1、Designation: C758 04 (Reapproved 2010)C758 18Standard Test Methods forChemical, Mass Spectrometric, Spectrochemical, Nuclear,and Radiochemical Analysis of Nuclear-Grade PlutoniumMetal1This standard is issued under the fixed designation C758; the number immediately following the designation indicates
2、 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 These test methods cover procedures for the che
3、mical, mass spectrometric, spectrochemical, nuclear, and radiochemicalanalysis of nuclear-grade plutonium metal to determine compliance with specifications.1.2 The analytical procedures appear in the following order:SectionsDissolution Procedure 2Plutonium by Controlled-Potential Coulometry 3Plutoni
4、um by Amperometric Titration with Iron (II) 2Plutonium by Ceric Sulfate Titration Test Method 3Plutonium by Diode Array Spectrophotometry 3Uranium by Arsenazo I Spectrophotometric Test Method 8 10Thorium by Thorin Spectrophotometric Test Method 11 13Iron by 1,10-Phenanthroline Spectrophotometric Tes
5、t Method 14 16Iron by 2,2-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
6、 the Direct Combustion-Thermal Conductivity TestMethod31 33Sulfur by Distillation-Spectrophotometric Test Method 34 36Isotopic Composition by Mass Spectrometry 37 and38Plutonium-238 Isotopic Abundance by Alpha SpectrometryAmericium-241 by Extraction and Gamma Counting 39 41Americium-241 by Gamma Cou
7、nting 3Gamma-Emitting Fission 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
8、 60Sample Preparation for Spectrographic Analysis for Trace Impuri-ties56 601.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.4 This standard does not purport to address all of the safety concerns, if any, associated with
9、its use. It is the responsibilityof the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine theapplicability of regulatory limitations prior to use. For specific safeguard and safety hazards statements, see Section 6.1.5 This internat
10、ional standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committ
11、ee.1 These test methods are under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 on Methodsof Test.Current edition approved Jan. 1, 2010Sept. 1, 2018. Published February 2010October 2018. Originally approved in 1973. Last previou
12、s edition approved in 20042010 asC758 04.C758 04 (2010). DOI: 10.1520/C0758-10.10.1520/C0758-18.2 Discontinued as of February 10, 1998.3 Discontinued as of November 15, 1992This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what change
13、s have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the officia
14、l document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States12. Referenced Documents2.1 ASTM Standards:4C697 Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Plutonium DioxidePowders and Pelle
15、tsC698 Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Mixed Oxides (U,Pu)O2)C759 Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Nuclear-Grade Plutonium Nitrate SolutionsC852C852/C852M Guide for Desi
16、gn Criteria for Plutonium GloveboxesC859 Terminology Relating to Nuclear MaterialsC1009 Guide for Establishing and Maintaining a Quality Assurance Program for Analytical Laboratories Within the NuclearIndustryC1068 Guide for Qualification of Measurement Methods by a Laboratory Within the Nuclear Ind
17、ustryC1108 Test Method for Plutonium by Controlled-Potential CoulometryC1128 Guide for Preparation of Working Reference Materials for Use in Analysis of Nuclear Fuel Cycle MaterialsC1156 Guide for Establishing Calibration for a Measurement Method Used to Analyze Nuclear Fuel Cycle MaterialsC1165 Tes
18、t Method for Determining Plutonium by Controlled-Potential Coulometry in H2SO4 at a Platinum Working ElectrodeC1168 Practice for Preparation and Dissolution of Plutonium Materials for AnalysisC1206 Test Method for Plutonium by Iron (II)/Chromium (VI) Amperometric Titration (Withdrawn 2015)5C1210 Gui
19、de for Establishing a Measurement System Quality Control Program for Analytical Chemistry Laboratories Withinthe Nuclear IndustryC1235 Test Method for Plutonium by Titanium(III)/Cerium(IV) Titration (Withdrawn 2005)5C1268 Test Method for Quantitative Determination of 241Am in Plutonium by Gamma-Ray
20、SpectrometryC1297 Guide for Qualification of Laboratory Analysts for the Analysis of Nuclear Fuel Cycle MaterialsC1307 Test Method for Plutonium Assay by Plutonium (III) Diode Array SpectrophotometryC1415 Test Method for238Pu Isotopic Abundance By Alpha SpectrometryC1432 Test Method for Determinatio
21、n of Impurities in Plutonium: Acid Dissolution, Ion Exchange Matrix Separation, andInductively Coupled Plasma-Atomic Emission Spectroscopic (ICP/AES) AnalysisD1193 Specification for Reagent Water3. Terminology3.1 For definitions of terms used in this test method but not defined herein, refer to Term
22、inology C859.4. Significance and Use4.1 These test methods are designed to show whether a given material meets the purchasers specifications.4.1.1 An assay is performed to determine whether the material has the specified plutonium content.4.1.2 Determination of the isotopic content of the plutonium
23、is made to establish whether the effective fissile content is incompliance with the purchasers specifications.4.1.3 Impurity content is verified by a variety of methods to ensure that the maximum concentration limit of specified impuritiesis not exceeded. Determination of impurities is also required
24、 for calculation of the equivalent boron content (EBC).4.2 Fitness for Purpose of Safeguards and Nuclear Safety ApplicationsMethods intended for use in safeguards and nuclearsafety applications shall meet the requirements specified by Guide C1068 for use in such applications.4. Committee C-26 Safegu
25、ards Statement64.1 The material (plutonium metal) to which these test methods apply is subject to nuclear safeguards regulations governing itspossession and use. The following analytical procedures in these test methods have been designed as technically acceptable forgenerating safeguards accountabi
26、lity measurement data: Plutonium by Controlled-Potential Coulometry; Plutonium by CericSulfate Titration; Plutonium by Amperometric Titration with Iron(II); Plutonium by Diode Array Spectrophotometry and IsotopicComposition by Mass Spectrometry.4.2 When used in conjunction with appropriate Certified
27、 Reference Materials (CRMs), these procedures can demonstratetraceability to the national measurement base. However, adherence to these procedures does not automatically guarantee regulatoryacceptance of the resulting safeguards measurements. It remains the sole responsibility of the user of these t
28、est methods to assurethat their application to safeguards has the approval of the proper regulatory authorities.4 For referenced ASTM Standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandardsvolume information, refer to the
29、 standards Document Summary page on the ASTM website.5 The last approved version of this historical standard is referenced on www.astm.org.C758 1825. Reagents and Materials5.1 Purity of ReagentsReagent grade chemicals shall be used in all test methods. Unless otherwise indicated, it is intendedthat
30、all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society,where such specifications are available.6 Other grades may be used, provided it is first ascertained that the reagent is of sufficienthigh purity to permit its use without lessen
31、ing the accuracy of the determination.5.2 Purity of WaterUnless otherwise indicated, reference to water shall be understood to mean reagent water conforming toSpecification D1193.6. Safety Hazards6.1 Since plutonium bearing materials are radioactive and toxic, adequate laboratory facilities, gloved
32、boxes, fume hoods, etc.,along with safe techniques, must be used in handling samples containing these materials. A detailed discussion of all theprecautions necessary is beyond the scope of these test methods; however, personnel who handle these materials should be familiarwith such safe handling pr
33、actices as are given in Guide C852C852/C852M and in Refs. (1-3).77. Sampling7.1 In the absence of ASTM test methods for sampling plutonium metal, alternative techniques are recommended (3-6).7.2 Cognizance shall be taken of the fact that various impurities can be introduced into samples during the p
34、rocess of sampling.The particular impurities introduced are a function of the method of sampling (for example, iron and alloying elements in drillturning, oxygen or components of cooling oil, or both, from lathe turnings, etc.). It is necessary for the purchaser and the sellerto recognize this possi
35、bility for contamination during sampling and mutually agree on the most suitable method.7.3 Sample size shall be sufficient to perform 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
36、necessary.7.4 All samples shall be identified clearly by the sellers button number and by the lot number, and all pieces of metal in thatlot shall be identified clearly by the lot number and the piece number.7.4.1 Alot is defined as a single button, fraction of a button, or multiple castings from a
37、single melt of plutonium metal. Buttons,fractions of buttons, or multiple castings are usually supplied in pieces of not less than 50 g.All pieces shall be identified positivelyas coming from a particular button, fraction of a button, or casting.7.4.2 A lot shall normally not be less than 1800 g of
38、plutonium, except as necessary to meet some special requirement. Themaximum size of a lot will depend on equipment size of the producer and criticality considerations.DISSOLUTION PROCEDURE(This practice is replaced by Standard Practice C1168).PLUTONIUM BY CONTROLLED-POTENTIAL COULOMETRY(This test me
39、thod was discontinued in 1992 and replaced by Test Method C1165)PLUTONIUM BY CONTROLLED-POTENTIAL COULOMETRY(With appropriate sample preparation, controlled-potential coulometric measurement as described in Test Method C1108 maybe used for plutonium determination.)PLUTONIUM BY AMPEROMETRIC TITRATION
40、 WITH IRON(II)(This test method was discontinued in 1992 and replaced by Test Method C1206)PLUTONIUM BY CERIC SULFATE TITRATION TEST METHOD(This test method is replaced by Test Method C1235.)TEST METHOD FOR PLUTONIUM ASSAY BY PLUTONIUM(III) DIODE ARRAY SPECTROPHOTOMETRY(With appropriate sample prepa
41、ration, the measurement described in Test Method C1307 may be used for plutoniumdetermination.)6 Reagent Chemicals, American Chemical Society Specifications,” American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar
42、Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the UnitesUnited States Pharmacopeia and NationalFoundary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.7 The boldface numbers in parentheses refer to the list of references at the end of these test methods.C758 183U
43、RANIUM BY ARSENAZO I SPECTROPHOTOMETRIC TEST METHOD8. Scope8.1 This test method covers the determination of uranium in the range from 300 to 3000 g/g of plutonium.8. Scope8.1 This test method covers the determination of uranium in the range from 300 to 3000 g/g of plutonium.9. Summary of Test Method
44、9.1 Plutonium metal dissolved in 6 N HCl is reduced to Pu(III) with hydroxylamine hydrochloride. The uranium and plutoniumare separated by anion exchange; then the uranium is determined by measuring the absorbance of the U(VI)-Arsenazo I complexin a 1-cm cell at a wavelength of 600 nm versus a reage
45、nt blank.10. Procedure10.1 Transfer an aliquot of sample solution, prepared in accordance with Practice C1168, that contains approximately 70 mgof plutonium, to a 50-mL beaker and add 1 mL of nitric acid (sp gr 1.42) and heat to boiling. Proceed with the determination ofuranium in accordance with th
46、e appropriate sections of Test Methods C759.NOTE 1Since the sample starts as plutonium metal and is then dissolved in acid and diluted to volume and an aliquot of this solution taken for theuranium determination, the following equation for calculating the uranium concentration must be substituted fo
47、r the equation given in 28.1 of TestMethods C759:R 5Y 2B!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 diluted, mL, andE = volume of aliquot of V used for uranium determination, mL,whe
48、re: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 calibration blanks.THORIUM BY THORIN SPECTROPHOTOMETRIC TEST METHOD11. Scope11.1 This test method covers the determination
49、of thorium in the range from 10 to 150 g/g of plutonium in nuclear-gradeplutonium metal.11. Scope11.1 This test method covers the determination of thorium in 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 is added as a carrier and is precipitated along with thorium as insolublefluoride, while the plutonium remains in solution and is decanted after centrifugation of the sample. The thorium and lanthanumfluoride precipitates are
