ASTM_C_698_-_16.pdf

Designation:C69816Standard Test Methods forChemical,Mass Spectrometric,and SpectrochemicalAnalysis of Nuclear-Grade Mixed Oxides(U,Pu)O2)1This standard is issued under the fixed designation C698;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 These test methods cover procedures for the chemical,mass spectrometric,and spectrochemical analysis of nuclear-grade mixed oxides,(U,Pu)O2,powders and pellets to deter-mine compliance with specifications.1.2 The analytical procedures appear in the following order:SectionsUranium in the Presence of Pu by Potentiometric Titration2Plutonium by Controlled-Potential Coulometry2Plutonium by Amperometric Titration with Iron(II)2Nitrogen by Distillation Spectrophotometry Using NesslerReagent8 to 15Carbon(Total)by Direct Combustion-Thermal Conductivity16 to 26Total Chlorine and Fluorine by Pyrohydrolysis27 to 34Sulfur by Distillation-Spectrophotometry35 to 43Moisture by the Coulometric,Electrolytic Moisture Analyzer44 to 51Isotopic Composition by Mass Spectrometry3Rare Earths by Copper Spark Spectroscopy52 to 59Trace Impurities by Carrier Distillation Spectroscopy60 to 68Impurities by Spark-Source Mass Spectrography69 to 75Total Gas in Reactor-Grade Mixed Dioxide Pellets4Tungsten by Dithiol-Spectrophotometry76 to 84Rare Earth Elements by Spectroscopy85 to 88Plutonium-238 Isotopic Abundance by Alpha Spectrometry5Americium-241 in Plutonium by Gamma-Ray SpectrometryUranium and Plutonium Isotopic Analysis by MassSpectrometry89 to 97Oxygen-to-Metal Atom Ratio by Gravimetry98 to 1051.3 The values stated in SI units are to be regarded asstandard.The values given in parentheses are for informationonly.1.4 This standard does not purport to address all of thesafety concerns,if any,associated with its use.It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.(For specific safetyprecaution statements,see Sections 6,13.2.5,41.7,and 93.6.1.)2.Referenced Documents2.1 ASTM Standards:6C697 Test Methods for Chemical,Mass Spectrometric,andSpectrochemical Analysis of Nuclear-Grade PlutoniumDioxide Powders and PelletsC833 Specification for Sintered(Uranium-Plutonium)Diox-ide PelletsC852 Guide for Design Criteria for Plutonium GloveboxesC859 Terminology Relating to Nuclear MaterialsC1068 Guide for Qualification of Measurement Methods bya Laboratory Within the Nuclear IndustryC1108 Test Method for Plutonium by Controlled-PotentialCoulometryC1165 TestMethodforDeterminingPlutoniumbyControlled-Potential Coulometry in H2SO4at a PlatinumWorking ElectrodeC1168 Practice for Preparation and Dissolution of PlutoniumMaterials for AnalysisC1204 Test Method for Uranium in Presence of Plutoniumby Iron(II)Reduction in Phosphoric Acid Followed byChromium(VI)TitrationC1206 Test Method for Plutonium by Iron(II)/Chromium(VI)Amperometric Titration(Withdrawn 2015)7C1233 Practice for Determining Equivalent Boron Contentsof Nuclear MaterialsC1268 Test Method for Quantitative Determination of241Am in Plutonium by Gamma-Ray SpectrometryC1415 Test Method for238Pu Isotopic Abundance By AlphaSpectrometryC1432 Test Method for Determination of Impurities inPlutonium:Acid Dissolution,Ion Exchange MatrixSeparation,and Inductively Coupled Plasma-AtomicEmission Spectroscopic(ICP/AES)AnalysisC1625 Test Method for Uranium and Plutonium Concentra-tions and Isotopic Abundances by Thermal IonizationMass Spectrometry1These test methods are under the jurisdiction of ASTM Committee C26 onNuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 onMethods of Test.Current edition approved June 1,2016.Published July 2016.Originally approvedin 1972.Last previous edition approved in 2010 as C698 10.DOI:10.1520/C0698-16.2Discontinued as of November 15,1992.3Discontinued as of May 30,1980.4Discontinued as of June 2016.5Discontinued as of January 1,2004.6For 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.7The last approved version of this historical standard is referenced onwww.astm.org.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 C1637 Test Method for the Determination of Impurities inPlutonium Metal:Acid Digestion and Inductively CoupledPlasma-Mass Spectroscopy(ICP-MS)AnalysisC1672 Test Method for Determination of Uranium or Pluto-nium Isotopic Composition or Concentration by the TotalEvaporation Method Using a Thermal Ionization MassSpectrometerC1817 Test Method for The Determination of the Oxygen toMetal(O/M)R