ASTM_C_697_-_16.pdf

Designation:C69716Standard Test Methods forChemical,Mass Spectrometric,and SpectrochemicalAnalysis of Nuclear-Grade Plutonium Dioxide Powders andPellets1This standard is issued under the fixed designation C697;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 plutonium dioxide powders and pellets to determinecompliance with specifications.1.2 The analytical procedures appear in the following order:SectionsPlutonium Sample Handling8 to 10Plutonium by Controlled-Potential Coulometry2Plutonium by Ceric Sulfate Titration3Plutonium by Amperometric Titration with Iron(II)2Plutonium by Diode Array Spectrophotometry3Nitrogen by Distillation Spectrophotometry Using NesslerReagent11 to 18Carbon(Total)by Direct CombustionThermal Conductivity19 to 29Total Chlorine and Fluorine by Pyrohydrolysis30 to 37Sulfur by Distillation Spectrophotometry38 to 46Plutonium Isotopic Analysis by Mass Spectrometry4Rare Earth Elements by Spectroscopy47 to 54Trace Elements by CarrierDistillation Spectroscopy55 to 62(Alternative:Impurities by ICP-AES or ICP-MS)Impurity Elements by Spark-Source Mass Spectrography63 to 69Moisture by the Coulometric Electrolytic Moisture Analyzer70 to 77Total Gas in Reactor-Grade Plutonium Dioxide Pellets5Plutonium-238 Isotopic Abundance by Alpha Spectrometry3Americium-241 in Plutonium by Gamma-Ray Spectrometry2Rare Earths By Copper Spark-Spectroscopy78 to 87Plutonium Isotopic Analysis by Mass Spectrometry88 to 96Oxygen-To-Metal Atom Ratio by Gravimetry97 to 1041.3 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 specificprecautionary statements,see Sections 6,16.2.5,44.7,51.9 and92.5.1.2.Referenced Documents2.1 ASTM Standards:6C757 Specification for Nuclear-Grade Plutonium DioxidePowder for Light Water ReactorsC852 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 AnalysisC1206 Test Method for Plutonium by Iron(II)/Chromium(VI)Amperometric Titration(Withdrawn 2015)7C1233 Practice for Determining Equivalent Boron Contentsof Nuclear MaterialsC1235 Test Method for Plutonium by Titanium(III)/Cerium(IV)Titration(Withdrawn 2005)7C1268 Test Method for Quantitative Determination of241Am in Plutonium by Gamma-Ray SpectrometryC1307 Test Method for Plutonium Assay by Plutonium(III)Diode Array SpectrophotometryC1415 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)Analysis1These 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 C697 10.DOI:10.1520/C0697-16.2Discontinued as of November 15,1992.3Discontinued as of January 1,2004.4Discontinued as of May 30,1980.5Discontinued as of June 2016.6For 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 C1625 Test Method for Uranium and Plutonium Concentra-tions and Isotopic Abundances by Thermal IonizationMass SpectrometryC1637 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 MassSpectrometerD1193 Specification for Reagent WaterD4327 Test Method for Anions in W