1、Nuclear energy Determination of chlorine and fluorine in uranium dioxide powder and sintered pelletsBS ISO 22875:2017BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06 ISO 2017Nuclear energy Determination of chlorine and fluorine in uranium dioxide powder and sintered
2、pelletsnergie nuclaire Dtermination du chlore et du fluor dans les poudres de dioxyde duranium et les pastilles frittesINTERNATIONAL STANDARDISO22875Second edition2017-08Reference numberISO 22875:2017(E)National forewordThis British Standard is the UK implementation of ISO 22875:2017.The UK particip
3、ation in its preparation was entrusted to Technical Committee NCE/9, Nuclear fuel cycle technology.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 are resp
4、onsible for its correct application. The British Standards Institution 2017 Published by BSI Standards Limited 2017ISBN 978 0 580 91678 6ICS 27.120.30Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standa
5、rds Policy and Strategy Committee on 30 September 2017.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STANDARDBS ISO 22875:2017 ISO 2017Nuclear energy Determination of chlorine and fluorine in uranium dioxide powder and sintered pelletsnergie nuclaire Dtermination du chlore
6、et du fluor dans les poudres de dioxyde duranium et les pastilles frittesINTERNATIONAL STANDARDISO22875Second edition2017-08Reference numberISO 22875:2017(E)BS ISO 22875:2017ISO 22875:2017(E)ii ISO 2017 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2017, Published in SwitzerlandAll rights rese
7、rved. 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 can be requested from either IS
8、O 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.orgBS ISO 22875:2017ISO 22875:2017(E)ii ISO 2017 All rights reservedCOPYRIGHT
9、PROTECTED DOCUMENT ISO 2017, Published 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
10、prior written permission. Permission 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 228
11、75:2017(E)Foreword ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 15 Reagents 16 Apparatus . 37 Procedure. 57.1 Calibration 57.1.1 Ion chromatography calibration 57.1.2 Millivoltmeter calibration 57.2 Sample pyrohydrolysis . 67.2.1 Blank test 67.2.2 Uranium
12、 dioxide powder sample 77.2.3 Uranium dioxide pellet sample . 77.3 Measurement of pyrohydrolysis solutions 87.3.1 Ion chromatography measurement . 87.3.2 Measurement with an ion-selective electrode . 88 Expression of results 88.1 Calculation 88.2 Validation limits 108.3 Determinations limits 108.4 D
13、etermination uncertainty 109 Test report 10Bibliography .12 ISO 2017 All rights reserved iiiContents PageBS ISO 22875:2017ISO 22875:2017(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparin
14、g 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 and non-governmental, in liai
15、son with ISO, also take part in the 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 Dire
16、ctives, Part 1. In particular the different 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
17、 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. 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 dec
18、larations 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 an endorsement.For an explanation on the voluntary nature of standards, the meaning of ISO specific terms and expressions related to conformi
19、ty assessment, as well as information 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 85, Nuclear energy, nuclear technolo
20、gies and radiological protection, Subcommittee SC 5, Nuclear installations, processes and technologies.This second edition cancels and replaces the first edition (ISO 22875:2008), which has been technically revised with the following changes: pyrohydrolysis temperature is lowered; information has be
21、en added concerning decomposition of species including fluoride and chloride (see footnote 2); calculation of the result takes into account pyrohydrolysis yield if needed.iv ISO 2017 All rights reservedBS ISO 22875:2017ISO 22875:2017(E)ForewordISO (the International Organization for Standardization)
22、 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 right to be repre
23、sented 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.The procedures used to devel
24、op 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 accordance with the editorial rules of the ISO/
25、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. Details of any patent rights identified during
26、 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 an endorsement.For an explanation on the vol
27、untary 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 following URL: www .iso .org/ iso/ foreword .h
28、tml.This document was prepared by Technical Committee ISO/TC 85, Nuclear energy, nuclear technologies and radiological protection, Subcommittee SC 5, Nuclear installations, processes and technologies.This second edition cancels and replaces the first edition (ISO 22875:2008), which has been technica
29、lly revised with the following changes: pyrohydrolysis temperature is lowered; information has been added concerning decomposition of species including fluoride and chloride (see footnote 2); calculation of the result takes into account pyrohydrolysis yield if needed.iv ISO 2017 All rights reserved
30、ISO 22875:2017(E)IntroductionThis document describes a method for determining the chlorine and fluorine concentrations in uranium dioxide and in sintered fuel pellets by pyrohydrolysis of samples, followed either by liquid ion-exchange chromatography or by selective electrode measurement of chlorine
31、 and fluorine ions.Many ion chromatography systems and ion-selective electrode measurement systems are available. The equipment and operating procedure are, therefore, not described in detail. ISO 2017 All rights reserved vBS ISO 22875:2017BS ISO 22875:2017Nuclear energy Determination of chlorine an
32、d fluorine in uranium dioxide powder and sintered pellets1 ScopeThis document describes a method for determining chlorine and fluorine in uranium dioxide powder and sintered pellets. It is applicable for the measurement of samples with a mass fraction of chlorine from 5 g/g to 500 g/g and with a mas
33、s fraction of fluorine from 2 g/g to 500 g/g.2 Normative 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 e
34、dition of the referenced document (including any amendments) applies.ISO 3696, Water for analytical laboratory use Specification and test methodsISO 9892:1992, Uranium metal, uranium dioxide powder and pellets, and uranyl nitrate solutions Determination of fluorine content Fluoride ion selective ele
35、ctrode method3 Terms and definitionsNo terms and definitions are listed in this document.ISO and IEC maintain terminological databases for use in standardization at the following addresses: IEC Electropedia: available at h t t p :/ www .electropedia .org/ ISO Online browsing platform: available at h
36、 t t p :/ www .iso .org/ obp4 PrincipleThe samples are pyrohydrolysed at 850 C to 1 000 C in a tubular furnace with steam or moist air or moist oxygen heated to the same temperature. Chlorine and fluorine are trapped as halogenated acids and entrained in an aqueous solution.Two measurement methods m
37、ay be used to measure the chlorine and fluorine ions:a) liquid ion chromatography;b) ion-selective electrode.5 ReagentsUse reagents of recognized analytical grade.5.1 Water, complying with at least grade 1 in accordance with ISO 3696.5.2 Anhydrous sodium chloride (NaCl).5.3 Anhydrous sodium fluoride
38、 (NaF).INTERNATIONAL STANDARD ISO 22875:2017(E) ISO 2017 All rights reserved 1BS ISO 22875:2017ISO 22875:2017(E)5.4 Sodium carbonate (Na2CO3).5.5 Anhydrous sodium bicarbonate (NaHCO3).5.6 Glacial acetic acid (CH3COOH), (CH3COOH) = 1,06 g/ml.5.7 Potassium acetate (CH3COOK).5.8 Concentrated eluent sol
39、ution, c(Na2CO3) = 0,018 mol/l and c(NaHCO3) = 0,017 mol/l.Dissolve 1,908 g of Na2CO3 (5.4) and 1,428 g of NaHCO3(5.5) in water (5.1). Pour into a 1 l volumetric flask. Dilute to 1 l with water (5.1). Homogenize.Instead of Na2CO3, the eluent solution can also be NaOH solution for instance, c(NaOH) =
40、 0,2 mol/l. This solution can be prepared by dilution in water (5.1) of concentrated sodium hydroxide solution (5.22).Depending of the sample to be measured and the column used, Na2CO3or NaOH is used.5.9 Standard eluent solution, add 100 ml of concentrated eluent solution (5.8) to a 1 l volumetric f
41、lask.Dilute to 1 l with water (5.1). Homogenize.5.10 Make-up eluent solution, c(Na2CO3) = 0,09 mol/l and c(NaHCO3) = 0,085 mol/l.Dissolve 9,540 g of Na2CO3(5.4) and 7,140 g of NaHCO3(5.5) in water (5.1). Pour into a 1 l volumetric flask. Dilute to 1 l with water (5.1). Homogenize.5.11 Buffer solutio
42、n, c(CH3COOH) = 0,005 mol/l and c(CH3COOK) = 0,005 mol/l.Pour 250 l of acetic acid (5.6) and 0,50 g of potassium acetate (5.7) into a 1 l polyethylene volumetric flask. Dilute to 1 l with water (5.1). Homogenize.The concentration of the buffer solution can alternatively be chosen between 0,001 mol/l
43、 and 0,1 mol/l.The buffer solution can also be NaOH solution for instance, c(NaOH) = 0,1 mol/l. Instead of Na2CO3, the eluent solution can also be NaOH solution for instance, c(NaOH) = 0,2 mol/l. This solution can be prepared by dilution in water (5.1) of concentrated sodium hydroxide solution (5.22
44、).If NaOH is used for the concentrated eluent solution (5.8), NaOH is also used for the buffer solution.5.12 Chloride reference solution, (Cl) = 1 g/l.Dissolve 1,648 g of dry anhydrous sodium chloride (5.2) in water (5.1). Pour into a 1 l volumetric flask. Dilute to 1 l with water (5.1). Homogenize.
45、To achieve dry sodium salt, heat at 120 C for 4 h just before use and keep in desiccators.5.13 Chloride reference solution, (Cl) = 0,1 g/l.Pipette 10 ml reference solution (5.12) into a 100 ml volumetric flask. Dilute to 100 ml with water (5.1). Homogenize.5.14 Chloride reference solution, (Cl) = 0,
46、01 g/l.Pipette 10 ml reference solution (5.13) into a 100 ml volumetric flask. Dilute to 100 ml with water (5.1) Homogenize.Solutions may be stored for two months.2 ISO 2017 All rights reservedBS ISO 22875:2017ISO 22875:2017(E)5.4 Sodium carbonate (Na2CO3).5.5 Anhydrous sodium bicarbonate (NaHCO3).5
47、.6 Glacial acetic acid (CH3COOH), (CH3COOH) = 1,06 g/ml.5.7 Potassium acetate (CH3COOK).5.8 Concentrated eluent solution, c(Na2CO3) = 0,018 mol/l and c(NaHCO3) = 0,017 mol/l.Dissolve 1,908 g of Na2CO3 (5.4) and 1,428 g of NaHCO3(5.5) in water (5.1). Pour into a 1 l volumetric flask. Dilute to 1 l wi
48、th water (5.1). Homogenize.Instead of Na2CO3, the eluent solution can also be NaOH solution for instance, c(NaOH) = 0,2 mol/l. This solution can be prepared by dilution in water (5.1) of concentrated sodium hydroxide solution (5.22).Depending of the sample to be measured and the column used, Na2CO3o
49、r NaOH is used.5.9 Standard eluent solution, add 100 ml of concentrated eluent solution (5.8) to a 1 l volumetric flask.Dilute to 1 l with water (5.1). Homogenize.5.10 Make-up eluent solution, c(Na2CO3) = 0,09 mol/l and c(NaHCO3) = 0,085 mol/l.Dissolve 9,540 g of Na2CO3(5.4) and 7,140 g of NaHCO3(5.5) in water (5.1). Pour into a 1 l volumetric flask. Dilute to 1 l with water (5.1). Homogenize.5.11 Buffer solution, c(CH3COOH) = 0,005 mol/l and c(CH3COOK) = 0,005 mol/l.Pour 250 l of acetic acid (5.
