1、Designation: C 761 04e1Standard Test Methods forChemical, Mass Spectrometric, Spectrochemical, Nuclear,and Radiochemical Analysis of Uranium Hexafluoride1This standard is issued under the fixed designation C 761; the number immediately following the designation indicates the year oforiginal adoption
2、 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.This standard has been approved for use by agencies of the Department of Defense. 4e1NO
3、TETwo versions of Table 1 appeared in this standard. The incorrect version was editorially deleted.1. Scope1.1 These test methods cover procedures for subsamplingand for chemical, mass spectrometric, spectrochemical,nuclear, and radiochemical analysis of uranium hexafluoride(UF6). Most of these test
4、 methods are in routine use todetermine conformance to UF6specifications in the Enrich-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
5、 determine how concernswith renumbering these sections, as analytical methods are replaced withstand-alone analytical methods, are best addressed in subsequent publica-tions.SectionsSubsampling of Uranium Hexafluoride 7 10Gravimetric Determination of Uranium 11 19Titrimetric Determination of Uranium
6、 20Preparation of High-Purity U3O821Isotopic Analysis 22Isotopic Analysis by Double-Standard Mass-SpectrometerMethod23 - 29Determination of Hydrocarbons, Chlorocarbons, and PartiallySubstituted Halohydrocarbons2936Atomic Absorption Determination of Antimony 36Spectrophotometric Determination of Brom
7、ine 37Titrimetric Determination of Chlorine 3844Determination of Silicon and Phosphorus 4551Determination of Boron and Silicon 5259Determination of Ruthenium 60Determination of Titanium and Vanadium 61Spectrographic Determination of Metallic Impurities 62Determination of Tungsten 63Determination of
8、Thorium and Rare Earths 6469Determination of Molybdenum 70Atomic Absorption Determination of Metallic Impurities 7176Impurity Determination by Spark-Source Mass Spectrography 77Determination of Boron-Equivalent Neutron Cross Section 78Determination of Uranium-233 Abundance by Thermal IonizationMass
9、Spectrometry79Determination of Uranium-232 by Alpha Spectrometry 8086Determination of Fission Product Activity 87Determination of Plutonium by Ion Exchange and Alpha Count-ing8892Determination of Plutonium by Extraction and Alpha Counting 93100Determination of Neptunium by Extraction and Alpha Count
10、ing 101108Atomic Absorption Determination of Chromium Soluble In Ura-nium Hexafluoride109115Atomic Absorption Determination of Chromium Insoluble In Ura-nium Hexafluoride116122Determination of Technetium-99 In Uranium Hexafluoride 123131Method for the Determiation of Gamma-Energy Emission Ratefrom F
11、ission Products in Uranium Hexafluoride132Determination of Metallic Impurities by ICP-AES 133142Determination of Molybdenum, Niobium, Tantalum, Titanium,and Tungsten by ICP-AES1431521.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theres
12、ponsibility 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 consideration statements, see Section 6.)2. Referenced Documents2.1 The following documents of the
13、 issue in effect on dateof material procurement form a part of this specification to theextent referenced herein:2.2 ASTM Standards:2C 696 Test Methods for Chemical, Mass Spectrometric, andSpectrochemical Analysis of Nuclear-Grade Uranium Di-oxide Powders and PelletsC 753 Specification for Nuclear-G
14、rade, Sinterable UraniumDioxide PowderC 787 Specification for Uranium Hexafluoride for Enrich-mentC 799 Test Methods for Chemical, Mass Spectrometric,Spectrochemical, Nuclear, and Radiochemical Analysis ofNuclear-Grade Uranyl Nitrate SolutionsC 996 Specification for Uranium Hexafluoride Enriched to1
15、These 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 July 1, 2004. Published August 2004. Originallyapproved in 1973. Last previous edition approved in 2001 as C 76
16、1 01.2For 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 International, 100 Barr Harbor Drive, PO
17、 Box C700, West Conshohocken, PA 19428-2959, United States.Less Than 5%235UC 1128 Preparation of Working Reference Materials for Usein the Analysis of Nuclear Fuel Cycle MaterialsC 1219 Test Methods for Arsenic in Uranium HexafluorideC 1233 Practice for Determining Equivalent Boron Con-tents of Nucl
18、ear MaterialsC 1267 Test Method for Uranium by Iron (II) Reduction inPhosphoric Acid Followed by Chromium (VI) Titration inthe Presence of VanadiumC 1287 Test Method for Determination of Impurities inUranium Dioxide by Inductively Coupled Plasma MassSpectrometryC 1295 Test Method for Gamma Energy Em
19、ission fromFission Products in Uranium Hexafluoride2C 1344 Test Method for Isotopic Analysis of UraniumHexafluoride by Single-Standard Gas Source Mass Spec-trometer MethodC 1346 Practice for Dissolution of UF6from P-10 TubesC 1380 Test Method for the Determination of UraniumContent and Isotopic Comp
20、osition of Isotope DilutionMass SpectrometryC 1413 Test Method for Isotopic Analysis of HydrolyzedUranium Hexafluoride and Uranyl Nitrate Solutions ByThermal Ionization Mass SpectrometryC 1428 Test Method for Isotopic Analysis of UraniumHexafluoride by Single-Standard Gas Source MultipleCollector Ma
21、ss Spectrometer MethodC 1429 Test Method for Isotopic Analysis of UraniumHexafluoride by Double-Standard Multi-Collector GasMass SpectrometerC 1441 Test Method for the Analysis of Refrigerant 114,Plus Other Carbon-Containing and Fluorine-ContainingCompounds in Uranium Hexafluoride via Fourier-Transf
22、orm Infrared (FTIR) SpectroscopyC 1474 Test Method for Analysis of Isotopic Compositionof Uranium in Nuclear-Grade Fuel Material by QuadrupoleInductively Coupled Plasma-Mass SpectrometryC 1477 Test Method for Isotopic Abundance Analysis ofUranium Hexafluoride by Multi-collector InductivelyCoupled Pl
23、asma-Mass SpectrometryC 1508 Test Method for Determination of Bromine andChlorine in UF6 and Uranyl Nitrate by X-Ray Fluores-cenceD 1193 Specification for Reagent WaterE60 Practice for Photometric and SpectrophotometricMethods for Chemical Analysis of MetalsE115 Practice for Photographic Processing
24、in OpticalEmission Spectrographic AnalysisE 130 Practice for Designation of Shapes and Sizes ofGraphite Electrodes2.3 American Chemical Society Specification:Reagent Chemicals32.4 Other Specifications:Uranium Hexafluoride: Base Charges, Use Charges, Spe-cial Charges, Table of Enriching Services, Spe
25、cifications,and Packaging4USEC 651 Good Handling and Practices for UF62.5 ANSI Standards:5ANSI N 14.1 Nuclear Material- Uranium Hexafluoride-Packaging for TransportISO 7195 Nuclear Energy-Packaging of Uranium Hexafluo-ride (UF6) for Transport3. Significance and Use3.1 Uranium hexafluoride is a basic
26、 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 designed to determine whether thematerial meets the requirements
27、 described in SpecificationC 787.4. Reagents4.1 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
28、available.6Other 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.4.2 Purity of WaterUnless otherwise indicated, referencesto water shall mean reagent water conformi
29、ng to SpecificationD 1193.75. Rejection5.1 Rejection or acceptance criteria are described in Speci-fications C 787 and C 996.6. Safety Considerations6.1 Since UF6is radioactive, toxic, and highly reactive,especially with reducing substances and moisture (see UraniumHexafluoride: Handling Procedures
30、and Container Criteria),appropriate facilities and practices for sampling and analysismust be provided.6.2 Committee C-26 Safeguards Statement:6.2.1 The material (uranium hexafluoride) to which thesetest methods apply, is subject to nuclear safeguards regulationsgoverning its possession and use. The
31、 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.3“Reagent Chemicals,American Chemical Society
32、 Specifications,” Washington,DC. For suggestions on the testing of reagents not listed by the American ChemicalSociety, See “Reagent Chemicals and Standards,” by Joseph Rosin, D.Van NostrandCo., Inc., New York, NY, and the “United States Pharmacopeia.”4United States Department of Energy, Oak Ridge,
33、TN 37830.5Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036.6The boldface numbers in parentheses refer to a list of references at the end ofthese test methods.7Type 1 and 2 water have been found to be suitable.C76104e126.2.2 When used in conjun
34、ction 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 the sole re
35、sponsibility of the user of these testmethods to assure that its application to safeguards has theapproval of the proper regulatory authorities.SUBSAMPLING OF URANIUM HEXAFLUORIDE(1, 2)67. Scope7.1 This test method is applicable to the subsampling (3) ofUF6from bulk sample containers into smaller co
36、ntainerssuitable for laboratory analyses. The procedure includessample filtration that facilitates determination of both solubleand insoluble chromium compounds.8. Summary of Test Method8.1 The UF6in the bulk sample container is liquefied andhomogenized by vigorous shaking. The container is inverted
37、and connected to the top of a heated vacuum-manifold system,and the subsample container is attached to the appropriate portof the system. The system is evacuated, and the liquid UF6isallowed to flow by gravity into the subsample container. Table1 summarizes the purpose of various subsamplings.8.2 If
38、 the determination of the volatile component of animpurity is needed (for example, chromium compounds), atotal gas tranfer may be necessary. In such case, the tared liquidUF6bulk sample container is connected to the top of the heatedmanifold without inversion, so that gaseous UF6is transferred.9. Ap
39、paratus9.1 Hot Water Bath.9.2 Heated Vacuum Manifold with Liquid Nitrogen ColdTrap (Table 1).NOTE 1All lines are38-in. (9.5-mm) Monel tubing.NOTE 2All valves are Monel diaphragm-type valves.NOTE 3The valves and lines are wrapped with heating tape to maintain a system temperature of about 80C.NOTE 4V
40、alve 2 is a 3-way valve modified to make it a 4-way valve. When the valve is closed, the polychlorotrifluoroethylene tube is isolated fromthe system, but the lines from Valve 1 to Valve 3 and to the bulk container are open.C76104e139.3 Gaseous Isotopic Abundance Sample Tube (Fig. 1).9.4 Polychlorotr
41、ifluoroethylene Sample Tube (Fig. 2).9.5 Polychlorotrifluoroethylene Knockout Cylinder (Fig.3), closed with a Cajon8M-16 VCR-1 female nut and an M-16VCR-4 male nut, or equivalent.9.6 Nickel Filter Disk, porous, 2-m, free of chromium (Fig.4). Mott Metallurgical Corp. or equivalent.99.7 Gas Sample Cyl
42、inder, 0.5 L.10. Procedure10.1 System Preparation:10.1.1 Place the bulk sample container in a water bath at90C 63C.10.1.2 After the UF6has been liquefied, remove the con-tainer from the bath, shake to homogenize the sample, andconnect it at the top of the vacuum-manifold system shown inTable 1. The
43、container will be inverted if liquid UF6must besubsampled.10.1.3 When a liquid subsample is required for uraniumanalysis or chemical impurity (metal, halogen), and TIMSisotopic analysis, connect a tared polychlorotrifluoroethylenesample tube at the Cajon connection at the bottom of thesystem. If thi
44、s subsample is not required, attach a blind fittingat this point.10.1.4 When a liquid subsample is required for gaseousisotopic analysis or all gas carbon compound determination,attach a tared isotopic abundance sample tube to the sampletube connection. If a subsample is not required, attach a cap a
45、tthis point.10.1.5 When a total gas UF6transfer is necessary, connectthe UF6bulk container without inversion. Attach a polychlo-rotrifluoroethylene knockout cylinder at the tube connectionand attach a cap at the fitting for isotopic abundance sampletube.10.1.6 Close Valve 4, then evacuate the entire
46、 system,except for the UF6bulk sample container.10.2 Sample Transfer to the polychlorotrifluoroethyleneTube:10.2.1 Close Valves 1, 2, and 3.10.2.2 To remove solid impurities, which may be present inthe bulk-container valve, open that valve and then close itquickly. Transfer this flush aliquot of liq
47、uid UF6to a polychlo-rotrifluoroethylene sample tube, as described below, and dis-card.10.2.3 Open the bulk-container valve; then open Valve 2slowly, allowing liquid UF6to flow into the polychlorotrifluo-roethylene tube. When the tube is half full of liquid UF6, closeValve 2.10.2.4 Close the bulk-co
48、ntainer valve.10.2.5 Open Valve 3 to remove UF6from the system. OpenValve 1 to ensure that the system is evacuated.10.2.6 Close Valve 3.10.2.7 Immerse the polychlorotrifluoroethylene tube in liq-uid nitrogen for 6 min.10.2.8 Open Valve 2 to ensure that the sample does not exerta detectable vapor pre
49、ssure.10.2.9 Close Valve 5.8Brand names mentioned in this procedure are intended to be typical, notlimiting. Another brand of comparable characteristics could perform equally well.9The filter disk should weigh approximately 1 g and be 16 mm in diameter by0.6 m thick. It should be of nickel powder produced from carbonyl nickel andformed by the no pressure sintering method in graphite or ceramic molds.FIG. 1 Isotopic Abundance Sample TubeFIG. 2 Small TFCE Sample TubeC76104e1410.2.10 Open Valves 3 and 4, and admit dry nitrogen or dryair until a pressure
