DIN EN ISO 15366-1-2016 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 10No 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!%X9u“2532282www.din.deDIN EN ISO 15

2、366-1Nuclear 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 microgram range and uraniumin the milligram range (ISO 1536

3、6-1:2014);English version EN ISO 15366-1:2016,English translation of DIN EN ISO 15366-1:2016-07Kernbrennstofftechnologie Chemische Trennung und Reinigung von Uran und Plutonium in Salpetersure-Lsungen fr Isotopen- und Isotopenverdnnungsanalysen mittels Lsemittelextraktions-Chromatographie Teil 1: Pr

4、oben mit Plutonium im Mikrogrammbereich und Uranium im Milligrammbereich (ISO 15366-1:2014);Englische Fassung EN ISO 15366-1:2016,Englische bersetzung von DIN EN ISO 15366-1:2016-07Technologie du combustible nuclaire Sparation et purification chimique de luranium et du plutonium dans les solutions d

5、acide nitrique par extraction chromatographique par solvant pour les mesures isotopiques et les analyses par dilution isotopique Partie 1: chantillons ayant des teneurs en plutonium de lordre du microgramme et en uranium de lordre du milligramme (ISO 15366-1:2014);Version anglaise EN ISO 15366-1:201

6、6,Traduction anglaise de DIN EN ISO 15366-1:2016-07www.beuth.deDocument comprises 16 pagesDTranslation by DIN-Sprachendienst.July 201607.16In case of doubt, the German-language original shall be considered authoritative.DIN EN ISO 15366-1:2016-07 2 A comma is used as the decimal marker. National for

7、eword International Standard 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/T

8、C 430 “Nuclear energy, nuclear technologies, 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 Kernt

9、echnik und Strahlenschutz. EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 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 e

10、xtraction chromatography Part 1: Samples containing plutonium in the microgram 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 chromatogra

11、phique par solvant pour les mesures isotopiques et les analyses par dilution 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 Plut

12、onium in Salpetersure-Lsungen fr Isotopen- und Isotopenverdnnungsanalysen 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

13、 bound to comply with the CEN/CENELEC Internal Regulations which stipulate 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 t

14、he CEN-CENELEC Management Centre or to any CEN member. This European 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 Cen

15、tre has the same status as the official versions. CEN members are the 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, Lithuan

16、ia, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-10

17、00 Brussels 2016 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 15366-1:2016 E EN ISO 15366-1:2016 (E) 2 Contents Page DIN EN ISO 15366-1:2016-07 European foreword . 3 Foreword 4 1 Scope 5 2 Principle of the method 5 3 Apparat

18、us . 5 4 Reagents . 6 5 Procedure (see Figure 1) 6 6 Characteristics of the separation 8 7 Quality control . 9 8 Interferences 9 Annex 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-oct

19、yl-phosphine-oxide (TOPO) . 11 A.1 General . 11 A.2 Apparatus 11 A.3 Coating the silica gel support with TOPO 11 A.4 Packing the columns . 12 A.5 Conditioning the columns . 12 Bibliography . 14 EN ISO 15366-1:2016 (E) 3 European foreword The text of ISO 15366-1:2014 has been prepared by Technical Co

20、mmittee 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 “Nuclear energy, nuclear technologies, and radiological protection” the s

21、ecretariat 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 standards shall be withdrawn at the latest by October 2016. Attention i

22、s 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 Internal Regulations, the national standards organizations of the fo

23、llowing 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, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands

24、, 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 modification. DIN EN ISO 15366-1:2016-07 ForewordISO (the International Orga

25、nization 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 been establis

26、hed 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 standardization

27、.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 accordance with th

28、e 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 any patent righ

29、ts 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 an explanation

30、 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 this document is

31、 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 been technically revised.ISO 15366 consists of

32、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 microgram range and uranium in the milligram

33、 range Part 2: Sample containing plutonium and uranium amounts in the nanogram range and belowEN ISO 15366-1:2016 (E) 4DIN EN ISO 15366-1:2016-07 1 ScopeThis part of ISO 15366 describes procedures to chemically separate and purify uranium and plutonium in dissolved solutions of irradiated light wate

34、r 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 ISO 15366, describes a technique for the separation of uranium and plut

35、onium 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 applicable to mixtures of uranium and plutonium in which the U/Pu-ratio c

36、an 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 separation is done with iron(II) sulfate and sodium nitrite. The extraction

37、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 products and other interfering elements are not retained. Plutonium is elut

38、ed 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 the determination of the isotopic abundance of 238Pu (mass spectrometr

39、y 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 exceed 0,1 mlmin1.Parallel measurement of blank and/or control sample is

40、 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 analysed materials are also prepared and separated along with the sampl

41、e 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.EN ISO 15366-1:2016 (E) 5DIN EN ISO 15366-1:2016-07 3.2 Disposable polypropylene or glass columns, of length 90 mm

42、, funnel reservoir 9,5 ml, support bed volume 1,4 ml, height of bed 26 mm, inner diameter of bed reservoir 8,4 mm. Frits of polyethylene or glass 20 m respectively 70 m porosity (See Figure A.1). Suitable polypropylene columns with polyethylene frits are available commercially and well adapted to ro

43、botized operation. 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 Standard laboratory equipment (flasks and beakers, pipettes, glassware, stands and supports for columns,

44、 sample vials, fraction tubes, etc.).3.5 Glass vials.4 ReagentsUse only reagents of recognized analytical grade. All aqueous solutions shall be prepared with distilled or de-ionized water (resistivity 1 Mm to 10 Mm).4.1 Concentrated nitric acid and nitric acid solutions, c(HNO3) = 6 moll1and 3 moll1

45、.4.2 Formic acid solution, c(HCOOH) = 1 moll1.4.3 Ammonium carbamate CAS No. 1111-78-0 solution, c(NH4CO2NH2) = 0,7 moll1.4.4 Silica gel 100, 63 m to 200 m, prewashed with 3 moll1nitric acid solution (4.1) and distilled or de-ionized water (see A.3.1).4.5 L(+)-Ascorbic acid solution c(C6H8O6) = 105m

46、oll1or c(C6H8O6) = 103moll1in formic acid solution (4.2)4.6 Tri-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(FeS

47、O4) = 0,1 moll1or c(FeSO4) = 0,8 moll1in water. To be prepared 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.5 Procedure (see Figure 1)5.1 The sample should contain 1 g to 150 g plutonium

48、 and 0,1 mg to 2 mg uranium in a volume of 0,5 ml of 3 moll1nitric acid solution (4.1). Whenever starting with dried samples, apply the following dissolution procedure.a) Add 0,5 ml of 6 moll1nitric acid solution (4.1) to the dried samples and evaporate slowly on the hot plate, keeping the temperatu

49、re slightly below the boiling point to avoid any splashing and bubbling until nitrate salts crystallize.NOTE This procedure is an example. If equivalent results could be expected, other conditions than these described in Clause 5, can be applied for sample preparation.EN ISO 15366-1:2016 (E) 6DIN EN ISO 15366-1:2016-07 b) Remove the sample vessels from the hot plate and redissolve the salts by adding 0,5 ml of 3 moll1nitric acid solution (4.1), while still warm (40 C