1、BSI Standards PublicationBS ISO 15366-1:2014Nuclear fuel technology Chemical separation andpurification of uraniumand plutonium in nitric acidsolutions for isotopic andisotopic dilution analysisby solvent extractionchromatographyPart 1: Samples containing plutonium inthe microgram range and uranium
2、in themilligram rangeBS EN ISO 15366-1:2016the microgram range and uranium in the milligram range (ISO 15366-1:2014)BS EN ISO 15366-1:2016 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO 15366-1:2016. It is identical to ISO 15366-1:2014. It supersedes BS ISO
3、 15366-1:2014 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee NCE/9, Nuclear fuel cycle technology.A list of organizations represented on this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 ne
4、cessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2016. Published by BSI Standards Limited 2016ISBN 978 0 580 90941 2ICS 27.120.30Compliance with a British Standard cannot confer immunity from legal obligations.This British Standar
5、d was published under the authority of the Standards Policy and Strategy Committee on 30 June 2014.Amendments/corrigenda issued since publicationDate Text affected31 May 2016 This corrigendum renumbers BS ISO 15366-1:2014 as BS EN ISO 15366-1:2016EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN
6、ISO 15366-1 April 2016 ICS 27.120.30 English Version Nuclear fuel technology - Chemical separation and purification of uranium and plutonium in nitric acid solutions for isotopic and isotopic dilution analysis by solvent extraction chromatography - Part 1: Samples containing plutonium in the microgr
7、am range and uranium in the milligram range (ISO 15366-1:2014) Technologie du combustible nuclaire - Sparation et purification chimiques de luranium et du plutonium dans les solutions dacide nitrique par extraction chromatographique par solvant pour les mesures isotopiques et les analyses par diluti
8、on isotopique - Partie 1: chantillons ayant des teneurs en plutonium de lordre du microgramme et en uranium de lordre du milligramme (ISO 15366-1:2014) Kernbrennstofftechnologie - Chemische Trennung und Reinigung von Uran und Plutonium in Salpetersure-Lsungen fr Isotopen- und Isotopenverdnnungsanaly
9、sen mittels Lsemittelextraktions-Chromatographie - Teil 1: Proben mit Plutonium im Mikrogrammbereich und Uranium im Milligrammbereich (ISO 15366-1:2014) This European Standard was approved by CEN on 21 February 2016. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which sti
10、pulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European
11、 Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are th
12、e national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romani
13、a, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey andUnited Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2016 CEN All rights of exploitation in any form and by an
14、y means reserved worldwide for CEN national Members. Ref. No. EN ISO 15366-1:2016 EBS ISO 15366-1:2014ISO 15366-1:2014(E) ISO 2014 All rights reserved iiiContents PageForeword iv1 Scope . 12 Principle of the method . 13 Apparatus . 14 Reagents 25 Procedure (see Figure 1) 26 Characteristics of the se
15、paration 47 Quality control 58 Interferences 5Annex A (normative) Packing and conditioning of the chromatographic columns as used in the ISO 15366 1 procedure, loaded with an inert silica support coated with tri-n-octyl-phosphine-oxide (TOPO) . 7Bibliography .10EN ISO 15366-1:2016 (E) 3 European for
16、eword The text of ISO 15366-1:2014 has been prepared by Technical Committee ISO/TC 85 “Nuclear energy, nuclear technologies, and radiological protection” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 15366-1:2016 by Technical Committee CEN/TC 430 “Nucl
17、ear energy, nuclear technologies, and radiological protection” the secretariat of which is held by AFNOR. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by October 2016, and conflicting national sta
18、ndards shall be withdrawn at the latest by October 2016. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. According to the CEN-CENELEC
19、Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Icelan
20、d, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 15366-1:2014 has been approved by CEN as EN ISO 15366-1:2016 without any modifica
21、tion. BS EN ISO 15366-1:2016EN ISO 15366-1:2016 (E)BS ISO 15366-1:2014ISO 15366-1:2014(E) ISO 2014 All rights reserved iiiContents PageForeword iv1 Scope . 12 Principle of the method . 13 Apparatus . 14 Reagents 25 Procedure (see Figure 1) 26 Characteristics of the separation 47 Quality control 58 I
22、nterferences 5Annex A (normative) Packing and conditioning of the chromatographic columns as used in the ISO 15366 1 procedure, loaded with an inert silica support coated with tri-n-octyl-phosphine-oxide (TOPO) . 7Bibliography .10BS EN ISO 15366-1:2016ISO 15366-1:2014(E)BS ISO 15366-1:2014ISO 15366-
23、1:2014(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 normally carried out through ISO technical committees. Each member body interested in a subject for w
24、hich 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 International Electrotechnical Commission (IEC) on all
25、 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 types of ISO documents should be noted. Thi
26、s document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2. www.iso.org/directivesAttention 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 su
27、ch 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. www.iso.org/patentsAny trade name used in this document is information given for the convenience of users and does not
28、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) see the following URL: Foreword - Supplementary informationTh
29、e committee responsible for this document is ISO/TC 85, Nuclear energy, nuclear technologies, and radiological protection, Subcommittee SC 5, Nuclear fuel cycle.This first edition, together with the first edition of ISO 15366-2, cancels and replaces the first edition of ISO 15366:1999, which has bee
30、n technically revised.ISO 15366 consists of the following parts, under the general title Chemical separation and purification of uranium and plutonium in nitric acid solutions for isotopic and isotopic dilution analysis by solvent extraction chromatography Part 1: Sample containing plutonium in the
31、microgram range and uranium in the milligram range Part 2: Sample containing plutonium and uranium amounts in the nanogram range and belowiv ISO 2014 All rights reservedBS ISO 15366-1:2014INTERNATIONAL STANDARD ISO 15366-1:2014(E)Nuclear fuel technology Chemical separation and purification of uraniu
32、m and plutonium in nitric acid solutions for isotopic and isotopic dilution analysis by solvent extraction chromatography Part 1: Samples containing plutonium in the microgram range and uranium in the milligram range1 ScopeThis part of ISO 15366 describes procedures to chemically separate and purify
33、 uranium and plutonium in dissolved solutions of irradiated light water reactor fuels and in samples of high active liquid waste of spent fuel reprocessing plants, prior to their isotopic analysis by e.g. mass spectrometric method (see ISO 82991) or alpha spectrometry (see ISO 114832).This part of I
34、SO 15366, describes a technique for the separation of uranium and plutonium in spent fuel type samples based on chromatographic method. The procedure applies to samples containing 1 g to 150 g Pu (IV) and (VI) and 0,1 mg to 2 mg U (IV) and (VI) in up to 2 ml of 3 moll1nitric acid solution. It is app
35、licable to mixtures of uranium and plutonium in which the U/Pu-ratio can range from 0 up to 200.2 Principle of the methodThe chemical separation is based on a column extraction chromatography using tri-n-octylphosphine-oxide (TOPO) as extractant.34The necessary valency adjustment prior to the separa
36、tion is done with iron(II) sulfate and sodium nitrite. The extraction process is performed in disposable columns loaded with a silica gel powder coated with the TOPO.5Plutonium(IV) and uranium(VI) in 3 moll1nitric acid medium are selectively extracted into the TOPO while americium, the fission produ
37、cts and other interfering elements are not retained. Plutonium is eluted after reduction to the trivalent state with ascorbic acid6; uranium is eluted by an ammonium carbamate solution. Besides the measurement by mass spectrometry, the plutonium fractions are also measured by alpha spectrometry for
38、the determination of the isotopic abundance of 238Pu (mass spectrometry might be biased by residual amounts of uranium in the plutonium fraction) and for checking the recovery of plutonium.In order to ensure favourable kinetics of the chemical reactions, the (gravity) column flow rates should not ex
39、ceed 0,1 mlmin1.Parallel measurement of blank and/or control sample is recommended to verify the analysis.Blanks are run in parallel with the samples to verify the absence of significant external cross-contamination and cross-contamination between samples.Control samples prepared from certified or a
40、nalysed materials are also prepared and separated along with the sample to verify that suitable valency adjustment, isotopic equilibration and separation efficiency are achieved.3 Apparatus3.1 Biological shielding, e.g. shielded glove box or fume cupboard. ISO 2014 All rights reserved 1BS EN ISO 153
41、66-1:2016ISO 15366-1:2014(E)BS ISO 15366-1:2014ISO 15366-1:2014(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 normally carried out through ISO technical c
42、ommittees. 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 work. ISO collaborates closely with t
43、he 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 different approval criteria needed for
44、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. www.iso.org/directivesAttention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO sh
45、all 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. www.iso.org/patentsAny trade name used in this document is inf
46、ormation 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) see
47、the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 85, Nuclear energy, nuclear technologies, and radiological protection, Subcommittee SC 5, Nuclear fuel cycle.This first edition, together with the first edition of ISO 15366-2, cancels and re
48、places the first edition of ISO 15366:1999, which has been technically revised.ISO 15366 consists of the following parts, under the general title Chemical separation and purification of uranium and plutonium in nitric acid solutions for isotopic and isotopic dilution analysis by solvent extraction c
49、hromatography Part 1: Sample containing plutonium in the microgram range and uranium in the milligram range Part 2: Sample containing plutonium and uranium amounts in the nanogram range and belowiv ISO 2014 All rights reservedBS ISO 15366-1:2014INTERNATIONAL STANDARD ISO 15366-1:2014(E)Nuclear fuel technology Chemical separation and purification of uranium and plutonium in nitric acid solutions for isotopic and isotopic dilution analysis by solvent extraction chromatography Part 1: Samples containing plutonium in the
