ASTM_C_1517_-_16.pdf

Designation:C151716Standard Test Method forDetermination of Metallic Impurities in Uranium Metal orCompounds by DC-Arc Emission Spectroscopy1This standard is issued under the fixed designation C1517;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 test method describes the steps necessary for thepreparation and determination of impurity metals in uraniummetal and uranium compounds by DC arc emission spectros-copy.1.2 The method is valid for those materials that can bedissolved in acid or converted to an oxide in a muffle furnace,or both(see Practice C1347).1.3 This method uses the carrier distillation technique toselectively carry the impurities into the arc,leaving theuranium oxide in the electrode.If it is necessary to determinethe carrier metal(usually a silver or strontium,or galliumcompound)as an impurity,another technique must be chosenfor that element.1.4 UnitsThe values stated in SI units are to be regardedas standard.The values given in parentheses are for informa-tion only.1.5 This standard may involve hazardous materials,opera-tions and equipment.This standard does not purport to addressall of the safety concerns,if any,associated with its use.It isthe responsibility of the user of this standard to establishappropriate safety and health practices and determine theapplicability of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:2C753 Specification for Nuclear-Grade,Sinterable UraniumDioxide PowderC761 Test Methods for Chemical,Mass Spectrometric,Spectrochemical,Nuclear,and Radiochemical Analysis ofUranium HexafluorideC776 Specification for Sintered Uranium Dioxide PelletsC788 Specification for Nuclear-Grade Uranyl Nitrate Solu-tion or CrystalsC859 Terminology Relating to Nuclear MaterialsC967 Specification for Uranium Ore ConcentrateC1347 Practice for Preparation and Dissolution of UraniumMaterials for AnalysisE130 Practice for Designation of Shapes and Sizes ofGraphite Electrodes(Withdrawn 2013)3E135 Terminology Relating to Analytical Chemistry forMetals,Ores,and Related Materials3.Terminology3.1 Except as otherwise defined herein,definitions of termsare as given in Terminologies C859 and E135.4.Summary of Test Method4.1 Uranium metal,solutions and compounds are convertedto uranium oxide(U3O8)in a muffle furnace.A weighedamount of the oxide is mixed with an appropriate spectro-graphic carrier and loaded into a graphite electrode.Theelectrode is excited in a DC arc and the light is dispersed by aspectrograph or spectrometer.The resulting spectrum is mea-sured electronically using a CCD,CID,or CMOS camerasensitive to the proper regions.The line intensities are com-pared directly to calibration curves derived from the arcedstandards.5.Significance and Use5.1 This test method is applicable to uranium metal,ura-nium oxides and compounds soluble in nitric or sulfuric acid,and uranium solutions which can be converted to uraniumoxide(U3O8)in a muffle furnace.It may be used to determinethe impurities in uranium compounds as listed in SpecificationsC753,C776,C788,and C967.6.Apparatus6.1 Spectrograph or SpectrometerA spectrograph withsufficient resolving power and linear dispersion to separate the1This test method is under the jurisdiction ofASTM Committee C26 on NuclearFuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods ofTest.Current edition approved April 1,2016.Published May 2016.Originallyapproved in 2002.Last previous edition approved in 2009 as C1517 09.DOI:10.1520/C1517-16.2For 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.3The 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 analytical lines from other lines in the spectrum of the samplein the spectral region of 230 to 855 nm is required.Somespectrographs may be able to access wavelengths lower than230 nm that may allow the determination of other analytes.Instruments with a reciprocal linear dispersion in the first orderof 0.5 nm/mm or less are satisfactory.The spectrometer shouldinclude a CCD,CID,or CMOS camera for electronic measure-ment of the resulting spectrum.6.2 Excitation SourceUse an arc power source capable ofproviding a dc arc of up to 14-A dc,depending on the carrierused and electrode design.6.3 Excitation StandConventional type with adjustablewater-cooled electrode holders(may be fitted with automaticsample changers if desired).6.4 Mixer,for dry materials.6.5 Platinum Crucible.6.6 Venting Tool,(see Fig.8,Test