1、Designation:C141114Standard Practice forThe Ion Exchange Separation of Uranium and PlutoniumPrior to Isotopic Analysis1This standard is issued under the fixed designation C1411;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year
2、 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 is for the ion exchange separation ofuranium and plutonium from each other and from otherimpurities for s
3、ubsequent isotopic analysis by thermal ioniza-tion mass spectrometry.Plutonium238 and uranium238,andplutonium241 and americium241,will appear as the samemass peak and must be chemically separated prior to analysis.Only high purity solutions can be analyzed reliably usingthermal ionization mass spect
4、rometry.1.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.3 This standard may involve hazardous material,operations,and equipment.This standard does not purport toaddress all of the safety concerns,if any,associated with itsu
5、se.It is the responsibility of the user of this standard toconsult and establish appropriate safety and health practicesand determine the applicability of regulatory limitations priorto use.2.Referenced Documents2.1 ASTM Standards:2C698 Test Methods for Chemical,Mass Spectrometric,andSpectrochemical
6、 Analysis of Nuclear-Grade Mixed Ox-ides(U,Pu)O2)C833 Specification for Sintered(Uranium-Plutonium)Diox-ide PelletsC859 Terminology Relating to Nuclear MaterialsC1008 Specification for Sintered(Uranium-Plutonium)Di-oxide PelletsFast Reactor FuelC1168 Practice for Preparation and Dissolution of Pluto
7、niumMaterials for AnalysisC1347 Practice for Preparation and Dissolution of UraniumMaterials for AnalysisC1625 Test Method for Uranium and Plutonium Concentra-tions and Isotopic Abundances by Thermal IonizationMass SpectrometryD1193 Specification for Reagent Water3.Terminology3.1 Definitions:For def
8、initions of terms used in thisstandard,refer to C859.4.Summary of Practice4.1 Solid samples are dissolved according to PracticesC1168,C1347,or other appropriate methods.The resultingsolution is processed by this practice to prepare separatesolutions of plutonium and uranium for mass spectrometriciso
9、topic analysis using Method C698 or Method C1625.Appropriate aliquants are taken to provide up to 1 mg ofplutonium on the ion exchange column to be separated from 10mg or less of uranium.Valence adjustment is obtained by usingone of two procedures as described in 4.1.1 and 4.1.2 or by analternative
10、method demonstrated by the user to perform theequivalent reduction/oxidation procedure.34.1.1 For any sample type,especially those containing largeamounts of impurities,ferrous sulfate may be used for reduc-tion.The aliquant is dissolved in 3 M HNO3.Ferrous sulfate isadded to reduce all plutonium(VI
11、)to plutonium(III),then 16M HNO3is added to oxidize plutonium(III)to plutonium(IV),and to adjust the final acid concentration to 8 M HNO3.4.1.2 A hydrogen peroxide reduction may be used forrelatively pure samples which do not contain excessiveamounts of oxidizing impurities.The aliquant is dissolved
12、 in 8M HNO3.Hydrogen peroxide is added to the aliquant prior tofuming to reduce plutonium(VI)to the lower oxidation states.The solution is warmed on a hot plate to destroy excesshydrogen peroxide and stabilize plutonium(IV)in solution.4,51This practice is under the jurisdiction of ASTM Committee C26
13、 on NuclearFuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods ofTest.Current edition approved Jan.1,2014.Published February 2014.Originallyapproved in 1990.Last previous edition approved in 2008 as C1411 08.DOI:10.1520/C1411-14.2For referenced ASTM standards,visit the ASTM
14、 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.3Reduction of all higher plutonium oxidation states to plutonium(III)by theaddition of hydroxylamine or NH2CLO4
15、,followed by oxidation to plutonium(IV)by sodium nitrite and subsequent boiling to eliminate the nitrous fumes has beenfound to be acceptable.This method avoids the addition of Fe,which could interferewith electrodeposition of prior to mass spectrometry analysis samples.4I.V.Kressin and G.R.Waterbur
16、y,Anal.Chem.34(12),1598(1962).Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 4.2 After valence adjustment,the resulting solution ispassed through an anion exchange column in the nitrate formwhich retains the plutonium;uranium and americium are notabsorbed.The adsorbed plutonium is washed with additional 8M nitric acid(HNO3)to remove impurities and then strippedfrom the column with 0.36 M hydrochloric acid(HCl)and 0.01M hydrofluoric a
