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TM_C_758_
_04_2010
Designation:C75804(Reapproved 2010)Standard Test Methods forChemical,Mass Spectrometric,Spectrochemical,Nuclear,and Radiochemical Analysis of Nuclear-Grade PlutoniumMetal1This standard is issued under the fixed designation C758;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,spectrochemical,nuclear,and radiochemi-cal analysis of nuclear-grade plutonium metal to determinecompliance with specifications.1.2 The analytical procedures appear in the following order:SectionsDissolution Procedure2Plutonium by Controlled-Potential Coulometry3Plutonium by Amperometric Titration with Iron(II)2Plutonium by Ceric Sulfate Titration Test Method3Plutonium by Diode Array Spectrophotometry3Uranium by Arsenazo I Spectrophotometric Test Method8 10Thorium by Thorin Spectrophotometric Test Method11 13Iron by 1,10-Phenanthroline Spectrophotometric Test Method14 16Iron by 2,2-Bipyridyl Spectrophotometric Test Method17 23Impurities by ICP-AESChloride by the Thiocyanate Spectrophotometric Test Method24 26Fluoride by Distillation-Spectrophotometric Test Method2728Nitrogen by Distillation-Nessler Reagent Spectrophotometric TestMethod2930Carbon by the Direct Combustion-Thermal Conductivity TestMethod31 33Sulfur by Distillation-Spectrophotometric Test Method34 36Isotopic Composition by Mass Spectrometry37 and38Plutonium-238 Isotopic Abundance by Alpha SpectrometryAmericium-241 by Extraction and Gamma Counting39 41Americium-241 by Gamma Counting3Gamma-Emitting Fission Products,Uranium,and Thorium byGamma-Ray Spectroscopy42 49Rare Earths by Copper Spark Spectrochemical Test Method50 52Tungsten,Niobium(Columbium),and Tantalum by Spectro-chemical Test Method53 55Sample Preparation for Spectrographic Analysis for Trace Impurities56 601.3 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,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 specificsafeguard and safety hazards statements,see Section 6.2.Referenced Documents2.1 ASTM Standards:4C697 Test Methods for Chemical,Mass Spectrometric,andSpectrochemical Analysis of Nuclear-Grade PlutoniumDioxide Powders and PelletsC698 Test Methods for Chemical,Mass Spectrometric,andSpectrochemical Analysis of Nuclear-Grade Mixed Ox-ides(U,Pu)O2)C759 Test Methods for Chemical,Mass Spectrometric,Spectrochemical,Nuclear,and Radiochemical Analysis ofNuclear-Grade Plutonium Nitrate SolutionsC852 Guide for Design Criteria for Plutonium GloveboxesC1009 Guide for Establishing and Maintaining a QualityAssurance Program forAnalytical Laboratories Within theNuclear IndustryC1068 Guide for Qualification of Measurement Methods bya Laboratory Within the Nuclear IndustryC1108 Test Method for Plutonium by Controlled-PotentialCoulometryC1128 Guide for Preparation of Working Reference Materi-als for Use in Analysis of Nuclear Fuel Cycle MaterialsC1156 Guide for Establishing Calibration for a Measure-ment Method Used to Analyze Nuclear Fuel Cycle Mate-rialsC1165 TestMethodforDeterminingPlutoniumbyControlled-Potential Coulometry in H2SO4at a PlatinumWorking ElectrodeC1168 Practice for Preparation and Dissolution of PlutoniumMaterials for 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 Jan.1,2010.Published February 2010.Originallyapproved in 1973.Last previous edition approved in 2004 as C758 04.DOI:10.1520/C0758-10.2Discontinued as of February 10,1998.3Discontinued as of November 15,19924For referenced ASTM Standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMStandardsvolume information,refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 C1206 Test Method for Plutonium by Iron(II)/Chromium(VI)Amperometric Titration(Withdrawn 2015)5C1210 Guide for Establishing a Measurement System Qual-ity Control Program for Analytical Chemistry Laborato-ries Within the Nuclear IndustryC1235 Test Method for Plutonium by Titanium(III)/Cerium(IV)Titration(Withdrawn 2005)5C1268 Test Method for Quantitative Determination of241Am in Plutonium by Gamma-Ray SpectrometryC1297 Guide for Qualification of Laboratory Analysts forthe Analysis of Nuclear Fuel Cycle MaterialsC1307 Test Method for Pluton