EN ISO 21483-2017 en Determination of solubility in nitric acid of plutonium in unirradiated mixed oxide fuel pellets (U Pu) O2.pdf

1、BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06Determination of solubility in nitric acid of plutonium in unirradiated mixed oxide fuel pellets (U, Pu) O2 (ISO 21483:2013)BS EN ISO 21483:2017EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 21483 October 2017

2、 ICS 27.120.30 English Version Determination of solubility in nitric acid of plutonium in unirradiated mixed oxide fuel pellets (U, Pu) O2 (ISO 21483:2013) Dtermination de la solubilit dans Iacide nitrique du plutonium des pastilles (U, Pu) O2 de combustibles doxydes mixtes non irradis (ISO 21483:20

3、13) Bestimmung der Lslichkeit in Salpetersure von Plutonium in unbestrahlten (U, Pu) O2-Mischoxid-Pellets (ISO 21483:2013) This European Standard was approved by CEN on 13 September 2017. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giv

4、ing 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 Standard exists in three off

5、icial 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 national standards bodies o

6、f 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, Serbia, Slovakia, Slovenia

7、, 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-1000 Brussels 2017 CEN All rights of exploitation in any form and by any means reserved wor

8、ldwide for CEN national Members. Ref. No. EN ISO 21483:2017 ENational forewordThis British Standard is the UK implementation of EN ISO 21483:2017. It is identical to ISO 21483:2013. It supersedes BS ISO 21483:2013, which is withdrawn.The UK participation in its preparation was entrusted to Technical

9、 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 responsible for its correct application. The British St

10、andards Institution 2018 Published by BSI Standards Limited 2018ISBN 978 0 580 96936 2ICS 27.120.30Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 January 201

11、8.Amendments/corrigenda issued since publicationDate Text affected31 January 2018 This corrigendum renumbers BS ISO 21483:2013 as BS EN ISO 21483:2017BRITISH STANDARDBS EN ISO 21483:2017EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 21483 October 2017 ICS 27.120.30 English Version Determin

12、ation of solubility in nitric acid of plutonium in unirradiated mixed oxide fuel pellets (U, Pu) O2 (ISO 21483:2013) Dtermination de la solubilit dans Iacide nitrique du plutonium des pastilles (U, Pu) O2 de combustibles doxydes mixtes non irradis (ISO 21483:2013) Bestimmung der Lslichkeit in Salpet

13、ersure von Plutonium in unbestrahlten (U, Pu) O2-Mischoxid-Pellets (ISO 21483:2013) This European Standard was approved by CEN on 13 September 2017. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status o

14、f 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 (English, French, German

15、). 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, Bulgaria, Croatia,

16、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, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey an

17、d United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2017 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. N

18、o. EN ISO 21483:2017 EBS EN ISO 21483:2017EN ISO 21483:2017 (E) 3 European foreword The text of ISO 21483:2013 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 be

19、en taken over as EN ISO 21483:2017 by Technical Committee CEN/TC 430 “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 b

20、y endorsement, at the latest by April 2018, and conflicting national standards shall be withdrawn at the latest by April 2018. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN shall not be held responsible for identifying any o

21、r 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 Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic

22、 of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 21483:2013 has bee

23、n approved by CEN as EN ISO 21483:2017 without any modification. BS EN ISO 21483:2017ISO 21483:2013(E) ISO 2013 All rights reserved iiiContents PageForeword iv1 Scope . 12 Principle 13 Interferences 14 Reagents 14.1 Concentrated nitric acid 14.2 Nitric acid high 14.3 Nitric acid low 14.4 Concentrate

24、d hydrofluoric acid 14.5 Mixture of acid . 14.6 Sodium hydroxide 25 Apparatus . 25.1 Analytical balance. 25.2 Dissolution apparatus with total reflux condenser . 25.3 Dissolution apparatus without total reflux condenser 25.4 Second dissolution apparatus (polytetrafluoroethylene, PTFE, high density p

25、olyethylene, HDPE) 25.5 Filter apparatus 26 Sampling 27 Procedure. 37.1 Preparation of the sample . 37.2 Dissolution procedure 37.3 Treatment of the residue 37.4 Plutonium determination 37.5 Repeat solubility test . 38 Expression of results 48.1 Method of calculation 48.2 Total uncertainty of the Pu

26、 measurement . 49 Test report . 4Bibliography 5BS EN ISO 21483:2017ISO 21483:2013(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 throu

27、gh 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 liaison with ISO, also take part in the work. ISO collabora

28、tes 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 Directives, Part 1. In particular the different approval cr

29、iteria 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. www.iso.org/directivesAttention is drawn to the possibility that some of the elements of this document may be the subject of pat

30、ent 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 declarations received. www.iso.org/patentsAny trade name used in th

31、is document is information given for the convenience of users and does not constitute an endorsement.The 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 of ISO 21483 cance

32、ls and replaces ISO 12184:1994, which has been technically revised.iv ISO 2013 All rights reservedBS EN ISO 21483:2017INTERNATIONAL STANDARD ISO 21483:2013(E)Determination of solubility in nitric acid of plutonium in unirradiated mixed oxide fuel pellets (U, Pu) O21 ScopeThis International Standard

33、specifies an analytical method for determining the solubility in nitric acid of plutonium in pellets of unirradiated mixed oxide fuel (light-water reactor fuels). The results provide information about the expected dissolution behaviour of irradiated pellets under industrial reprocessing conditions.

34、In this aspect, the specific conditions (e.g. time of the test) may vary depending upon the need to match to a specific reprocessors requirements. The test is aimed at determining solubility under equilibrium conditions rather than the kinetics of dissolution and hence allows for a second dissolutio

35、n period.2 PrincipleA specified number of mixed oxide pellets of known plutonium content and mass are dissolved in a boiling nitric acid solution. The initial concentration of the nitric acid, the final content of U, Pu and the boiling time are carefully controlled. The undissolved residue is then d

36、issolved quantitatively by boiling in a mixture of nitric acid and hydrofluoric acid. The plutonium content of this residue is determined by an appropriate analytical method. The solubility is expressed by the ratio of the amount of plutonium dissolved in nitric acid to the amount of plutonium in th

37、e sample.3 InterferencesThe dissolution apparatus (Clause 5) and the reagents shall not be contaminated with fluoride, as fluoride can cause an increase in the solubility of the pellets in nitric acid.4 ReagentsUse only reagents of analytical grade and distilled or demineralised water or water of eq

38、uivalent purity. Prepare the reagents in compliance with the local laboratory safety instructions.4.1 Concentrated nitric acid = 1,40 g/ml or more4.2 Nitric acid highSolution c(HNO3) = 10 mol/l4.3 Nitric acid lowSolution c(HNO3) = 0,5 mol/l.4.4 Concentrated hydrofluoric acid = 1,13 g/ml4.5 Mixture o

39、f acidNitric acid, solution c(HNO3) = 14,4 mol/l and hydrofluoric acid, solution c(HF) = 0,05 mol/l. ISO 2013 All rights reserved 1BS EN ISO 21483:2017ISO 21483:2013(E)4.6 Sodium hydroxideSolution c(NaOH) = 2 mol/l (optional).5 ApparatusUsual laboratory apparatus and, in particular, the following.5.

40、1 Analytical balanceBalance with a 0,1 mg accuracy or better.5.2 Dissolution apparatus with total reflux condenserConsisting of dissolver flask (glass borosilicate or high density polyethylene HDPE are suitable), heater, total reflux condenser and gas inlet tube. The volume capacity of the flask sha

41、ll reflect the sample size selected in Clause 6.5.3 Dissolution apparatus without total reflux condenserConsisting of dissolver flask (glass borosilicate or high density polyethylene HDPE are suitable), heater, condenser and gas washer bottle. The volume capacity of the flask shall reflect the sampl

42、e size selected in Clause 6.5.4 Second dissolution apparatus (polytetrafluoroethylene, PTFE, high density polyeth-ylene, HDPE)For the dissolution with nitric acid/hydrofluoric acid mixture. This second dissolution is carried out with total reflux condenser (Clause 5).5.5 Filter apparatusApparatus co

43、nsisting of a vacuum funnel and a nitric-acid-resistant filter of a pore size less or equal to 1 micron (e.g. nitrocellulose or polycarbonate membrane filter 1 m).6 SamplingThe sample size shall be large enough to be representative of the lot, both whole and broken pellets are acceptable for this te

44、st. The minimum sample size could be chosen as a function of the pellet composition and the laboratorys detection limit. In any way, the minimum size must be equal or greater than 1 pellet.2 ISO 2013 All rights reservedBS EN ISO 21483:2017ISO 21483:2013(E)7 Procedure7.1 Preparation of the sampleWeig

45、h the pellets and transfer quantitatively into the dissolver flask (5.2 and 5.3). In order to reach a heavy metal concentration of around 1 mol/l, the total volume V, in litres, of nitric acid solution (4.2) to be used is given byVmcM= wherem is the sum of the mass of uranium and plutonium in the sa

46、mple in grams,M is the average atomic weights of the metals, in grams per mole;c is the concentration of the uranium and plutonium in the solution, in moles per litre (c = 1 mol/l). This value corresponds to the practice of the “reprocessing dissolution of spent fuel”.7.2 Dissolution procedureIntrod

47、uce the calculated volume of nitric acid solution (4.2) into the flask containing the sample pellets. Boil the contents of the flask under reflux for the specified period (examples are 10 h and 18 h). The time required for the solubility test is dependent upon the commercial contract and agreed with

48、 the commercial customer. Boiling shall begin within 30 min. Cooling to below around 50 C should be ended within 30 min. To avoid a delay in cooling, compressed air may be passed through the solution. The arising nitrous vapour may be trapped in a gas washer bottle filled with sodium hydroxide solut

49、ion (4.6)7.3 Treatment of the residueQuantitatively transfer the solution and the undissolved residue into the filter apparatus and filter the solution using the vacuum funnel. Thoroughly rinse the residue on the filter with nitric acid solution (4.3)If the filtered residue is seen to contain fragments of pellets, this may be indicative of a problem with the manufacture of MOX material. Repeat the test using a tared filter to weigh the residue (7.5).Place the filter and the residue in a dissolver flask (5.4) and add around 25 ml of