ASTM_C_1637_-_13.pdf

Designation:C163713Standard Test Method forthe Determination of Impurities in Plutonium Metal:AcidDigestion and Inductively Coupled Plasma-MassSpectroscopy(ICP-MS)Analysis1This standard is issued under the fixed designation C1637;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year of last revision.A number in parentheses indicates the year of last reapproval.Asuperscript epsilon()indicates an editorial change since the last revision or reapproval.1.Scope1.1 This Test Method covers the determination of 58 traceelements in plutonium(Pu)metal.The Pu sample is dissolvedin acid,and the concentration of the trace impurities aredetermined by Inductively Coupled Plasma-Mass Spectros-copy(ICP-MS).1.2 This Test Method is specific for the determination oftrace impurities in Pu metal.It may be applied to other types ofPu materials,such as Pu oxides,if the samples are dissolvedand oxidized to the Pu(IV)state.However,it is the responsi-bility of the user to evaluate the performance of other matrices.1.3 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all of thesafety concerns associated with its use.It is the responsibilityof the user of this method to establish appropriate safety andhealth practices and to determine the applicability of regula-tory limitations prior to use of this standard.2.Referenced Documents2.1 ASTM Standards:2C757 Specification for Nuclear-Grade Plutonium DioxidePowder,SinterableC758 Test Methods for Chemical,Mass Spectrometric,Spectrochemical,Nuclear,and Radiochemical Analysis ofNuclear-Grade Plutonium MetalC759 Test Methods for Chemical,Mass Spectrometric,Spectrochemical,Nuclear,and Radiochemical Analysis ofNuclear-Grade Plutonium Nitrate SolutionsC1168 Practice for Preparation and Dissolution of PlutoniumMaterials for AnalysisC1432 Test Method for Determination of Impurities inPlutonium:Acid Dissolution,Ion Exchange MatrixSeparation,and Inductively Coupled Plasma-AtomicEmission Spectroscopic(ICP/AES)AnalysisD1193 Specification for Reagent Water3.Summary of Test Method3.1 A sample of Pu metal is dissolved in a small volume of6 M hydrochloric acid(HCl).Then,10 M nitric acid(HNO3)/0.03 M hydrofluoric acid(HF)is added to the dissolved Pu tooxidize the Pu to the Pu(IV)state.An aliquot of the originalsample is taken and diluted with 1%HNO3by volume to aprescribed volume.Aliquots from a second dilution of theoriginal sample are used to prepare run batch dilutions that areanalyzed for trace impurities by ICP-MS.34.Significance and Use4.1 This test method may be run together with Test MethodC1432 to analyze for trace impurities in Pu metal.Using thetechnique described in this test method and the techniquedescribed in Test Method C1432 will provide the analyst witha more thorough verification of the impurity concentrationscontained in the Pu metal sample.In addition,Test MethodC1432 can be used to determine impurity concentrations foranalytes such as Ca,Fe,Na,and Si,which have not beendetermined using this test method.4.2 This test method can be used on Pu matrices in nitratesolutions.4.3 This test method has been validated for use on materialsthat meet the specifications described in Specification C757and Test Methods C758 and C759.4.4 This test method has been validated for all elementslisted in Table 1.1This test method is under the jurisdiction ofASTM Committee C26 on NuclearFuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods ofTest.Current edition approved Jan.1,2013.Published January 2013.Originallyapproved in 2006.Last previous edition approve in 2006 as D1637 06.DOI:10.1520/C1637-13.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMStandards volume information,refer to the standards Document Summary page onthe ASTM website.3“Inductively Coupled Plasma Mass Spectrometry Using the VG ElementalPlasma Quad,”Actinide Analytical Chemistry Procedures,Los Alamos NationalLaboratory,ANC102 R.1.2,LA-UR-05-7605,2004.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.Interferences5.1 Ions from doubly charged(2+)species are formed in theICP-MS.The actinide related spectral interferences are fromactinide 2+and actinide-oxide 2+.The spectral interferencesare observed at 120.5 and 127.5 atomic mass unit(amu),whenanalyzing plutonium-239.5.2 Spectral interferences from the argon plasma and theacid used to transport the sample to the plasma.These spectralinterferences occur between 12 and 80 amu.5.3 Ions from plutonium cause a matrix related signalsuppression.Signal suppression increases as the Pu concentra-tion increases.In order to minimize signal suppression effectsfrom Pu,samples are diluted so that the concentration of Pu inthe analyzed aliquot is less