1、Designation: C761 11Standard 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.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1
3、 These test methods cover or give reference to proce-dures for subsampling and for 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 Enrich
4、ment and Conversion Facilities.1.2 The analytical procedures in this document appear in thefollowing order:NOTE 1Subcommittee C26.05 will confer with C26.02 concerningthe renumbered section in Test Methods C761 to determine how concernswith renumbering these sections are best addressed in subsequent
5、 publi-cations as analytical methods are replaced with stand-alone analyticalmethods.SectionsSubsampling of Uranium Hexafluoride 7Gravimetric Determination of Uranium 8 16Titrimetric Determination of Uranium 17Preparation of High-Purity U3O818Isotopic Analysis 19Determination of Hydrocarbons, Chloro
6、carbons, and PartiallySubstituted Halohydrocarbons2026Determination of Antimony 27Determination of Bromine 28Determination of Chlorine 29 35Determination of Silicon and Phosphorus 36 42Determination of Boron and Silicon 43Determination of Ruthenium 44Determination of Titanium and Vanadium 45Spectrog
7、raphic Determination of Metallic Impurities 46Determination of Tungsten 47Determination of Thorium and Rare Earths 48Determination of Molybdenum 49Atomic Absorption Determination of Metallic Impurities 50 55Impurity Determination by Spark-Source Mass Spectrography 56Determination of Boron-Equivalent
8、 Neutron Cross Section 57Determination of Uranium-233 Abundance by Thermal IonizationMass Spectrometry58Determination of Uranium-232 by Alpha Spectrometry 59 65Determination of Fission Product Activity 66Determination of Plutonium by Ion Exchange and Alpha Count-ing6771Determination of Plutonium by
9、Extraction and Alpha Counting 72 79Determination of Neptunium by Extraction and Alpha Counting 80 87Atomic Absorption Determination of Chromium Soluble In Ura-nium Hexafluoride8894Atomic Absorption Determination of Chromium Insoluble In Ura-nium Hexafluoride95 101Determination of Technetium-99 In Ur
10、anium Hexafluoride 102 110Method for the Determiation of Gamma-Energy Emission Ratefrom Fission Products in Uranium Hexafluoride111Determination of Metallic Impurities by ICP-AES 112 121Determination of Molybdenum, Niobium, Tantalum, Titanium,and Tungsten by ICP-AES122 1311.3 The values stated in SI
11、 units are to be regarded asstandard. No other units of measurement are included in 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 and health
12、practices and determine the applica-bility of regulatory limitations prior to use. (For specificsafeguard and safety consideration statements, see Section 6.)2. Referenced Documents2.1 The following documents of the issue in effect on dateof material procurement form a part of this specification to
13、theextent referenced herein:2.2 ASTM Standards:2C787 Specification for Uranium Hexafluoride for Enrich-mentC799 Test Methods for Chemical, Mass Spectrometric,Spectrochemical, Nuclear, and Radiochemical Analysis ofNuclear-Grade Uranyl Nitrate SolutionsC859 Terminology Relating to Nuclear MaterialsC99
14、6 Specification for Uranium Hexafluoride Enriched toLess Than 5 %235UC1128 Guide for Preparation of Working Reference Mate-rials for Use in Analysis of Nuclear Fuel Cycle MaterialsC1219 Test Methods for Arsenic in Uranium HexafluorideC1233 Practice for Determining Equivalent Boron Contentsof Nuclear
15、 Materials1These test methods are under the jurisdiction of ASTM Committee C26 onNuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 onMethods of Test.Current edition approved May 15, 2011. Published July 2011. Originallyapproved in 1973. Last previous edition approved in 200
16、4 as C761 04e1. DOI:10.1520/C0761-11.2For referenced ASTM 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.1Copyright ASTM Internat
17、ional, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.C1267 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 Co
18、mpounds by InductivelyCoupled Plasma Mass SpectrometryC1295 Test Method for Gamma Energy Emission fromFission Products in Uranium Hexafluoride and UranylNitrate SolutionC1344 Test Method for Isotopic Analysis of UraniumHexafluoride by Single-Standard Gas Source Mass Spec-trometer MethodC1346 Practic
19、e for Dissolution of UF6from P-10 Tubes,C1380 Test Method for the Determination of UraniumContent and Isotopic Composition by Isotope DilutionMass SpectrometryC1413 Test Method for Isotopic Analysis of HydrolyzedUranium Hexafluoride and Uranyl Nitrate Solutions byThermal Ionization Mass Spectrometry
20、C1428 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 Refrigeran
21、t 114,Plus Other Carbon-Containing and Fluorine-ContainingCompounds in Uranium Hexafluoride via Fourier-Transform Infrared (FTIR) SpectroscopyC1474 Test Method forAnalysis of Isotopic Composition ofUranium in Nuclear-Grade Fuel Material by QuadrupoleInductively Coupled Plasma-Mass SpectrometryC1477
22、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 Meth
23、od 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 f
24、or 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, a
25、nd RelatedMaterials by Spectrophotometry2.3 American Chemical Society Specification:Reagent Chemicals32.4 Other Specifications:Uranium Hexafluoride : Base Charges, Use Charges, Spe-cial Charges, Table of Enriching Services, Specifications,and Packaging4USEC 651 Good Handling and Practices for UF62.5
26、 ANSI Standards:5ANSI 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. Significance and Use3.1 Uranium hexafluoride is a basic material used to preparenuclear reactor fuel. To be sui
27、table for this purpose the materialmust meet criteria for uranium content, isotopic composition,metallic impurities, hydrocarbon and halohydrocarbon content.These test methods are designed to determine whether thematerial meets the requirements described in SpecificationsC787 and C996.4. Reagents4.1
28、 Purity of ReagentsReagent grade chemicals shall beused in all procedures. Unless otherwise indicated, all reagentsshall conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society, wheresuch specifications are available.3Other grades may be used,provided th
29、at it is first established that the reagent to be used isof sufficiently high purity to permit its use without lesseningthe accuracy of the determination.4.2 Purity of WaterUnless otherwise indicated, referencesto water shall mean reagent water conforming to SpecificationD1193.65. Rejection5.1 Rejec
30、tion or acceptance criteria are described in Speci-fications C787 and C996.6. Safety Considerations6.1 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),
31、appropriate facilities and practicesfor sampling and analysis must be provided.6.2 Hydrofluoric acid is a highly corrosive acid that canseverely burn skin, eyes, and mucous membranes. Hydroflu-oric acid is similar to other acids in that the initial extent of theburn depends on the concentration, the
32、 temperature, and theduration of the contact with the acid. Hydrofluoric acid differs3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for
33、 LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K. and the United States Pharmacopeia andNational Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.4United States Department of Energy, Oak Ridge, TN 37830.5Available from American National Standards Institute (ANSI), 25 W. 43rd St
34、.,4th Floor, New York, NY 10036.6Type 1 and 2 water have been found to be suitable.C761 112from other acids because the fluoride ion readily penetrates theskin, causing destruction of deep issue layers. Unlike otheracids that are rapidly neutralized, hydrofluoric acid reactionswith tissue may contin
35、ue for days if left untreated. Due to theserious consequences of hydrofluoric acid burns, prevention ofexposure or injury of personnel is the primary goal. Utilizationof appropriate laboratory controls (hoods) and wearing ad-equate personal protective equipment to protect from skin andeye contact is
36、 essential.6.3 Committee C-26 Safeguards Statement:6.3.1 The material (uranium hexafluoride) to which thesetest methods apply, is subject to nuclear safeguards regulationsgoverning its possession and use. The following analyticalprocedures in these test methods have been designated astechnically acc
37、eptable for generating safeguards accountabilitymeasurement data: Gravimetric Determination of Uranium;Titrimetric Determination of Uranium; All Isotopic Analyses.6.3.2 When used in conjunction with appropriate certifiedReference Materials (CRMs), these procedures can demon-strate traceability to th
38、e 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 its application to safeguards has theapproval of th
39、e proper regulatory authorities.SUBSAMPLING OF URANIUM HEXAFLUORIDE7. Scope7.1 This test method has been discontinued (see C76104e1). The subsampling of UF6from bulk sample contain-ers into smaller containers suitable for laboratory analyses hasbeen published as a separate Practice, C1689.GRAVIMETRI
40、C DETERMINATION OF URANIUM8. Scope8.1 Practice C1346 is applicable to the hydrolysis of ura-nium hexafluoride in polychlorotrifluoroethylene (P10) tubes.The following test method is then applicable to the directgravimetric determination of uranium.9. Summary of Test Method9.1 Asample of uranium hexa
41、fluoride is weighed, cooled inliquid nitrogen, and hydrolyzed with water. The uranyl fluoridesolution produced is evaporated to dryness and converted touranic oxide by pyrohydrolysis. The uranium content is deter-mined from the weight of the uranium oxide after correctingfor stoichiometry based on i
42、sotopic content, ignition condi-tions, and nonvolatile impurities. Ref. (1-4).710. Interferences10.1 Nonvolatile impurities affect the accuracy of themethod and must be measured by spectrographic analysis withcorrections applied.11. Apparatus11.1 Polytrifluorochloroethylene (PTFCE) Sample Tube,TFCE
43、Gasket, Flare Nut, and Plug, see Fig. 1.11.2 Platinum Boat and CoverThe cover should be plati-num gauze (52 mesh) and shaped to cover the boat (Fig. 2).11.3 Muffle Furnace, must be capable of operating continu-ously at 875C and maintain this temperature within 625C.7The boldface numbers in parenthes
44、es refer to a list of references at the end ofthese test methods.FIG. 1 Example of a Polychlorotrifluoroethylene P-10 TubeC761 113The furnace shall be equipped with a steam supply that ispassed through a tube furnace to preheat the steam to 875C.11.4 Tube Furnace, must be capable of operating contin
45、u-ously at 875C and maintain this temperature within 25C.11.5 Infrared Heat Lamps, 250 watts.11.6 Analytical Balance.11.7 Vacuum Oven.11.8 Dewar Flask, stainless steel.11.9 Spatula, platinum.11.10 PTFCE Rod, 120 mm long and 1.6 mm in diameter.11.11 Forceps, platinum tipped.11.12 Jig, suitable for ho
46、lding the TFCE sample tube so thatit can be opened with a wrench.11.13 Box Wrench, to fit sample tube plug.11.14 Beaker, stainless steel, 125 mL capacity.12. Reagents12.1 Liquid Nitrogen.12.2 Nitric Acid (sp gr 1.42)concentrated nitric acid(HNO3).12.3 Nitric Acid (4M)Mix 500 mLof concentrated HNO3wi
47、th 1500 mL of distilled water.12.4 Detergent.13. Sampling13.1 A UF6sample is taken as described in Practice C1689.14. Procedure14.1 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 t
48、he sample if aleak is indicated.14.2 Allow the sample tube to stand overnight in thelaboratory.14.3 Wipe the sample tube with a lint-free tissue to removeany moisture or foreign material that might be adhering.14.4 Weigh the sample tube to the nearest 0.1 mg.14.5 Heat the platinum boat and screen in
49、 the pyrohydroly-sis furnace at 875C for 20 min.14.6 Cool the platinum boat and store in a desiccator for 40min. Weigh the boat and screen to the nearest 0.1 mg.14.7 Freeze the sample by immersing the sample tube inliquid nitrogen for 10 min.14.8 Add enough chilled water to the tared platinum boat toimmerse the sample tube (about 50 mL).14.9 Place the sample tube in the jig and loosen the plugwith the box wrench.14.10 Remove the sample tube from the jig and unscrew theplug while holding the sample tube in an upright position.14.11 Remove the
