ASTM_C_1163_-_14.pdf

Designation:C116314Standard Practice forMounting Actinides for Alpha Spectrometry UsingNeodymium Fluoride1This standard is issued under the fixed designation C1163;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 covers the preparation of separated frac-tions of actinides for alpha spectrometry.It is applicable to anyof the actinides that can be dissolved in dilute hydrochloricacid.Examples of applicable samples would be the finalelution from an ion exchange separation or the final strip froma solvent extraction separation.21.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.3 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 a specifichazard statement,see Section 9.2.Referenced Documents2.1 ASTM Standards:3C859 Terminology Relating to Nuclear MaterialsC1284 Practice for Electrodeposition of the Actinides forAlpha SpectrometryD1193 Specification for Reagent WaterD3084 Practice for Alpha-Particle Spectrometry of Water3.Terminology3.1 For definitions of terms in this standard,refer toTerminology C859.4.Summary of Test Method4.1 Guidance is provided for the sample mounting ofseparated actinides using coprecipitation with neodymiumfluoride.The purified samples are prepared and mounted on amembrane filter to produce a deposit that yields alpha spectraof sufficient quality for most analytical methodologies.Samples can be prepared more rapidly using coprecipitationthan by electrodeposition and have comparable resolution.5.Significance and Use5.1 The determination of actinides by alpha spectrometry isan essential function of many environmental and other pro-grams.Alpha spectrometry allows the identification and quan-tification of most alpha-emitting actinides.Although numerousseparation methods are used,the final sample preparationtechnique has historically been by electrodeposition(PracticeC1284).However,electrodepositionmayhavesomedrawbacks,such as time required,incompatibility with priorchemistry,thick deposits,and low recoveries.These problemsmay be minimized by using the neodymium fluoride copre-cipitation method whose performance is well documented(1-6).4To a lesser extent cerium fluoride has been used(7)butis not addressed in this practice.5.2 The sample mounting technique described in this prac-tice is rapid,adds an additional purification step,since onlythose elements that form insoluble fluorides are mounted,andthe sample and filter media can be dissolved and remounted ifproblems occur.The recoveries are better and resolutionapproaches normal in electrodeposited samples.Recoveries aresufficiently high that for survey work,if quantitative recoveriesare not necessary,tracers can be omitted.Drawbacks to thistechnique include use of very hazardous hydrofluoric acid andthe possibility of a non-reproducible and ill-defined countinggeometry from filters that are not flat and may not be suitablefor long retention.Also,although the total turn around time forcoprecipitation may be less than for electrodeposition,copre-cipitation requires more time and attention from the analyst.6.Interferences6.1 Calculation of a result from a sample that gives poorresolution should not be attempted since it probably implies anerror in performing the separation or mounting procedure.1This practice is under the jurisdiction ofASTM Committee C26 on the NuclearFuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods ofTest.Current edition approved June 1,2014.Published July 2014.Originally approvedin 1992.Last previous edition approved in 2008 as C1163 08.DOI:10.1520/C1163-14.2Hindman,F.D.,“Actinide Separations for Spectrometry Using NeodymiumFluoride Coprecipitation,”Analytical Chemistry,58,1986,pp.12381241.3For 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.4The boldface numbers in parentheses refer to a list of references at the end ofthis standard.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 7.Apparatus7.1 Alpha SpectrometerA system should be assembledthat is capable of 60 to 70 keV resolution on an actual sampleprepared by this practice,have a counting efficiency of greaterthan 20%,and a background of less than 0.005 cpm over eachdesignated energy region.Resolution is defined as the full-width at half-ma