1、Designation: C 758 04Standard Test Methods forChemical, Mass Spectrometric, Spectrochemical, Nuclear,and Radiochemical Analysis of Nuclear-Grade PlutoniumMetal1This standard is issued under the fixed designation C 758; the number immediately following the designation indicates the year oforiginal ad
2、option or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 These test methods cover procedures for the chemical,mass spectrometr
3、ic, spectrochemical, nuclear, and radiochemi-cal analysis of nuclear-grade plutonium metal to determinecompliance with specifications.1.2 The analytical procedures appear in the following order:SectionsDissolution Procedure2Plutonium by Controlled-Potential Coulometry3Plutonium by Amperometric Titra
4、tion with Iron (II)2Plutonium by Ceric Sulfate Titration Test Method3Plutonium by Diode Array Spectrophotometry3Uranium by Arsenazo I Spectrophotometric Test Method 8-10Thorium by Thorin Spectrophotometric Test Method 11-13Iron by 1,10-Phenanthroline Spectrophotometric Test Method 14-16Iron by 2,28-
5、Bipyridyl Spectrophotometric Test Method 17-23Impurities by ICP-AESChloride by the Thiocyanate Spectrophotometric Test Method 24-26Fluoride by Distillation-Spectrophotometric Test Method 2728Nitrogen by Distillation-Nessler Reagent Spectrophotometric TestMethod2930Carbon by the Direct Combustion-The
6、rmal Conductivity TestMethod31-33Sulfur by Distillation-Spectrophotometric Test Method 34-36Isotopic Composition by Mass Spectrometry 37and38Plutonium-238 Isotopic Abundance by Alpha SpectrometryAmericium-241 by Extraction and Gamma Counting 39-41Americium-241 by Gamma Counting3Gamma-Emitting Fissio
7、n Products, Uranium, and Thorium byGamma-Ray Spectroscopy42-49Rare Earths by Copper Spark Spectrochemical Test Method 50-52Tungsten, Niobium (Columbium), and Tantalum by Spectro-chemical Test Method53-55Sample Preparation for Spectrographic Analysis for Trace Impurities56-601.3 This standard does no
8、t 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. For specificsafeguard and safety hazard
9、s statements, see Section 6.2. Referenced Documents2.1 ASTM Standards:4C 697 Test Methods for Chemical, Mass Spectrometric, andSpectrochemical Analysis of Nuclear-Grade PlutoniumDioxide Powders and PelletsC 698 Test Methods for Chemical, Mass Spectrometric, andSpectrochemical Analysis of Nuclear-Gra
10、de Mixed Oxides(U, Pu)O2)C 759 Test Methods for Chemical, Mass Spectrometric,Spectrochemical, Nuclear, and Radiochemical Analysis ofNuclear-Grade Plutonium Nitrate SolutionsC 852 Guide for Design Criteria for Plutonium GloveboxesC 1009 Guide for Establishing a Quality Assurance Pro-gram for Analytic
11、al Chemistry Laboratories Within theNuclear IndustryC 1068 Guide for Qualification of Measurement Methodsby a Laboratory Within the Nuclear IndustryC 1108 Test Method for Plutonium by Controlled-PotentialCoulometryC 1128 Guide for Preparation of Working Reference Mate-rials for Use in the Analysis o
12、f Nuclear Fuel CycleMaterialsC 1156 Guide for Establishing Calibration for a Measure-ment Method Used to Analyze Nuclear Fuel Cycle Mate-rialsC 1165 Test Method for Determining Plutonium byControlled-Potential Coulometry in H2SO4at a PlatinumWorking ElectrodeC 1168 Practice for Preparation and Disso
13、lution of Pluto-nium Materials for AnalysisC 1206 Test Method for Plutonium by Iron (II)/Chromium1These test methods are under the jurisdiction of ASTM Committee C-26 onNuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 onMethods of Test.Current edition approved Jan. 1, 2004
14、. Published February 2004. Originallyapproved in 1973. Last previous edition approved in 1998 as C 758 98.2Discontinued as of February 10, 1998.3Discontinued as of November 15, 19924For referenced ASTM Standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.or
15、g. For Annual Book of ASTMStandardsvolume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.(VI) Amperometric TitrationC 1210 Guide for Establishing a Measure
16、ment SystemQuality Control Program for Analytical Chemistry Labo-ratories Within the Nuclear IndustryC 1235 Standard Test Method for Plutonium byTitanium(III)/Cerium(IV) TitrationC 1268 Test Method for Quantitative Determination ofAmericium 241 in Plutonium by Gamma-Ray Spectrom-etryC 1297 Guide for
17、 Qualification of Laboratory Analysts forthe Analysis of Nuclear Fuel Cycle MaterialsC 1307 Test Method for Plutonium Assay by Plutonium(III)Diode Array SpectrophotometryC 1415 Test Method for238Pu Isotopic Abundance by AlphaSpectrometryC 1432 Test Method for Determination of Impurities inPlutonium:
18、 Acid Dissolution, Ion-Exchange Matrix Sepa-ration, and Inductively Coupled Plasma-Atomic EmissionSpectroscopic (ICP/AES) AnalysisD 1193 Specification for Reagent Water33. Significance and Use3.1 These test methods are designed to show whether agiven material meets the purchasers specifications.3.1.
19、1 An assay is performed to determine whether thematerial has the specified plutonium content.3.1.2 Determination of the isotopic content of the plutoniumis made to establish whether the effective fissile content is incompliance with the purchasers specifications.3.1.3 Impurity content is verified by
20、 a variety of methods toensure that the maximum concentration limit of specifiedimpurities is not exceeded. Determination of impurities is alsorequired for calculation of the equivalent boron content (EBC).4. Committee C-26 Safeguards Statement54.1 The material (plutonium metal) to which these testm
21、ethods apply is subject to nuclear safeguards regulationsgoverning its possession and use. The following analyticalprocedures in these test methods have been designed astechnically acceptable for generating safeguards accountabilitymeasurement data: Plutonium by Controlled-Potential Cou-lometry; Plu
22、tonium by Ceric Sulfate Titration; Plutonium byAmperometric Titration with Iron(II); Plutonium by DiodeArray Spectrophotometry and Isotopic Composition by MassSpectrometry.4.2 When used in conjunction with appropriate CertifiedReference Materials (CRMs), these procedures can demon-strate traceabilit
23、y to the national measurement base. However,adherence to these procedures does not automatically guaran-tee regulatory acceptance of the resulting safeguards measure-ments. It remains the sole responsibility of the user of these testmethods to assure that their application to safeguards has theappro
24、val of the proper regulatory authorities.5. Reagents and Materials5.1 Purity of ReagentsReagent grade chemicals shall beused in all test methods. Unless otherwise indicated, it isintended that all reagents shall conform to the specifications ofthe Committee on Analytical Reagents of the American Che
25、mi-cal Society, where such specifications are available.6Othergrades may be used, provided it is first ascertained that thereagent is of sufficient high purity to permit its use withoutlessening the accuracy of the determination.5.2 Purity of WaterUnless otherwise indicated, referenceto water shall
26、be understood to mean reagent water conformingto Specification D 1193.6. Safety Hazards6.1 Since plutonium bearing materials are radioactive andtoxic, adequate laboratory facilities, gloved boxes, fume hoods,etc., along with safe techniques, must be used in handlingsamples containing these materials
27、. A detailed discussion of allthe precautions necessary is beyond the scope of these testmethods; however, personnel who handle these materialsshould be familiar with such safe handling practices as aregiven in Guide C 852 and in Refs. (1-3).77. Sampling7.1 In the absence of ASTM test methods for sa
28、mplingplutonium metal, alternative techniques are recommended(3-6).7.2 Cognizance shall be taken of the fact that variousimpurities can be introduced into samples during the process ofsampling. The particular impurities introduced are a functionof the method of sampling (for example, iron and alloyi
29、ngelements in drill turning, oxygen or components of cooling oil,or both, from lathe turnings, etc.). It is necessary for thepurchaser and the seller to recognize this possibility forcontamination during sampling and mutually agree on the mostsuitable method.7.3 Sample size shall be sufficient to pe
30、rform the following:7.3.1 Quality verification tests at the sellers plant,7.3.2 Acceptance tests at the purchasers plant, and7.3.3 Referee tests in the event these become necessary.7.4 All samples shall be identified clearly by the sellersbutton number and by the lot number, and all pieces of metali
31、n that lot shall be identified clearly by the lot number and thepiece number.7.4.1 A lot is defined as a single button, fraction of a button,or multiple castings from a single melt of plutonium metal.Buttons, fractions of buttons, or multiple castings are usuallysupplied in pieces of not less than 5
32、0 g. All pieces shall beidentified positively as coming from a particular button,fraction of a button, or casting.5Based upon Committee C-26 Safeguards Matrix (C 1009, C 1068, C 1128,C 1156, C 1210, C 1297).6“Reagent Chemicals, American Chemical Society Specifications,” Am. Chemi-cal Soc., Washingto
33、n, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see “Reagent Chemicals and Standards,” by JosephRosin, D. Van Nostrand Co., Inc., New York, NY, and the “United StatesPharmacopeia.”7The boldface numbers in parentheses refer to the list of references at th
34、e end ofthese test methods.C7580427.4.2 A lot shall normally not be less than 1800 g ofplutonium, except as necessary to meet some special require-ment. The maximum size of a lot will depend on equipmentsize of the producer and criticality considerations.DISSOLUTION PROCEDURE(This practice is replac
35、ed by Standard Practice C 1168).PLUTONIUM BY CONTROLLED-POTENTIALCOULOMETRY(This test method was discontinued in 1992 and replaced byTest Method C 1165)PLUTONIUM BY CONTROLLED-POTENTIALCOULOMETRY(With appropriate sample preparation, controlled-potentialcoulometric measurement as described in Test Me
36、thod C 1108may be used for plutonium determination.)PLUTONIUM BY AMPEROMETRIC TITRATIONWITH IRON(II)(This test method was discontinued in 1992 and replaced byTest Method C 1206)PLUTONIUM BY CERIC SULFATE TITRATION TESTMETHOD(This test method is replaced by Test Method C 1235.)TEST METHOD FOR PLUTONI
37、UM ASSAY BYPLUTONIUM(III) DIODE ARRAYSPECTROPHOTOMETRY(With appropriate sample preparation, the measurementdescribed in Test Method C 1307 may be used for plutoniumdetermination.)URANIUM BY ARSENAZO ISPECTROPHOTOMETRIC TEST METHOD8. Scope8.1 This test method covers the determination of uranium inthe
38、 range from 300 to 3000 g/g of plutonium.9. Summary of Test Method9.1 Plutonium metal dissolved in 6 N HCl is reduced toPu(III) with hydroxylamine hydrochloride. The uranium andplutonium are separated by anion exchange; then the uraniumis determined by measuring the absorbance of the U(VI)-Arsenazo
39、I complex in a 1-cm cell at a wavelength of 600 nmversus a reagent blank.10. Procedure10.1 Transfer an aliquot of sample solution, prepared inaccordance with Practice C 1168, that contains approximately70 mg of plutonium, to a 50-mL beaker and add 1 mL of nitricacid (sp gr 1.42) and heat to boiling.
40、 Proceed with thedetermination of uranium in accordance with the appropriatesections of Test Methods C 759.NOTE 1Since the sample starts as plutonium metal and is thendissolved in acid and diluted to volume and an aliquot of this solutiontaken for the uranium determination, the following equation fo
41、r calculat-ing the uranium concentration must be substituted for the equation givenin 28.1 of Test Methods C 759:R 5 Y 2 B!D/AW (1)where:R = micrograms U per gram Pu,A, B = constants in linear calibration equation,D = dilution factor = V/Ewhere:V = volume in which sample solution was di-luted, mL, a
42、ndE = volume of aliquot of V used for uraniumdetermination, mL,W = weight of test portion of Pu metal sample, g, andY = a b = corrected absorbance of sample,where:a = absorbance of sample solution, andb = average absorbance of duplicate calibrationblanks.THORIUM BY THORIN SPECTROPHOTOMETRICTEST METH
43、OD11. Scope11.1 This test method covers the determination of thoriumin the range from 10 to 150 g/g of plutonium in nuclear-gradeplutonium metal.12. Summary of Test Method12.1 To an acid solution of plutonium metal, lanthanum isadded as a carrier and is precipitated along with thorium asinsoluble fl
44、uoride, while the plutonium remains in solution andis decanted after centrifugation of the sample. The thorium andlanthanum fluoride precipitates are dissolved in perchloric acidand the absorbance of the thorium-Thorin complex is measuredat a wavelength of 545 nm versus a reference solution. Themola
45、r absorptivity of the colored complex is of 15 600 forthorium concentration in the range from 5 to 70 g Th/10 mLof solution.13. Procedure13.1 Transfer an aliquot of solution of plutonium metal,prepared in accordance with Sections 6 and 7 of these testmethods, that contains from 10 to 70 g of thorium
46、 and nogreater than 500 mg of plutonium, into a 20-mL beaker.13.2 Determine the thorium concentration in accordancewith the appropriate sections of Test Methods C 759.NOTE 2Since the starting sample is plutonium metal the followingequation for calculating the thorium concentration must be substitute
47、d forthe equation given in 49.3 of Test Methods C 759:Th, g/g of Pu 5 Y 2 B!D/AW (2)where:A, B = constants in the linear calibration equation,C758043W = sample weight, g,D = dilution factor = V/Ewhere:V = volume to which dissolved plutonium metalis diluted, mL, andE = volume of aliquot of V taken fo
48、r determina-tion, mL,Y = a b = corrected absorbance of sample solutionwhere:a = absorbance of sample solution, andb = average absorbance from the duplicate re-agent blanks (see section 47.2.1 of TestMethods C 759).IRON BY 1,10-PHENANTHROLINESPECTROPHOTOMETRIC TEST METHOD14. Scope14.1 This test metho
49、d covers the determination of micro-gram quantities of iron in nuclear-grade plutonium metal.15. Summary of Test Method15.1 Ferric iron is reduced to ferrous iron with hydroxy-lamine hydrochloride. Solutions of 1,10-phenanthroline andacetate buffer are added and the pH adjusted to 3.5 to 4.5. Theabsorbance of the red-orange complex (C12H8N2)3Fe+2isread at 508 nm against a sample blank containing all of thereagents except the 1,10-phenanthroline.16. Procedure16.1 Dissolve a sample of plutonium metal in HCl asdescribed in Test Method C 1206.16.2 Determine the i
