ASTM_C_1474_-_00_2011.pdf

Designation:C147400(Reapproved 2011)Standard Test Method forAnalysis of Isotopic Composition of Uranium in Nuclear-Grade Fuel Material by Quadrupole Inductively CoupledPlasma-Mass Spectrometry1This standard is issued under the fixed designation C1474;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 is applicable to the determination ofthe isotopic composition of uranium(U)in nuclear-grade fuelmaterial.The following isotopic weight percentages are deter-mined using a quadrupole inductively coupled plasma-massspectrometer(Q-ICP-MS):233U,234U,235U,236U,and238U.The analysis can be performed on various material matricesafter acid dissolution and sample dilution into water or dilutenitric(HNO3)acid.These materials include:fuel product,uranium oxide,uranium oxide alloys,uranyl nitrate(UNH)crystals,and solutions.The sample preparation discussed inthis test method focuses on fuel product material but may beused for uranium oxide or a uranium oxide alloy.Otherpreparation techniques may be used and some references aregiven.Purification of the uranium by anion-exchange extrac-tion is not required for this test method,as it is required byother test methods such as radiochemistry and thermal ioniza-tion mass spectroscopy(TIMS).This test method is alsodescribed in ASTM STP 13442.1.2 The233U isotope is primarily measured as a qualitativemeasure of its presence by comparing the233U peak intensityto a background point since it is not normally found present inmaterials.The example data presented in this test method donot contain any233U data.A233U enriched standard is given inSection 8,and it may be used as a quantitative spike additionto the other standard materials listed.1.3 A single standard calibration technique is used.Optimalaccuracy(or a low bias)is achieved through the use of a singlestandard that is closely matched to the enrichment of thesamples.The intensity or concentration is also adjusted towithin a certain tolerance range to provide good statisticalcounting precision for the low-abundance isotopes while main-taining a low bias for the high-abundance isotopes,resultingfrom high-intensity dead time effects.No blank subtraction orbackground correction is utilized.Depending upon the stan-dards chosen,enrichments between depleted and 97%can bequantified.The calibration and measurements are made bymeasuring the intensity ratios of each low-abundance isotopeto the intensity sum of233U,234U,235U,236U,and238U.Thehigh-abundance isotope is obtained by difference.1.4 The values stated in SI units are to be regarded as thestandard.The values given in parentheses are for informationonly.The instrument is calibrated and the samples measured inunits of isotopic weight percent(Wt%).For example,the235Uenrichment may be stated as Wt%235U or as g235U/100 g ofU.Statements regarding dilutions,particularly for ug/g con-centrations or lower,are given assuming a solution density of1.0 since the uranium concentration of a solution is notimportant when making isotopic ratio measurements other thanto maintain a reasonably consistent intensity within a tolerancerange.1.5 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.Specific precau-tionary statements are given in Section 9.2.Referenced Documents2.1 ASTM Standards:3C753 Specification for Nuclear-Grade,Sinterable UraniumDioxide PowderC776 Specification for Sintered Uranium Dioxide PelletsC778 Specification for SandC833 Specification for Sintered(Uranium-Plutonium)Diox-ide PelletsC859 Terminology Relating to Nuclear Materials1This 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 June 1,2011.Published June 2011.Originallyapproved in 2000.Last previous edition approved in 2006 as C1474 00(2006)1.DOI:10.1520/C1474-00R11.2Policke,T.A.,Bolin,R.N.,and Harris,T.L.,“Uranium Isotope Measurementsby Quqdrupole ICP-MS for Process Monitoring of Enrichment,”Symposium onApplications of Inductively Coupled Plasma-Mass Spectrometry to RadionuclideDeterminations:Second Volume,ASTM STP 1344,ASTM,1998,p.3.3For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 C1347 Practice for Preparation and Dissolution