1、Designation: C889 11Standard 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 case of
2、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 These test meth
3、ods cover procedures for the chemicaland mass spectrometric analysis of nuclear-grade gadoliniumoxide powders to determine compliance with specifications.1.2 The analytical procedures appear in the following order:SectionsCarbon by Direct CombustionThermal Conductivity2C1408 Test Method for Carbon (
4、Total) in Uranium OxidePowders and Pellets By Direct Combustion-Infrared Detec-tion Method3Total Chlorine and Fluorine by Pyrohydrolysis IonSelective Electrode4C1502 Test Method for Determination of Total Chlorine andFluorine in Uranium Dioxide and Gadolinium Oxide5Loss of Weight on Ignition 7-13Sul
5、fur by CombustionIodometric Titration2Impurity Elements by a Spark-Source Mass Spectrographic2C761 Test Methods for Chemical, Mass Spectrometric, Spec-trochemical,Nuclear, and Radiochemical Analysis of UraniumHexafluoride3C1287 Test Method for Determination of Impurities In Ura-nium Dioxide By Induc
6、tively Coupled Plasma Mass Spec-trometry3Gadolinium Content in Gadolinium Oxide by ImpurityCorrection14-171.3 The values stated in SI 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 concern
7、s, if any, associated with its use. It is theresponsibility 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 specific hazardstatements, see Section 5.2. Referenced Documents2.1 ASTM Standar
8、ds:3C761 Test Methods for Chemical, Mass Spectrometric,Spectrochemical, Nuclear, and Radiochemical Analysis ofUranium HexafluorideC888 Specification for Nuclear-Grade Gadolinium Oxide(Gd2O3) PowderC1287 Test Method for Determination of Impurities inNuclear Grade Uranium Compounds by InductivelyCoupl
9、ed Plasma Mass SpectrometryC1408 Test Method for Carbon (Total) in Uranium OxidePowders and Pellets By Direct Combustion-Infrared De-tection MethodC1502 Test Method for Determination of Total Chlorineand Fluorine in Uranium Dioxide and Gadolinium OxideD1193 Specification for Reagent Water3. Signific
10、ance and Use3.1 Gadolinium oxide powder is used, with subsequentprocessing, in nuclear fuel applications, such as an addition touranium dioxide. These test methods are designed to determinewhether the material meets the requirements described inSpecification C888.3.1.1 The material is analyzed to de
11、termine whether itcontains the minimum gadolinium oxide content specified.3.1.2 The loss on ignition and impurity content are deter-mined to ensure that the weight loss and the maximumconcentration limit of specified impurity elements are notexceeded.1These test methods are under the jurisdiction of
12、 ASTM Committee C26 onNuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 onMethods of Test.Current edition approved June 1, 2011. Published June 2011. Originallyapproved in 1978. Last previous edition approved in 2006 as C889 06. DOI:10.1520/C0889-11.2Discontinued January 19
13、99. See C88990.3For 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.4Discontinued March 2005. See C1408.5Discontin
14、ued March 2005. See C88990.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4. Reagents4.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform
15、to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.6Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the det
16、ermination.4.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water as definedin Specification D1193.5. Hazards5.1 Proper precautions should be taken to prevent inhalationor ingestion of gadolinium oxide powders or dust duringgrinding or handling op
17、erations.5.2 Workers should observe precautions as specified invendor supplied Material Safety Data Sheets (MSDS).6. Sampling6.1 Criteria for sampling this material are given in Specifi-cation C888.CARBON BY DIRECT COMBUSTIONTHERMAL CONDUCTIVITYThis Test Method was discontinued in January 1999 andre
18、placed by C1408TOTAL CHLORINE AND FLUORINE BYPYROHYDROLYSIS IONSELECTIVE ELECTRODEThis Test Method was discontinued in March 2005 andreplaced by C1502LOSS OF WEIGHT ON IGNITION7. Scope7.1 This test method covers the loss-on-ignition of volatileconstituents from nuclear-grade gadolinium oxide (Gd2O3)
19、powder.8. Summary of Test Method8.1 A weighed sample of gadolinium oxide is heated to aminimum of 900C for2hinair.Upon cooling, the sample isreweighed. The loss in weight is the difference between theinitial and final weight.9. Apparatus9.1 Combustion EquipmentA suitable muffle furnace ca-pable of h
20、eating to 1000C.9.2 Crucible, ceramic, nickel, or platinum with a 10-gcapacity.9.3 Desiccator.9.4 Balance.10. Reagent10.1 Drying Desiccant.11. Procedure11.1 Heat the furnace to 925 6 25C.11.2Weigh5gofGd2O3to the nearest 1 mg.11.3 Insert the crucible into the furnace.11.4 Heat for 2 h.11.5 Cool the G
21、d2O3sample in a desiccator to roomtemperature.11.6 Remove the crucible from the desiccator and reweigh.12. Calculation12.1 Calculate the percent weight loss as follows:Percent weight loss 5 A 2 B!100! / W (1)where:A = weight of crucible plus Gd2O3before heating, g,B = weight of crucible plus Gd2O3af
22、ter heating, g, andW = sample mass, g of Gd2O3.13. Precision and Bias13.1 The relative standard deviation for measuring loss ofvolatile constituents on ignition is 1%.13.2 Since there is no accepted reference material suitablefor determining bias for the procedure in this test method, nostatement on
23、 bias is being made.SULFUR BY COMBUSTIONIODOMETRICTITRATIONThis Test Method was discontinued in January 1999.IMPURITY ELEMENTS BY A SPARK-SOURCE MASSSPECTROGRAPHIC METHODICP-AES as described in C761 or Inductively CoupledPlasma Mass Spectrometry (ICP-MS) described in C1287may be used to determine bo
24、ron, cadmium, thorium,dysprosium, europium, samarium, terbium, andytterbium as impurity elements and other impurities.Powder must be analyzed as-received (not ignited), andreported in g oxide per g gadolinium oxide to performimpurity calculations in sections 14-17GADOLINIUM CONTENT IN GADOLINIUM OXI
25、DEBY IMPURITY CORRECTION METHOD14. Scope14.1 The percent gadolinium oxide content of powders,exclusive of volatiles, is determined by calculation after thematerial has been analyzed to determine the total impurities.15. Summary of Test Method15.1 The total gadolinium content of gadolinium oxidepowde
26、rs is determined by calculation after the sample has beenanalyzed by the following procedures:15.1.1 Loss of Weight on Ignition, Sections 7-13.6Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted
27、by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.C889 11215.1.2 Impurity Elements by ICP-MS or ICP-AES, ele-ments as specif
28、ied in C88816. Calculation16.1 If the concentration of an impurity element is a“less-than” (), (that is, a concentration expressed as being lessthan the lower detection limit of the analytical method), thisless-than value shall be used as the concentration of thatelement in the following calculation
29、s.16.2 Calculate the percent gadolinium oxide as follows:G 5 100 2 IS! 1024! 1 ILI!100! (2)where:G = percent gadolinium oxideIS= total g spectrographic impurities as oxides, per gramgadolinium oxide powder sample,ILI= gram loss-on-ignition impurity per gram gadoliniumoxide powder sample,17. Precisio
30、n and Bias17.1 Since this is a calculation, precision and bias willdepend upon relative standard deviation of the individualimpurities analyzed. Therefore, no statement on precision andbias is being made.ASTM International takes no position respecting the validity of any patent rights asserted in co
31、nnection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the respo
32、nsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful
33、 consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International,
34、100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).C889 113
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