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

1、English price group 11No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 27.120.30!%X9w“2532284www.din.deDIN EN ISO 15

2、366-2Nuclear 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 below (ISO 15366-2:2014);Eng

3、lish version EN ISO 15366-2:2016,English translation of DIN EN ISO 15366-2:2016-07Kernbrennstofftechnologie Chemische Trennung und Reinigung von Uran und Plutonium in Salpetersure-Lsungen fr Isotopen- und Isotopenverdnnungsanalysen mittels Lsemittelextraktions-Chromatographie Teil 2: Proben mit Plut

4、onium und Uranium im Nanogrammbereich und weniger (ISO 15366-2:2014);Englische Fassung EN ISO 15366-2:2016,Englische bersetzung von DIN EN ISO 15366-2:2016-07Technologie du combustible nuclaire Sparation et purification chimique de luranium et du plutonium dans les solutions dacide nitrique par extr

5、action chromatographique par solvant pour les mesures isotopiques et les analyses par dilution isotopique Partie 2: chantillons ayant des teneurs en plutonium et en uranium de lordre du nanogramme et infrieures (ISO 15366-2:2014);Version anglaise EN ISO 15366-2:2016,Traduction anglaise de DIN EN ISO

6、 15366-2:2016-07www.beuth.deDTranslation by DIN-Sprachendienst.Document comprises 16 pagesJuly 201607.16In case of doubt, the German-language original shall be considered authoritative.DIN EN ISO 15366-2:2016-07 2 A comma is used as the decimal marker. National foreword International Standard ISO 15

7、366-2:2014 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 “Nuclear energy, nuclear tech

8、nologies, and radiological protection” (Secretariat: AFNOR, France). The responsible German body involved in its preparation was DIN-Normenausschuss Materialprfung (DIN Standards Committee Materials Testing), Working Committee NA 062-07 FBR Fachbereichsbeirat Kerntechnik und Strahlenschutz. EUROPEAN

9、 STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 15366-2 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: Sa

10、mples containing plutonium and uranium in the nanogram 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 e

11、t les analyses par dilution isotopique Partie 2: 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 Isotopenverdnn

12、ungsanalysen mittels Lsemittelextraktions-Chromatographie 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 stipul

13、ate 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 St

14、andard 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 the n

15、ational 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, Romania,

16、Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATIO N 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

17、 means reserved worldwide for CEN national Members. Ref. No. EN ISO 15366-2:2016 E EN ISO 15366-2:2016 (E) Contents Page 2DIN EN ISO 15366-2:2016-07 European foreword . 3 Foreword 4 1 Scope 5 2 Principle of the method 5 3 Apparatus . 6 4 Reagents . 6 5 Procedure (see Figure 1) 7 6 Characteristics of

18、 the separation 9 7 Quality control . 9 8 Interferences . 10 Annex 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) . 11 A.1 General . 11 A.2 Appar

19、atus 11 A.3 Coating the polyethylene support with TOPO . 11 A.4 Packing the columns . 12 A.5 Conditioning the columns . 12 Bibliography . 14 EN ISO 15366-2:2016 (E) European foreword The text of ISO 15366-2:2014 has been prepared by Technical Committee ISO/TC 85 “Nuclear energy, nuclear technologies

20、, 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 “Nuclear energy, nuclear technologies, and radiological protection” the secretariat of which is held by AFNOR. This European Sta

21、ndard 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 standards shall be withdrawn at the latest by October 2016. Attention is drawn to the possibility that some of the elements of

22、 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 Internal Regulations, the national standards organizations of the following countries are bound to implement this European

23、Standard: 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, Romania, Slovakia, Slovenia

24、, 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 modification. 3DIN EN ISO 15366-2:2016-07 ForewordISO (the International Organization for Standardization) is a worldwide federatio

25、n 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 represented on that committee.

26、 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 develop this document and thos

27、e 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/IEC Directives, Part 2. w

28、ww.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 any patent rights identified during the development of the document w

29、ill 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 an explanation on the meaning of ISO specific terms and expressions

30、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 this document is ISO/TC 85, Nuclear Energy, Subcommittee SC 5, Nuclear

31、 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 general title Chemical separation and purification of uranium and plu

32、tonium 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 plutonium and uranium amounts in the nanogram range and belowEN ISO

33、 15366-2:2016 (E) 4DIN EN ISO 15366-2:2016-07 1 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 in samples of high active liquid waste of spent fuel reprocessing plants, prior

34、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 the same chemistry, using smaller columns, different support material and special

35、 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 preparation of the columns and the column support materials.In comparison with ISO 153

36、66-1, 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 based on a column extraction chromatography using tri-n-octylphosphine-oxide (TO

37、PO) 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 silica gel powder coated with the TOPO. Plutonium(IV) and uranium(VI) in 3 moll1

38、nitric 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 acid5; uranium is eluted by an ammonium carbamate solution and finally purified f

39、rom 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 measurement of blank and/or control sample is recommended to verify the analysis.Blan

40、ks 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 prepared and separated along with the sample to verify that suitable valency adjustm

41、ent, isotopic equilibration and separation efficiency are achieved.The whole process is carried out under clean conditions preferably in a laminar flow fume hood.EN ISO 15366-2:2016 (E) 5DIN EN ISO 15366-2:2016-07 3 Apparatus3.1 Biological shielding, e.g. shielded glove box or fume cupboard, prefera

42、bly a laminar flow fume cupboard.3.2 Disposable polypropylene columns and frits (see Figure A.1). Type: micro-column. The packing and conditioning of the columns are described in Annex A. The chromatographic columns shall be disposed of in the radioactive waste after use.3.3 Two hot plates.3.4 Stand

43、ard laboratory equipment (flasks and beakers, pipettes, glassware, stands and supports for columns, sample vials, fraction tubes, etc.). It is recommended to leach all equipment, which will be in contact with samples, eluates or eluents with nitric acid (4.1) and distilled water before use. After dr

44、ying, store it in plastic bags in a clean area.3.5 PTFE vials, of dimensions: volume 15 ml, diameter 28 mm, height 37 mm. With screw caps and metal jackets.These vials may be used at least 10 times, after a careful cleaning with hot nitric acid, followed by a rinsing with demineralized or de-ionized

45、 water.4 ReagentsUse only reagents of recognized suprapure grade or equivalent. All aqueous solutions shall be prepared with distilled water (resistivity 1 Mm to 10 Mm).4.1 Concentrated nitric acid and nitric acid solutions, c(HNO3) = 6 moll1and 3 moll1.4.2 Formic acid solution, c(HCOOH) = 1 moll1.4

46、.3 Ammonium carbamate CAS No. 1111-78-0 solution, c(NH4CO2NH2) = 0,7 moll1.4.4 Polyethylene powder1)GUR X 117/PE-UHMW Ultra-high-molecular grain size 25 m to 95 m, pore size 5 m (see A.2.5).4.5 L(+)-Ascorbic acid solution c(C6H8O6) = 105moll1or c(C6H8O6) = 103moll1in formic acid solution (4.2)4.6 Tr

47、i-n-octylphosphine-oxide, c(TOPO) = 0,2 moll1solution in cyclohexane.WARNING This reagent is flammable and should always be handled in a well-ventilated place and never in the vicinity of a naked flame.4.7 Iron(II) sulfate solution, c(FeSO4) = 0,1 moll1or c(FeSO4) = 0,8 moll1in water. To be prepared

48、 freshly for each working session.4.8 Sodium nitrite solution, c(NaNO2) = 1 moll1or c(NaNO2) = 5 moll1in water. To be prepared freshly for each working session.4.9 Aqua regia, mixture 3:1 (per volume) of concentrated hydrochloric acid and concentrated nitric acid.1) Silica gel may also be used. See

49、ISO 15366-1.EN ISO 15366-2:2016 (E) 6DIN EN ISO 15366-2:2016-07 4.10 Concentrated hydrochloric acid and hydrochloric acid solution c(HCl) = 6 moll14.11 Anion exchange resin AG MP1, slurry in distilled water. Fill the mini-columns (3.2) with about 0,5 ml of the slurry. Condition the columns with two times 1 ml of distilled water and with three times 1 ml concentrated hydrochloric acid (4.10) immediately before use.5 Procedure (see Figure 1)NOTE This procedure is an example. If e