ASTM C761-2018 Standard Test Methods for Chemical Mass Spectrometric Spectrochemical Nuclear and Radiochemical Analysis of Uranium Hexafluoride《六氟化铀化学、质谱、光谱化学、核化学和放射化学分析的标准试验方法》.pdf

1、Designation: C761 18Standard Test Methods forChemical, Mass Spectrometric, Spectrochemical, Nuclear,and Radiochemical Analysis of Uranium Hexafluoride1This standard is issued under the fixed designation C761; 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 These test methods cover or give reference to proce-dures for subsampling and fo

3、r chemical, mass spectrometric,spectrochemical, nuclear, and radiochemical analysis of ura-nium hexafluoride (UF6). Most of these test methods are inroutine use to determine conformance to UF6specifications inthe Enrichment and Conversion Facilities.1.2 The analytical procedures in this document app

4、ear in thefollowing order:NOTE 1Subcommittee C26.05 will confer with C26.02 concerning therenumbered section in Test Methods C761 to determine how concernswith renumbering these sections are best addressed in subsequent publi-cations as analytical methods are replaced with stand-alone analyticalmeth

5、ods.SectionsSubsampling of Uranium Hexafluoride 8Gravimetric Determination of Uranium 9 17Titrimetric Determination of Uranium 18Preparation of High-Purity U3O819Isotopic Analysis 20Determination of Hydrocarbons, Chlorocarbons, and PartiallySubstituted Halohydrocarbons21 27Determination of Antimony

6、28Determination of Bromine 29Determination of Chlorine 30 36Determination of Silicon and Phosphorus 37 43Determination of Boron and Silicon 44Determination of Ruthenium 45Determination of Titanium and Vanadium 46Spectrographic Determination of Metallic Impurities 47Determination of Tungsten 48Determ

7、ination of Thorium and Rare Earths 49Determination of Molybdenum 50Atomic Absorption Determination of Metallic Impurities 51 56Impurity Determination by Spark-Source Mass Spectrography 57Determination of Boron-Equivalent Neutron Cross Section 58Determination of Uranium-233 Abundance by Thermal Ioniz

8、ationMass Spectrometry59Determination of Uranium-232 by Alpha Spectrometry 60 66Determination of Fission Product Activity 67Determination of Plutonium by Ion Exchange and AlphaCounting68 72Determination of Plutonium by Extraction and Alpha Counting 73 80Determination of Neptunium by Extraction and A

9、lpha Counting 81 88Atomic Absorption Determination of Chromium Soluble InUranium Hexafluoride89 95Atomic Absorption Determination of Chromium Insoluble InUranium Hexafluoride101 102Determination of Technetium-99 In Uranium Hexafluoride 103 110Method for the Determination of Gamma-Energy Emission Rat

10、efrom Fission Products in Uranium Hexafluoride112Determination of Metallic Impurities by ICP-AES 113 122Determination of Molybdenum, Niobium, Tantalum, Titanium,and Tungsten by ICP-AES123 1321.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included i

11、n thisstandard.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 standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitatio

12、ns prior to use.(For specific safeguard and safety consideration statements, seeSection 7.)1.5 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standar

13、ds, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 The following documents of the issue in effect on dateof material procurement form a part of this specification to theextent referenced herein:2.2 ASTM Standar

14、ds:2C787 Specification for Uranium Hexafluoride for Enrich-mentC799 Test Methods for Chemical, Mass Spectrometric,Spectrochemical, Nuclear, and RadiochemicalAnalysis ofNuclear-Grade Uranyl Nitrate SolutionsC859 Terminology Relating to Nuclear Materials1These test methods are under the jurisdiction o

15、f ASTM Committee C26 onNuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 onMethods of Test.Current edition approved Feb. 1, 2018. Published February 2018. Originallyapproved in 1973. Last previous edition approved in 2011 as C761 11. DOI:10.1520/C0761-18.2For referenced AST

16、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 Conshohoc

17、ken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organiz

18、ation Technical Barriers to Trade (TBT) Committee.1C996 Specification for Uranium Hexafluoride Enriched toLess Than 5 %235UC1128 Guide for Preparation of Working Reference Materi-als for Use in Analysis of Nuclear Fuel Cycle MaterialsC1219 Test Methods for Arsenic in Uranium Hexafluoride(Withdrawn 2

19、015)3C1233 Practice for Determining Equivalent Boron Contentsof Nuclear MaterialsC1267 Test Method for Uranium by Iron (II) Reduction inPhosphoric Acid Followed by Chromium (VI) Titration inthe Presence of VanadiumC1287 Test Method for Determination of Impurities inNuclear Grade Uranium Compounds by

20、 InductivelyCoupled Plasma Mass SpectrometryC1295 Test Method for Gamma Energy Emission fromFission and Decay Products in Uranium Hexafluoride andUranyl Nitrate SolutionC1344 Test Method for Isotopic Analysis of UraniumHexafluoride by Single-Standard Gas Source Mass Spec-trometer MethodC1346 Practic

21、e for Dissolution of UF6from P-10 TubesC1380 Test Method for the Determination of Uranium Con-tent and Isotopic Composition by Isotope Dilution MassSpectrometryC1413 Test Method for Isotopic Analysis of HydrolyzedUranium Hexafluoride and Uranyl Nitrate Solutions byThermal Ionization Mass Spectrometr

22、yC1428 Test Method for Isotopic Analysis of UraniumHexafluoride by SingleStandard Gas Source MultipleCollector Mass Spectrometer MethodC1429 Test Method for Isotopic Analysis of UraniumHexafluoride by Double-Standard Multi-Collector GasMass SpectrometerC1441 Test Method for The Analysis of Refrigera

23、nt 114,Plus Other Carbon-Containing and Fluorine-ContainingCompounds in Uranium Hexafluoride via Fourier-Transform Infrared (FTIR) SpectroscopyC1474 Test Method for Analysis of Isotopic Composition ofUranium in Nuclear-Grade Fuel Material by QuadrupoleInductively Coupled Plasma-Mass SpectrometryC147

24、7 Test Method for Isotopic Abundance Analysis ofUranium Hexafluoride and Uranyl Nitrate Solutions byMulti-Collector, Inductively Coupled Plasma-Mass Spec-trometryC1508 Test Method for Determination of Bromine andChlorine in UF6and Uranyl Nitrate by X-Ray Fluores-cence (XRF) SpectroscopyC1539 Test Me

25、thod for Determination of Technetium-99 inUranium Hexafluoride by Liquid Scintillation CountingC1561 Guide for Determination of Plutonium and Neptu-nium in Uranium Hexafluoride and U-Rich Matrix byAlpha SpectrometryC1636 Guide for the Determination of Uranium-232 inUranium HexafluorideC1689 Practice

26、 for Subsampling of Uranium HexafluorideC1742 Test Method for Isotopic Analysis of UraniumHexafluoride by Double Standard Single-Collector GasMass Spectrometer MethodD1193 Specification for Reagent WaterD3084 Practice for Alpha-Particle Spectrometry of WaterE60 Practice for Analysis of Metals, Ores,

27、 and RelatedMaterials by Spectrophotometry2.3 American Chemical Society Specification:Reagent Chemicals42.4 Other Specifications:Uranium Hexafluoride: Base Charges, Use Charges, SpecialCharges, Table of Enriching Services, Specifications, andPackaging5USEC 651 Good Handling and Practices for UF62.5

28、ANSI Standards:6ANSI N 14.1 Nuclear Material-Uranium Hexafluoride-Packaging for Transport2.6 ISO Standards:ISO 7195 Nuclear Energy-Packaging of Uranium Hexafluo-ride (UF6) for Transport3. Terminology3.1 Definitions:3.1.1 For definitions of terms relating to the nuclear fuelcycle, refer to Terminolog

29、y C859.4. Significance and Use4.1 Uranium hexafluoride is a basic material used to preparenuclear reactor fuel. To be suitable for this purpose the materialmust meet criteria for uranium content, isotopic composition,metallic impurities, hydrocarbon and halohydrocarbon content.These test methods are

30、 designed to determine whether thematerial meets the requirements described in SpecificationsC787 and C996.5. Reagents5.1 Purity of ReagentsReagent grade chemicals shall beused in all procedures. Unless otherwise indicated, all reagentsshall conform to the specifications of the Committee onAnalytica

31、l Reagents of the American Chemical Society, wheresuch specifications are available.4Other grades may be used,provided that it is first established that the reagent to be used isof sufficiently high purity to permit its use without lesseningthe accuracy of the determination.5.2 Purity of WaterUnless

32、 otherwise indicated, referencesto water shall mean reagent water conforming to SpecificationD1193.73The last approved version of this historical standard is referenced onwww.astm.org.4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggesti

33、ons on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K. and the United States Pharmacopeia andNational Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.5United States Department of Ener

34、gy, Oak Ridge, TN 37830.6Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036.7Type 1 and 2 water have been found to be suitable.C761 1826. Rejection6.1 Rejection or acceptance criteria are described in Speci-fications C787 and C996.7. Safety Cons

35、iderations7.1 Since UF6is radioactive, toxic, and highly reactive,especially with reducing substances and moisture (see UraniumHexafluoride: Handling Procedures and Container Criteria,sections 2.4 through 2.6), appropriate facilities and practicesfor sampling and analysis must be provided.7.2 Hydrof

36、luoric acid is a highly corrosive acid that canseverely burn skin, eyes, and mucous membranes. Hydroflu-oric acid differs from other acids because the fluoride ionreadily penetrates the skin, causing destruction of deep tissuelayers. Unlike other acids that are rapidly neutralized, hydro-fluoric aci

37、d reactions with tissue may continue for days if leftuntreated. Familiarization and compliance with the Safety DataSheet is essential.7.3 Committee C26 Safeguards Statement:7.3.1 The material (uranium hexafluoride) to which thesetest methods apply, is subject to nuclear safeguards regulationsgoverni

38、ng its possession and use. The following analyticalprocedures in these test methods have been designated astechnically acceptable for generating safeguards accountabilitymeasurement data: Gravimetric Determination of Uranium;Titrimetric Determination of Uranium; All Isotopic Analyses.7.3.2 When used

39、 in conjunction with appropriate certifiedReference Materials (CRMs), these procedures can demon-strate traceability 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 t

40、he sole responsibility of the user of these testmethods to assure that its application to safeguards has theapproval of the proper regulatory authorities.SUBSAMPLING OF URANIUM HEXAFLUORIDE8. Scope8.1 This test method has been discontinued (seeC761 041). The subsampling of UF6from bulk samplecontain

41、ers into smaller containers suitable for laboratory analy-ses has been published as a separate Practice C1689.GRAVIMETRIC DETERMINATION OF URANIUM9. Scope9.1 Practice C1346 is applicable to the hydrolysis of ura-nium hexafluoride in polychlorotrifluoroethylene (P10) tubes.The following test method i

42、s then applicable to the directgravimetric determination of uranium.10. Summary of Test Method10.1 A sample of uranium hexafluoride is weighed, cooledin liquid nitrogen, and hydrolyzed with water. The uranylfluoride solution produced is evaporated to dryness and con-verted to uranic oxide by pyrohyd

43、rolysis. The uranium contentis determined from the weight of the uranium oxide aftercorrecting for stoichiometry based on isotopic content, ignitionconditions, and nonvolatile impurities. Ref. (1-4).811. Interferences11.1 Nonvolatile impurities affect the accuracy of themethod and must be measured b

44、y spectrographic analysis withcorrections applied.12. Apparatus12.1 Polytrifluorochloroethylene (PTFCE) Sample Tube,TFCE Gasket, Flare Nut, and Plug, see Fig. 1.12.2 Platinum Boat and CoverThe cover should be plati-num gauze (52 mesh) and shaped to cover the boat (Fig. 2).12.3 Muffle Furnace, must b

45、e capable of operating continu-ously at 875C and maintain this temperature within 625C.The furnace shall be equipped with a steam supply that ispassed through a tube furnace to preheat the steam to 875C.12.4 Tube Furnace, must be capable of operating continu-ously at 875C and maintain this temperatu

46、re within 25C.12.5 Infrared Heat Lamps, 250 watts.12.6 Analytical Balance.12.7 Vacuum Oven.12.8 Dewar Flask, stainless steel.12.9 Spatula, platinum.12.10 PTFCE Rod, 120 mm long and 1.6 mm in diameter.12.11 Forceps, platinum tipped.12.12 Jig, suitable for holding the TFCE sample tube so thatit can be

47、 opened with a wrench.12.13 Box Wrench, to fit sample tube plug.12.14 Beaker, stainless steel, 125 mL capacity.13. Reagents13.1 Liquid Nitrogen.13.2 Nitric Acid (sp gr 1.42)concentrated nitric acid(HNO3).13.3 Nitric Acid (4M)Mix 500 mL of concentrated HNO3with 1500 mL of distilled water.13.4 Deterge

48、nt.14. Sampling14.1 A UF6sample is taken as described in Practice C1689.15. Procedure15.1 Inspect the PTFCE sample tube for leaks.NOTE 2An indication of a leak is a yellow-green residue on the flarenut and cap or a yellow discoloration in the tube. Discard the sample if aleak is indicated.15.2 Allow

49、 the sample tube to stand overnight in thelaboratory.8The boldface numbers in parentheses refer to a list of references at the end ofthese test methods.C761 18315.3 Wipe the sample tube with a lint-free tissue to removeany moisture or foreign material that might be adhering.15.4 Weigh the sample tube to the nearest 0.1 mg.15.5 Heat the platinum boat and screen in the pyrohydroly-sis furnace at 875C for 20 min.15.6 Cool the platinum boat and store in a desiccator for 40min. Weigh the boat and screen to the nearest 0.1 mg.15.7 Freeze the