.ISO and IEC
36、 maintain terminological databases for use in standardization at the following addresses: ISO Online browsing platform: available at h t t p :/ www .iso .org/ obp IEC Electropedia: available at h t t p :/ www .electropedia .org/ 3.1total chlorinetotal amount of the element chlorine present3.2organic
37、ally bound chlorineamount of organically bound chlorine present4 Microcoulometric method4.1 PrincipleDetermination of the chlorine content of the sample by combustion under controlled conditions in a quartz tube at high temperature. The combustion gases are fed through an electrolyte solution where
38、all chlorine, now transformed to hydrogen chloride, is absorbed and determined by microcoulometry. For determination of the organically bound chlorine content, the inorganic chlorine compounds are extracted with dilute nitric acid before combustion.NOTE 1 If determination of organically bound chlori
39、ne is not required, the extraction with acid nitrate is omitted.NOTE 2 Any bromine present will interfere and cause a positive error. For details, see 4.11.INTERNATIONAL STANDARD ISO 11480:2017(E) ISO 2017 All rights reserved 1BS ISO 11480:2017ISO 11480:2017(E)4.2 Chemicals and reagentsAll chemicals
40、 used shall be of analytical reagent grade. Water for the preparation of solutions, or used in the procedure, shall be distilled water of high purity or equivalent. High blanks (see 4.8) can be due to impure water. The water can then be purified by treating it with activated carbon (4.2.4).4.2.1 Aci
41、d nitrate solution, stock solution. Dissolve 17 g of sodium nitrate (NaNO3) in distilled water. Add 1,4 ml of nitric acid (HNO3) density 1,40 g/ml, and dilute to 1 l with distilled water. (This solution is only required for the determination of organically bound chlorine.)4.2.2 Acid nitrate solution
42、, working solution. Dilute 50 ml of the stock solution (4.2.1) to 1 l with distilled water. (This solution is only required for the determination of organically bound chlorine.)4.2.3 Sulfuric acid (H2SO4), density 1,84 g/ml.4.2.4 Activated carbon, for adsorption of water-soluble organic material in
43、the determination of organically bound chlorine. (Suitable carbon is provided by manufacturers of combustion apparatus.)4.2.5 Electrolyte solution, for use in the microcoulometer. Dilute 75 ml of glacial (98 %) acetic acid (CH3COOH) to 100 ml with water.Addition of sodium perchlorate (NaClO4) and su
44、lfamic acid (NH2SO3H) to the absorption solution is recommended by some manufacturers of microcoulometers. Such additions are optional.One manufacturer recommends a solution prepared by dissolving 1,35 g of sodium acetate (NaCH3COO) in 850 ml of glacial acetic acid and diluting to 1 000 ml with wate
45、r.4.2.6 Hydrochloric acid, c(HCl) = 0,010 0 mol/l.4.2.7 2-Chlorobenzoic acid reference solution. Dissolve 110,3 mg of ClC6H4COOH in distilled water and dilute to 100 ml in a volumetric flask. This solution contains 250 mg of organically bound chlorine per litre. Dilute the solution as required befor
46、e use.4.2.8 Compressed gases. Oxygen is required for the combustion. Other gases may also be required in order to control the combustion. It is essential that all gases used are free from chlorine and bromine in any form.NOTE It has been reported that chlorinated solvents have been used to clean the
47、 gas containers.4.3 PrecautionsChlorine compounds in small quantities are present almost everywhere, in chemicals, on the surfaces of the equipment, on the skin and in the laboratory air. It is therefore of utmost importance to take every measure to avoid contamination of samples and solutions. In p
48、articular, the risk of contamination from the laboratory air should be observed. Such contamination can come from reagents (solvents) stored in the laboratory, as well as from outdoor sources, for example, a bleaching plant.Clean all equipment before use with dilute nitric acid and flush with pure w
49、ater.4.4 ApparatusOf the items listed below, items 4.4.1 through 4.4.4 are required only if organic chlorine has to be determined. Item 4.4.7 is required only if total chlorine has to be determined.4.4.1 Conical flasks, 250 ml, of chemically resistant glass, with standard tapered glass stoppers or polytetrafluoroethylene (PTFE)-lined screw caps.2 ISO 2017 All rights reservedBS ISO 11480:2017ISO 11480:2017(E)4.2 Chemicals and reagentsAll chemicals used shall be of analytical reagent grade. Water for the preparat
