1、Designation:C143215Standard Test Method forDetermination of Impurities in Plutonium:Acid Dissolution,Ion Exchange Matrix Separation,and Inductively CoupledPlasma-Atomic Emission Spectroscopic(ICP/AES)Analysis1This standard is issued under the fixed designation C1432;the number immediately following
2、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 covers the d
3、etermination of 25 ele-ments in plutonium(Pu)materials.The Pu is dissolved in acid,the Pu matrix is separated from the target impurities by an ionexchange separation,and the concentrations of the impuritiesare determined by inductively coupled plasma-atomic emissionspectroscopy(ICP-AES).1.2 This tes
4、t method is specific for the determination ofimpurities in 8 M HNO3solutions.Impurities in other pluto-nium materials,including plutonium oxide samples,may bedetermined if they are appropriately dissolved(see PracticeC1168)and converted to 8 M HNO3solutions.1.3 The values stated in SI units are to b
5、e regarded asstandard.The values given in parentheses are mathematicalconversions that are provided for information only and are notconsidered standard.1.4 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 s
6、tandard 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,SinterableC758 Test Methods for Chemical,Mass Spectrometric,Spe
7、ctrochemical,Nuclear,and Radiochemical Analysis ofNuclear-Grade Plutonium MetalC759 Test Methods for Chemical,Mass Spectrometric,Spectrochemical,Nuclear,and Radiochemical Analysis ofNuclear-Grade Plutonium Nitrate SolutionsC859 Terminology Relating to Nuclear MaterialsC1168 Practice for Preparation
8、and Dissolution of PlutoniumMaterials for AnalysisD1193 Specification for Reagent Water3.Terminology3.1 Except as otherwise defined herein,definitions of termsare as given in Terminology C859.4.Summary of Test Method4.1 A sample of plutonium metal is dissolved in a smallvolume of 6 M hydrochloric ac
9、id(HCl).Then,10 M(HNO3)/0.03 M hydrofluoric acid(HF)is added to the dissolvedplutonium to oxidize the plutonium to the Pu(IV)state.Thesample solution is loaded onto a nitrate anion exchange resinand eluted with 8 M HNO3/0.006 M HF.The rinses contain thetarget metallic impurities and less than 15 g/m
10、L Pu.Theplutonium is stripped from the anion exchange resin with 0.1M HCl.The rinses containing the metallic impurities areanalyzed by ICP-AES.5.Significance and Use5.1 This test method can be used on plutonium matrices innitrate solutions.5.2 This test method has been validated for all elementslist
11、ed in Test Methods C757 except sulfur(S)and tantalum(Ta).5.3 This test method has been validated for all of the cationelements measured in Table 1.Phosphorus(P)requires avacuum or an inert gas purged optical path instrument.6.Interferences6.1 Plutonium concentrations of less than 50 g/mL in thefinal
12、 aqueous phase do not significantly affect the analyticalresults for most elements.Interference studies should be madeto determine the degree of Pu and other elemental interferenceson the target analytes;background and interelement correctionsmay be required.1This test method is under the jurisdicti
13、on ofASTM Committee C26 on NuclearFuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods ofTest.Current edition approved June 1,2015.Published July 2015.Originally approvedin 1999.Last previous edition approved in 2008 as C1432 03(2008).DOI:10.1520/C1432-15.2For referenced AST
14、M 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 1
15、9428-2959.United States1 7.Apparatus7.1 An ICP-AES equipped with a Charge Injection Device(CID)detector or an ICP-AES with a spectral bandpass of 0.05nm or less is required to provide the necessary spectralresolution.The spectrometer may be either a simultaneousmultielement or a sequential spectrome
16、ter.The spectrometermay be either an inert gas-path or vacuum instrument;theappropriate spectral lines should be selected for each specificinstrument.Either an analog or digital readout system may beused.7.2 The ICP-AES is interfaced to an enclosure.The torchbox is contained with an enclosure,since plutonium containingmaterials may come in direct contact with the torch despite thesubstantial removal by ion exchange in 10.3.A possible setupis described in ASTM STP 951.37.3 Vacuum manifold set at
