EN ISO 15366-2-2016 en Nuclear fuel technology - Chemical separation and purification of uranium and plutonium in nitric acid solutions for isotopic and isotopic dilution analysis .pdf

1、BS ISO 15366-2:2014Nuclear fuel technology Chemical separation andpurification of uraniumand plutonium in nitric acidsolutions for isotopic andisotopic dilution analysisby solvent extractionchromatographyPart 2: Samples containing plutonium anduranium in the nanogram range and belowBS EN ISO 15366-2

2、:2016(ISO 15366-2:2014)BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06BS EN ISO 15366-2:2016 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO 15366-2:2016. It is identical to ISO 15366-2:2014. It supersedes BS ISO 15366-2:201

3、4 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee NCE/9, Nuclear fuel cycle technology.A list of organizations represented on this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 necessary prov

4、isions of a contract. Users are responsible for its correct application. The British Standards Institution 2016. Published by BSI Standards Limited 2016ISBN 978 0 580 90934 4ICS 27.120.30Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was publis

5、hed under the authority of the Standards Policy and Strategy Committee on 30 June 2014.Amendments/corrigenda issued since publicationDate Text affected30 June 2016 This corrigendum renumbers BS ISO 15366-2:2014 as BS EN ISO 15366-2:2016EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 15366-2

6、 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 2: Samples containing plutonium and uranium in the nanogr

7、am range and below (ISO 15366-2:2014) 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 dilution isotopique - Partie 2:

8、 chantillons ayant des teneurs en plutonium et en uranium de lordre du nanogramme et infrieures (ISO 15366-2:2014) Kernbrennstofftechnologie - Chemische Trennung und Reinigung von Uran und Plutonium in Salpetersure-Lsungen fr Isotopen- und Isotopenverdnnungsanalysen mittels Lsemittelextraktions-Chro

9、matographie - Teil 2: Proben mit Plutonium und Uranium im Nanogrammbereich und weniger (ISO 15366-2:2014)This European Standard was approved by CEN on 21 February 2016. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European S

10、tandard 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 Standard exists in three official versions (Eng

11、lish, 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 the national standards bodies of Austria, Belgium,

12、 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, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerlan

13、d, 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 any means reserved worldwide for CEN national Memb

14、ers. Ref. No. EN ISO 15366-2:2016 EBS ISO 15366-2:2014ISO 15366-2:2014(E) ISO 2014 All rights reserved iiiContents PageForeword iv1 Scope . 12 Principle of the method . 13 Apparatus . 24 Reagents 25 Procedure (see Figure 1) 36 Characteristics of the separation 57 Quality control 58 Interferences 6An

15、nex A (normative) Packing and conditioning of the chromatographic mini-columns as used in the ISO 15366-2 procedure, loaded with an inert polyethylene support coated with tri-n-octyl-phosphine-oxide (TOPO) 7Bibliography .10BS EN ISO 15366-2:2016EN ISO 15366-2:2016 (E)EN ISO 15366-2:2016 (E) 3 Europe

16、an foreword The text of ISO 15366-2:2014 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 15366-2:2016 by Technical Committee CEN/TC 430

17、 “Nuclear 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 nation

18、al standards 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-CE

19、NELEC 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,

20、Iceland, 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 15366-2:2014 has been approved by CEN as EN ISO 15366-2:2016 without any mo

21、dification. BS ISO 15366-2:2014ISO 15366-2:2014(E) ISO 2014 All rights reserved iiiContents PageForeword iv1 Scope . 12 Principle of the method . 13 Apparatus . 24 Reagents 25 Procedure (see Figure 1) 36 Characteristics of the separation 57 Quality control 58 Interferences 6Annex A (normative) Packi

22、ng and conditioning of the chromatographic mini-columns as used in the ISO 15366-2 procedure, loaded with an inert polyethylene support coated with tri-n-octyl-phosphine-oxide (TOPO) 7Bibliography .10BS EN ISO 15366-2:2016ISO 15366-2:2014(E)BS ISO 15366-2:2014ISO 15366-2:2014(E)ForewordISO (the Inte

23、rnational 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 has

24、 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 s

25、tandardization.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 acco

26、rdance 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 such patent rights. Details of a

27、ny 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 constitute an endorsement.For

28、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 informationThe committee responsible for th

29、is document is ISO/TC 85, Nuclear Energy, Subcommittee SC 5, Nuclear Fuel Technology.This first edition, together with the first edition of ISO 15366-1, cancels and replaces the first edition of ISO 15366:1999, which has been technically revised.ISO 15366 consists of the following parts, under the g

30、eneral 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 microgram range and uranium in the milligram range Part 2: Sample containing

31、 plutonium and uranium amounts in the nanogram range and belowiv ISO 2014 All rights reservedBS ISO 15366-2:2014INTERNATIONAL STANDARD ISO 15366-2:2014(E)Nuclear fuel technology Chemical separation and purification of uranium and plutonium in nitric acid solutions for isotopic and isotopic dilution

32、analysis by solvent extraction chromatography Part 2: Samples containing plutonium and uranium in the nanogram range and below1 ScopeThis part of ISO 15366 describes procedures to chemically separate and purify uranium and plutonium in dissolved solutions of irradiated light water reactor fuels and

33、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 ISO 15366 describes a slightly different separation technique from ISO 15366-1, based on t

34、he same chemistry, using smaller columns, different support material and special purification steps, applicable to samples containing plutonium and uranium amounts in the nanogram range and below. The detection limits were found to be 500 pg plutonium and 500 pg uranium. Annex A describes the prepar

35、ation of the columns and the column support materials.In comparison with ISO 15366-1, as uranium and plutonium amounts are lowest, additional purification on an anion exchange resin is performed.2 Principle of the methodThe chemical separation of small plutonium and uranium amounts (500 pg) is also

36、based on a column extraction chromatography using tri-n-octylphosphine-oxide (TOPO) as extractant.34The necessary valency adjustment prior to the separation is done with iron(II) sulfate and sodium nitrite. The extraction process is performed in disposable mini-columns loaded with a polyethylene or

37、silica gel powder coated with the TOPO. Plutonium(IV) and uranium(VI) in 3 moll1nitric acid medium are selectively extracted into the TOPO while americium, the fission products and other interfering elements are not retained. Plutonium is eluted after reduction to the trivalent state with ascorbic a

38、cid5; uranium is eluted by an ammonium carbamate solution and finally purified from ammonium salts by an ion exchange separation6or fuming by 14 moll1nitric acid.In order to ensure a favourable kinetics of chemical reactions the (gravity) column flow rates should not exceed 0,4 mlmin1.Parallel measu

39、rement 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 or cross-contamination between samples.Control samples prepared from certified or analysed materials are also prep

40、ared and separated along with the sample to verify that suitable valency adjustment, isotopic equilibration and separation efficiency are achieved.The whole process is carried out under clean conditions preferably in a laminar flow fume hood. ISO 2014 All rights reserved 1BS EN ISO 15366-2:2016ISO 1

41、5366-2:2014(E)BS ISO 15366-2:2014ISO 15366-2:2014(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. Eac

42、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

43、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

44、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 shall not be hel

45、d 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 information given

46、 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 the following

47、URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 85, Nuclear Energy, Subcommittee SC 5, Nuclear Fuel Technology.This first edition, together with the first edition of ISO 15366-1, cancels and replaces the first edition of ISO 15366:1999, which has been t

48、echnically 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 mic

49、rogram 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 15366-2:2014INTERNATIONAL STANDARD ISO 15366-2:2014(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 2: Samples containing plutonium and uranium in the nanogram range and below1 ScopeThis part of ISO