1、Designation: C889 11C889 18Standard Test Methods forChemical and Mass Spectrometric Analysis of Nuclear-Grade Gadolinium Oxide (Gd2O3) Powder1This standard is issued under the fixed designation C889; the number immediately following the designation indicates the year oforiginal adoption or, in the c
2、ase 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 U.S. Department of Defense.1. Scope1.1 The
3、se test methods cover procedures for the chemical and mass spectrometric analysis of nuclear-grade gadolinium oxidepowders to determine compliance with specifications.1.2 The analytical procedures appear in the following order:SectionsCarbon by Direct CombustionThermal Conductivity 2C1408 Test Metho
4、d for Carbon (Total) in Uranium OxidePowders and Pellets By Direct Combustion-InfraredDetection Method3C1408 Test Method for Carbon (Total) in Uranium OxidePowders and Pellets By Direct Combustion-InfraredDetection Method3Total Chlorine and Fluorine by Pyrohydrolysis IonSelective Electrode4C1502 Tes
5、t Method for Determination of Total Chlorine andFluorine in Uranium Dioxide and Gadolinium Oxide3C1502 Test Method for Determination of Total Chlorine andFluorine in Uranium Dioxide and Gadolinium Oxide3Loss of Weight on Ignition 7 13Loss of Weight on Ignition 8 14Sulfur by CombustionIodometric Titr
6、ation 5Impurity Elements by a Spark-Source Mass SpectrographicMethodC761 Test Methods for Chemical, Mass Spectrometric,Spectrochemical,Nuclear, and Radiochemical Analysis ofUranium Hexafluoride3C761 Test Methods for Chemical, Mass Spectrometric,Spectrochemical, Nuclear, and Radiochemical Analysis of
7、Uranium Hexafluoride3C1287 Test Method for Determination of Impurities InUranium Dioxide By InductivelyCoupled Plasma Mass Spectrometry3C1287 Test Method for Determination of Impurities inNuclear Grade Uranium Compounds by InductivelyCoupled Plasma Mass Spectrometry3Gadolinium Content in Gadolinium
8、Oxide by ImpurityCorrection14 17Gadolinium Content in Gadolinium Oxide by ImpurityCorrection Method15 181.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1 These test methods are under the jurisdiction of ASTM Committee C26
9、on Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 on Methodsof Test.Current edition approved June 1, 2011Feb. 1, 2018. Published June 2011February 2018. Originally approved in 1978. Last previous edition approved in 20062011 asC889 06.C889 11. DOI: 10.1520/C0889-11.10.15
10、20/C0889-18.2 Discontinued January 1999. See C889C1408903 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.4 Dis
11、continued March 2005. See C1408C1502.5 Discontinued March 2005.January 1999. See C889C889 90.90.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 po
12、ssible 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,
13、West Conshohocken, PA 19428-2959. United States11.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determ
14、ine theapplicability of regulatory limitations prior to use. For specific hazard statements, see Section 56.1.5 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of Intern
15、ational Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:3C761 Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of UraniumHexafluorideC8
16、59 Terminology Relating to Nuclear MaterialsC888 Specification for Nuclear-Grade Gadolinium Oxide (Gd2O3) PowderC1287 Test Method for Determination of Impurities in Nuclear Grade Uranium Compounds by Inductively Coupled PlasmaMass SpectrometryC1408 Test Method for Carbon (Total) in Uranium Oxide Pow
17、ders and Pellets By Direct Combustion-Infrared Detection MethodC1502 Test Method for Determination of Total Chlorine and Fluorine in Uranium Dioxide and Gadolinium OxideD1193 Specification for Reagent Water3. Terminology3.1 Definitions:3.1.1 For definitions of terms relating to the nuclear fuel cycl
18、e, refer to Terminology C859.4. Significance and Use4.1 Gadolinium oxide powder is used, with subsequent processing, in nuclear fuel applications, such as an addition to uraniumdioxide. These test methods are designed to determine whether the material meets the requirements described in Specificatio
19、nC888.4.1.1 The material is analyzed to determine whether it contains the minimum gadolinium oxide content specified.4.1.2 The loss on ignition and impurity content are determined to ensure that the weight loss and the maximum concentrationlimit of specified impurity elements are not exceeded.5. Rea
20、gents5.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, wheresuch specifications are available.6 Other grad
21、es may be used, provided it is first ascertained that the reagent is of sufficiently highpurity to permit its use without lessening the accuracy of the determination.5.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean reagent water as defined inSpecificatio
22、n D1193.6. Hazards6.1 Proper precautions should be taken to prevent inhalation or ingestion of gadolinium oxide powders or dust during grindingor handling operations.6.2 Workers should observe precautions as specified in vendor supplied Material Safety Data Sheets (MSDS).7. Sampling7.1 Criteria for
23、sampling this material are given in Specification C888.6 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 Standards for Laboratory Chemicals, BDH L
24、td., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.C889 182CARBON BY DIRECT COMBUSTIONTHERMAL CONDUCTIVITYThis Test Method was discontinued in January 1999 and replaced by C1408TOTAL CHLORINE AND FLUORINE BY P
25、YROHYDROLYSIS IONSELECTIVE ELECTRODEThis Test Method was discontinued in March 2005 and replaced by C1502LOSS OF WEIGHT ON IGNITION7. Scope7.1 This test method covers the loss-on-ignition of volatile constituents from nuclear-grade gadolinium oxide (Gd2O3) powder.8. Scope8.1 This test method covers
26、the loss-on-ignition of volatile constituents from nuclear-grade gadolinium oxide (Gd2O3) powder.9. Summary of Test Method9.1 A weighed sample of gadolinium oxide is heated to a minimum of 900C for 2 h in air. Upon cooling, the sample isreweighed. The loss in weight is the difference between the ini
27、tial and final weight.10. Apparatus10.1 Combustion EquipmentA suitable muffle furnace capable of heating to 1000C.10.2 Crucible, ceramic, nickel, or platinum with a 10-g capacity.10.3 Desiccator.10.4 Balance.11. Reagent11.1 Drying Desiccant.12. Procedure12.1 Heat the furnace to 925 6 25C.12.2 Weigh
28、5 g of Gd2O3 to the nearest 1 mg.12.3 Insert the crucible into the furnace.12.4 Heat for 2 h.12.5 Cool the Gd2O3 sample in a desiccator to room temperature.12.6 Remove the crucible from the desiccator and reweigh.13. Calculation13.1 Calculate the percent weight loss as follows:Percent weight loss5A
29、2B!100!/W (1)where:A = weight of crucible plus Gd2O3 before heating, g,B = weight of crucible plus Gd2O3 after heating, g, andW = sample mass, g of Gd2O3.14. Precision and Bias14.1 The relative standard deviation for measuring loss of volatile constituents on ignition is 1%.14.2 Since there is no ac
30、cepted reference material suitable for determining bias for the procedure in this test method, nostatement on bias is being made.C889 183SULFUR BY COMBUSTIONIODOMETRICTITRATIONThis Test Method was discontinued in January 1999.IMPURITY ELEMENTS BY A SPARK-SOURCE MASSSPECTROGRAPHIC METHODICP-AES as de
31、scribed in C761 or Inductively Coupled Plasma Mass Spectrometry (ICP-MS) described in C1287 maybe used to determine boron, cadmium, thorium, dysprosium, europium, samarium, terbium, and ytterbium as impurityelements and other impurities. Powder must be analyzed as-received (not ignited), and reporte
32、d in g oxide per g gado-linium oxide to perform impurity calculations in sections 1415 1718GADOLINIUM CONTENT IN GADOLINIUM OXIDEBY IMPURITY CORRECTION METHOD14. Scope14.1 The percent gadolinium oxide content of powders, exclusive of volatiles, is determined by calculation after the materialhas been
33、 analyzed to determine the total impurities.15. Scope15.1 The percent gadolinium oxide content of powders, exclusive of volatiles, is determined by calculation after the materialhas been analyzed to determine the total impurities.16. Summary of Test Method16.1 The total gadolinium content of gadolin
34、ium oxide powders is determined by calculation after the sample has been analyzedby the following procedures:16.1.1 Loss of Weight on Ignition, Sections 78 1314.16.1.2 Impurity Elements by ICP-MS or ICP-AES, elements as specified in Specification C888.17. Calculation17.1 If the concentration of an i
35、mpurity element is a“ less-than”a “less-than” (), (that is, a concentration expressed as beingless than the lower detection limit of the analytical method), this less-than value shall be used as the concentration of that elementin the following calculations.17.2 Calculate the percent gadolinium oxid
36、e as follows:G 51002IS! 1024!1ILI!100! (2)where:G = percent gadolinium oxideIS = total g spectrographic impurities as oxides, per gram gadolinium oxide powder sample,ILI = gram loss-on-ignition impurity per gram gadolinium oxide powder sample,18. Precision and Bias18.1 Since this is a calculation, p
37、recision and bias will depend upon relative standard deviation of the individual impuritiesanalyzed. Therefore, no statement on precision and bias is being made.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this sta
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