1、Designation:C128710Standard Test Method forDetermination of Impurities in Nuclear Grade UraniumCompounds by Inductively Coupled Plasma MassSpectrometry1This standard is issued under the fixed designation C1287;the number immediately following the designation indicates the year oforiginal adoption or
2、,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 covers the determination of 67 ele-ments in uranium dioxide samples a
3、nd nuclear grade uraniumcompounds and solutions without matrix separation by induc-tively coupled plasma mass spectrometry(ICP-MS).Theelements are listed in Table 1.These elements can also bedetermined in uranyl nitrate hexahydrate(UNH),uraniumhexafluoride(UF6),triuranium octoxide(U3O8)and uraniumtr
4、ioxide(UO3)if these compounds are treated and converted tothe same uranium concentration solution.1.2 The elements boron,sodium,silicon,phosphorus,potassium,calcium and iron can be determined using differenttechniques.The analysts instrumentation will determinewhich procedure is chosen for the analy
5、sis.1.3 The test method for technetium-99 is given in AnnexA1.1.4 The values stated in SI units are to be regarded asstandard.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
6、-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.WarningTheICP-MS is a source of intense ultra-violet radiation from theradio frequency induced plasma.Protection from radio fre-quency radiation and UV radiation is provided by the instru-ment
7、 under normal operation.2.Referenced Documents2.1 ASTM Standards:2C753 Specification for Nuclear-Grade,Sinterable UraniumDioxide PowderC776 Specification for Sintered Uranium Dioxide PelletsC787 Specification for Uranium Hexafluoride for Enrich-mentC788 Specification for Nuclear-Grade Uranyl Nitrate
8、 Solu-tion or CrystalsC967 Specification for Uranium Ore ConcentrateC996 Specification for Uranium Hexafluoride Enriched toLess Than 5%235UC1346 Practice for Dissolution of UF6from P-10 Tubes,C1347 Practice for Preparation and Dissolution of UraniumMaterials for AnalysisD1193 Specification for Reage
9、nt Water3.Summary of Test Method3.1 The sample is dissolved in acid if it is not already asolution.A fixed quantity of internal standard is added tomonitor and correct for signal instability.The level of impuri-ties in the solution is measured by ICP-MS.Customizedsoftware calculates the concentratio
10、n of each element.3.2 Uranium-concentration-matched standard solutions areused to calibrate the ICP-MS instrument.The calibration islinear up to at least 0.2 g/ml(100 g/g U)for each analyte.3,43.3 Microwave dissolution may be used as an alternatedissolution method.4.Significance and Use4.1 This test
11、 method is capable of measuring the elementslisted in Table 1,some of which are required by SpecificationsC753,C776,C787,C788,C967 and C996.1This test method is under the jurisdiction ofASTM Committee C26 on NuclearFuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods ofTest.
12、Current edition approved June 1,2010.Published July 2010.Originally approvedin 1994.Last previous edition approved in 2003 as C1287 03.DOI:10.1520/C1287-10.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMSta
13、ndards volume information,refer to the standards Document Summary page onthe ASTM website.3“ICP-MS Versus Conventional Methods for the Analysis of Trace Impurities inNuclear Fuel,”by Allenby,P.,Clarkson,A.S.,Makinson,P.R.,presented at 2ndSurrey Conference on Plasma Source Mass Spectrometry,Guildford
14、,UK,July1987.4“Trace Metals in NBL Uranium Standard CRM 124 Using ICP-MS,”byAldridge,A.J.,Clarkson,A.S.,Makinson,P.R.,Dawson,K.W.,presented at 1stDurham International Conference on Plasma Source Mass Spectrometry,Durham,UK,September 1988.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700
15、,West Conshohocken,PA 19428-2959.United States1 5.Apparatus5.1 ICP-MS,controlled by computer and fitted with theassociated software and peripherals.May be fitted with coldplasma option.Current instrumentation is available with dy-namic reaction cell or collision cell options.5.2 Autosampler,with tub
16、e racks and disposable plasticsample tubes compatible with 5.1(optional).5.3 Variable Micropipettes:5.3.1 10 L to 100 L capacity.5.3.2 100 L to 1000 L capacity.5.3.3 1000 L to 10.00 mL capacity.5.4 Volumetric Flasks:5.4.1 50 mL capacitypolypropylene.5.4.2 100 mL capacitypolypropylene.5.4.3 1 L capacityglass.5.5 Platinum Dish100 mL capacity.5.6 Silica Beaker250 mL capacity.5.7 Watch Glasses75 mm diameter.5.8 Polypropylene Tubes50 mL,with graduation marksand with caps.6.Reagents6.1 The sensitivity
