1、Designation: C759 10C759 18Standard Test Methods forChemical, Mass Spectrometric, Spectrochemical, Nuclear,and Radiochemical Analysis of Nuclear-Grade PlutoniumNitrate Solutions1This standard is issued under the fixed designation C759; the number immediately following the designation indicates the y
2、ear 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 chemical,
3、 mass spectrometric, spectrochemical, nuclear, and radiochemicalanalysis of nuclear-grade plutonium nitrate solutions to determine compliance with specifications.1.2 The analytical procedures appear in the following order:SectionsPlutonium by Controlled-Potential Coulometry 2Plutonium by Amperometri
4、c Titration with Iron(II) 2Plutonium by Diode Array SpectrophotometryFree Acid by Titration in an Oxalate Solution 8 to 15Free Acid by Iodate Precipitation-Potentiometric TitrationTest Method16 to 22Uranium by Arsenazo I Spectrophotometric Test Method 23 to 33Thorium by Thorin Spectrophotometric Tes
5、t Method 34 to 42Iron by 1,10-Phenanthroline Spectrophotometric Test Method 43 to 50Impurities by ICP-AESChloride by Thiocyanate Spectrophotometric Test Method 51 to 58Fluoride by Distillation-Spectrophotometric Test Method 59 to 66Sulfate by Barium Sulfate Turbidimetric Test Method 67 to 74Isotopic
6、 Composition by Mass Spectrometry 75 to 76Plutonium 238 Isotopic Abundance by Alpha SpectrometryPlutonium-238 Isotopic Abundance by Alpha SpectrometryAmericium-241 by Extraction and Gamma Counting 77 to 85Americium-241 by Gamma Counting 86 to 94Gamma-Emitting Fission Products, Uranium, and Thorium b
7、yGamma-Ray Spectroscopy94 to 102Rare Earths by Copper Spark Spectrochemical Test Method 103 to 105Tungsten, Niobium (Columbium), and Tantalum by Spectrochemical Test Method106 to 114Tungsten, Niobium (Columbium), and Tantalum by Spectro-chemical Test Method106 to 114Sample Preparation for Spectrogra
8、phic Analysis for GeneralImpurities115 to 1181.3 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityo
9、f 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 hazard statements, see Section 6.1.5 This international standard was developed in acc
10、ordance 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) Committee.1 These test methods are under t
11、he jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 on Methodsof Test.Current edition approved June 1, 2010Sept. 1, 2018. Published July 2010October 2018. Originally approved in 1973. Last previous edition approved in 20042010 asC759 0
12、4.C759 10. DOI: 10.1520/C0759-10.10.1520/C0759-18.2 Discontinued as of November 15, 1992.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible
13、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 official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Co
14、nshohocken, PA 19428-2959. United States12. Referenced Documents2.1 ASTM Standards:3C697 Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Plutonium DioxidePowders and PelletsC852C852/C852M Guide for Design Criteria for Plutonium GloveboxesC859 Terminology
15、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 IndustryC1108 Test Method for Plutonium by Controlled-Po
16、tential 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 Test Method for Determining Plutonium by Controlled-Pote
17、ntial Coulometry in H2SO4 at a Platinum Working ElectrodeC1206 Test Method for Plutonium by Iron (II)/Chromium (VI) Amperometric Titration (Withdrawn 2015)4C1210 Guide for Establishing a Measurement System Quality Control Program for Analytical Chemistry Laboratories Withinthe Nuclear IndustryC1235
18、Test Method for Plutonium by Titanium(III)/Cerium(IV) Titration (Withdrawn 2005)4C1268 Test Method for Quantitative Determination of 241Am in Plutonium by Gamma-Ray SpectrometryC1297 Guide for Qualification of Laboratory Analysts for the Analysis of Nuclear Fuel Cycle MaterialsC1307 Test Method for
19、Plutonium Assay by Plutonium (III) Diode Array SpectrophotometryC1415 Test Method for238Pu Isotopic Abundance By Alpha SpectrometryC1432 Test Method for Determination of Impurities in Plutonium: Acid Dissolution, Ion Exchange Matrix Separation, andInductively Coupled Plasma-Atomic Emission Spectrosc
20、opic (ICP/AES) AnalysisD1193 Specification for Reagent WaterE50 Practices forApparatus, Reagents, and Safety Considerations for ChemicalAnalysis of Metals, Ores, and Related MaterialsE115 Practice for Photographic Processing in Optical Emission Spectrographic Analysis (Withdrawn 2002)4E116 Practice
21、for Photographic Photometry in Spectrochemical Analysis (Withdrawn 2002)43. Terminology3.1 For definitions of terms used in this test method but not defined herein, refer to Terminology C859.4. Significance and Use4.1 These test methods are designed to show whether a given material meets the purchas
22、ers 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 in the plutonium-nitrate solution is made to establish whether theeffective fissile content is in compliance with the purc
23、hasers specifications.4.1.3 Impurity content is determined by a variety of methods to ensure that the maximum concentration limit of specifiedimpurities is not exceeded. Determination of impurities is also required for calculation of the equivalent boron content (EBC).4.2 Fitness for Purpose of Safe
24、guards 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 C26 Safeguards Statement54.1 The material (plutonium nitrate) to which these test methods apply i
25、s subject to nuclear safeguards regulations governingits possession and use. The following analytical procedures in these test methods have been designated as technically acceptablefor generating safeguards accountability measurement data: Plutonium by Controlled-Potential Coulometry; Plutonium byAm
26、perometric Titration with Iron(II); Plutonium by Diode Array Spectrophotometry and Isotopic Composition by MassSpectrometry.4.2 When used in conjunction with appropriate Certified Reference Materials (CRMs), these procedures can demonstratetraceability to the national measurement base. However, adhe
27、rence to these procedures does not automatically guarantee regulatoryacceptance of the resulting safeguards measurements. It remains the sole responsibility of the user of these test methods to assurethat their application to safeguards has the approval of the proper regulatory authorities.3 For ref
28、erenced 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 standards Document Summary page on the ASTM website4 The last approved version of this historical standard is referenced
29、 on www.astm.org.C759 1825. Reagents and Materials5.1 Purity of ReagentsReagent grade chemicals shall be used in all test methods. Unless otherwise indicated, it is intendedthat all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society,
30、where such specifications are available.5 Other grades may be used, provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy of the determination.5.2 Purity of WaterUnless otherwise indicated, reference to water shall be underst
31、ood to mean reagent water conforming toSpecification D1193.6. Safety Hazards6.1 Since plutonium bearing materials are radioactive and toxic, adequate laboratory facilities, gloved boxes, fume hoods, etc.,along with safe techniques, must be used in handling samples containing these materials. A detai
32、led 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 practices as are given in Guide C852C852/C852M and in Refs (1) through (2).66.2 Adequate laboratory facilities, such as fu
33、me hoods and controlled ventilation, along with safe techniques, must be used inthis procedure. Extreme care should be exercised in using hydrofluoric and other hot, concentrated acids. Use of proper gloves isrecommended. Refer to the laboratorys chemical hygiene plan and other applicable guidance f
34、or handling chemical andradioactive materials and for the management of radioactive, mixed, and hazardous waste.6.3 Hydrofluoric acid is a highly corrosive acid that can severely burn skin, eyes, and mucous membranes. Hydrofluoric acidis similar to other acids in that the initial extent of a burn de
35、pends on the concentration, the temperature, and the duration of contactwith the acid. Hydrofluoric acid differs from other acids because the fluoride ion readily penetrates the skin, causing destructionof deep tissue layers. Unlike other acids that are rapidly neutralized, hydrofluoric acid reactio
36、ns with tissue may continue for daysif left untreated. Due to the serious consequence of hydrofluoric acid burns, prevention of exposure or injury of personnel is theprimary goal. Utilization of appropriate laboratory controls (hoods) and wearing adequate personal protective equipment to protectfrom
37、 skin and eye contact is essential.7. Sampling7.1 A sample representative of the lot shall be taken from each lot into a container or multiple containers that are of suchcomposition that corrosion, chemical change, radiolytic decomposition products, and method of loading or sealing will not disturbt
38、he chemical or physical properties of the sample. (Aflame-sealed quartz vial that is suitable for accommodating pressure resultingfrom radiolytic decomposition is generally considered to be an acceptable sample container.)7.2 Sample size shall be sufficient to perform the following:7.2.1 Assay and a
39、cceptance tests at the sellers plant,7.2.2 Assay and acceptance tests at the purchasers plant, and7.2.3 Referee tests in the event they become necessary.7.3 All samples shall be identified clearly, including the sellers lot number.7.3.1 A lot is defined as any quantity of aqueous plutonium nitrate s
40、olution that is uniform in isotopic, chemical, and physicalcharacteristics by virtue of having been mixed in such a manner as to be thoroughly homogeneous.7.3.2 All containers used for a lot shall be identified positively as containing material from a particular homogeneous solution.5 Reagent Chemic
41、als, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and Nation
42、alFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.6 The boldface numbers in parentheses refer to the list of references at the end of these test methods.C759 183PLUTONIUM BY CONTROLLED-POTENTIAL COULOMETRY(This test method was discontinued in 1992 and replaced by Test Method C11
43、65.)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 WITH IRON(II)(This test method was discontinued in 1992 and
44、 replaced by Test Method C1206.)TEST METHOD FOR PLUTONIUM ASSAY BY PLUTONIUM(III) DIODE ARRAY SPECTROPHOTOMETRY(With appropriate sample preparation, the measurement described in Test Method C1307 may be used for plutonium determi-nation.)FREE ACID BY TITRATION IN AN OXALATE SOLUTION8. Scope8.1 This
45、test method covers the determination of free acid in plutonium nitrate solutions (3, 4).8. Scope8.1 This test method covers the determination of free acid in plutonium nitrate solutions (3, 4).9. Summary of Test Method9.1 Free acid is determined by titrating an aliquot of sample, which contains an e
46、xcess of ammonium oxalate added to complexthe plutonium, back to the original pH of the ammonium oxalate solution with standard sodium hydroxide solution. Micropipetsand microburets are required to measure the small volume of sample and titrant used.10. Interferences10.1 Any metal ions not complexed
47、 by oxalate which form precipitates at the pH of the end point of the titration will causeinterference in this test method.NOTE 1A “rule of thumb” is that 1 mL of saturated ammonium oxalate solution will complex 6.4 mg of plutonium.11. Apparatus11.1 Magnetic Stirrer.11.2 Microburet.11.3 Micropipets.
48、11.4 pH Meter.12. Reagents and Materials12.1 Ammonium Oxalate Solution, saturated.12.2 Nitric Acid (3.50 N)Prepare solution by diluting concentrated nitric acid (HNO3, sp gr 1.42) with water. Standardize bytitrating 0.500-mL aliquots with 0.100 N NaOH solution.12.3 Sodium Hydroxide Solution (0.100 N
49、)Prepare and standardize in accordance with Practices E50.13. Procedure13.1 Transfer 1.0 mL of saturated ammonium oxalate solution to a small vial and dilute to about 2 mL with water.13.2 Add a stirring bar and insert the electrodes and start stirrer. When the pH value becomes stable, record the value as thepH of reagent.NOTE 2Normally, the pH value for the saturated solution is approximately 6.4.13.3 Add 20 L of sample to the vial, rinse the pipet thoroughly with water, and stir the solution for 1 min.13.4 Titrate with 0.100 N NaOH solution to within one pH uni
