ASTM_C_1168_-_15.pdf

Designation:C116815Standard Practice forPreparation and Dissolution of Plutonium Materials forAnalysis1This standard is issued under the fixed designation C1168;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 practice is a compilation of dissolution techniquesfor plutonium materials that are applicable to the test methodsused for characterizing these materials.Dissolution treatmentsfor the major plutonium materials assayed for plutonium oranalyzed for other components are listed.Aliquots of thedissolved samples are dispensed on a weight basis when one ofthe analyses must be highly reliable,such as plutonium assay;otherwise they are dispensed on a volume basis.1.2 Procedures in this practice are intended for the dissolu-tion of plutonium metal,plutonium oxide,and uranium-plutonium mixed oxides.Aliquots of dissolved samples areanalyzed using test methods,such as those developed bySubcommittee C26.05 on Methods of Test,to demonstratecompliance with applicable requirements.These may includeproduct specifications such as Specifications C757 and C833.1.3 One or more of the procedures in this practice may beapplicable to unique plutonium materials,such as alloys,compounds,and scrap materials.The user must determine theapplicability of this practice to such materials.1.4 The treatments,in order of presentation,are as follows:Procedure NumberProcedure TitleSection1Dissolution of Plutonium Metal with Hydrochloric Acid at RoomTemperature92Dissolution of Plutonium Metal with Hydrochloric Acid and Heating103Dissolution of Plutonium Metal with Sulfuric Acid114Dissolution of Plutonium Oxide and Uranium-Plutonium MixedOxide by the Sealed-Reflux Technique125Dissolution of Plutonium Oxide and Uranium-Plutonium MixedOxides by Sodium Bisulfate Fusion136Dissolution of Uranium-Plutonium Mixed Oxides and Low-FiredPlutonium Oxide in Beakers147Open-Vessel(with Reflux Condenser)Dissolution of PlutoniumOxide Powder158Open-Vessel(with Reflux Condenser)Dissolution of Mixed OxidePowder169Closed-Vessel Hot Block Dissolution of Plutonium Oxide Powder1710Open-Vessel(with Reflux Condenser)Dissolution of Mixed OxidePellets181This practice is under the jurisdiction of ASTM Committee C26 on NuclearFuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods ofTest.Current edition approved Sept.1,2015.Published October 2015.Originallyapproved in 1990.Last previous edition approved in 2008 as C1168 08.DOI:10.1520/C1168-15.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 1.5 The values stated in SI units are to be regarded asstandard.Values in parentheses(non-SI units),where provided,are for information only and are not considered standard.1.6 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.2.Referenced Documents2.1 ASTM Standards:2C757 Specification for Nuclear-Grade Plutonium DioxidePowder,SinterableC833 Specification for Sintered(Uranium-Plutonium)Diox-ide PelletsC859 Terminology Relating to Nuclear MaterialsC1145 Terminology of Advanced CeramicsC1210 Guide for Establishing a Measurement System Qual-ity Control Program for Analytical Chemistry Laborato-ries Within the Nuclear IndustryD1193 Specification for Reagent WaterD7439 Test Method for Determination of Elements in Air-borne Particulate Matter by Inductively Coupled Plasma-Mass SpectrometryE1154 Specification for Piston or Plunger Operated Volu-metric Apparatus2.2 ISO Standards:3ISO 8655 Piston-Operated Volumetric Instruments(6 parts)3.Terminology3.1 DefinitionsExcept as otherwise defined herein,defini-tions of terms are as given in Terminology C859.3.2 Definitions of Terms Specific to This Standard:3.2.1 calcination,n(calcine,v)firing or heating of agranular or particulate solid at less than fusion temperature,butsufficient to remove most of its chemically combined volatilematter and otherwise to develop the desired properties for use.C11453.2.2 reagent blank,nsolution containing all reagentsused in sample preparation,in the same quantities used forpreparation of blank and sample solutions.D74394.Summary of Dissolution Procedures4.1 Most plutonium-containing samples are dissolved withvarious mineral acids and,except for plutonium metal,withapplied heat.In some cases,dissolution-resistant materials aredissolved in heated and sealed containers in which pressuriza-tion provides a higher temperature than is attained at ambientpressure.4.2 The dissolved materials are quantitatively transferred toa tared polyethylene dispensing bottle