1、Designation: C 889 06Standard Test Methods forChemical and Mass Spectrometric Analysis of Nuclear-Grade Gadolinium Oxide (Gd2O3) Powder1This standard is issued under the fixed designation C 889; the number immediately following the designation indicates the year oforiginal adoption or, in the case o
2、f 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.1. Scope1.1 These test m
3、ethods 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 Conductivity2C 1408 Test Method for Carb
4、on (Total) in Uranium OxidePowders and Pel lets By Direct Combustion-Infrared Detec-tion Method3Total Chlorine and Fluorine by Pyrohydrolysis IonSelective Electrode-Loss of Weight on Ignition 7-13Sulfur by CombustionIodometric Titration2Impurity Elements by a Spark-Source Mass Spectrographic2C 761 T
5、est Methods for Chemical, Mass Spectrometric,Spectrochemical,Nuclear, and Radiochemical Analysis ofUranium Hexafluoride3C 1287 Test Method for Determination of Impurities In Ura-nium Dioxide By Inductively Coupled Plasma Mass Spec-trometry3Gadolinium Content in Gadolinium Oxide by ImpurityCorrection
6、14-17C 1502 Test Method for Determination of Total Chlorine andFluorine in Uranium Dioxide and Gadolinium Oxide41.3 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 saf
7、ety 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 Standards:3C 761 Test Methods for Chemical, Mass Spectrometric,Spectrochemical, Nuclear, and Radiochemical Analysis ofUranium
8、 HexafluorideC 888 Specification for Nuclear-Grade Gadolinium Oxide(Gd2O3)PowderC 1287 Test Method for Determination of Impurities inNuclear Grade Uranium Compounds by InductivelyCoupled Plasma Mass SpectrometryC 1408 Test Method for Carbon (Total) in Uranium OxidePowders and Pellets By Direct Combu
9、stion-Infrared De-tection MethodC 1502 Test Method for Determination of Total Chlorineand Fluorine in Uranium Dioxide and Gadolinium OxideD 1193 Specification for Reagent Water3. Significance and Use3.1 Gadolinium oxide powder is used, with subsequentprocessing, in nuclear fuel applications, such as
10、 an addition touranium dioxide. These test methods are designed to determinewhether the material meets the requirements described inSpecification C 888.3.1.1 The material is analyzed to determine whether itcontains the minimum gadolinium oxide content specified.3.1.2 The loss on ignition and impurit
11、y content are deter-mined to ensure that the weight loss and the maximumconcentration limit of specified impurity elements are notexceeded.4. Reagents4.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to
12、the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.5Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determ
13、ination.1These test methods are under the jurisdiction of ASTM Committee C26 onNuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.05 onMethods of Test.Current edition approved Jan. 1, 2006. Published February 2006. Originallyapproved in 1978. Last previous edition approved in 19
14、99 as C 889 99.2Discontinued January 1999. See C 88990.3For 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.4Disco
15、ntinued March 2005. See C 88990.5“Reagent Chemicals, American Chemical Society Specifications,” Am. Chemi-cal Soc., Washington, DC. For suggestions on the testing of reagents not listed bytheAmerican Chemical Society, see “Reagent Chemicals and Standards,” by JosephRosin, D. Van Nostrand Co., Inc.,
16、New York, NY, and the “United StatesPharmacopeia.”1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water as definedin Specification
17、D 1193.5. Hazards5.1 Proper precautions should be taken to prevent inhalationor ingestion of gadolinium oxide powders or dust duringgrinding or handling operations.5.2 Workers should observe precautions as specified invendor supplied Material Safety Data Sheets (MSDS).6. Sampling6.1 Criteria for sam
18、pling this material are given in Specifi-cation C 888.CARBON BY DIRECT COMBUSTIONTHERMAL CONDUCTIVITYThis Test Method was discontinued in January 1999 andreplaced by C 1408TOTAL CHLORINE AND FLUORINE BYPYROHYDROLYSIS IONSELECTIVE ELECTRODEThis Test Method was discontinued in March 2005 andreplaced b
19、y C 1408LOSS OF WEIGHT ON IGNITION7. Scope7.1 This test method covers the loss-on-ignition of volatileconstituents from nuclear-grade gadolinium oxide (Gd2O3)powder.8. Summary of Test Method8.1 A weighed sample of gadolinium oxide is heated to aminimum of 900C for2hinair.Upon cooling, the sample isr
20、eweighed. The loss in weight is the difference between theinitial and final weight.9. Apparatus9.1 Combustion EquipmentA suitable muffle furnace ca-pable of heating 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.
21、 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 Gd2O3sample in a desiccator to roomtemperature.11.6 Remove the crucible from the desiccator and reweigh.12. Calculation12.1 Calculate the perce
22、nt 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 Gd2O3after heating, g, andW = sample mass, g of Gd2O3.13. Precision and Bias13.1 The relative standard deviation for measuring loss ofvolatile consti
23、tuents 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 bias is being made.SULFUR BY COMBUSTIONIODOMETRICTITRATIONThis Test Method was discontinued in January 1999.IMPURITY ELEMENTS BY A SPARK-SOUR
24、CE MASSSPECTROGRAPHIC METHODICP-AES as described in C761 or Inductively CoupledPlasma Mass Spectrometry (ICP-MS) described in C1287may be used to determine boron, cadmium, thorium,dysprosium, europium, samarium, terbium, andytterbium as impurity elements and other impurities.Powder must be analyzed
25、as-received (not ignited), andreported in g oxide per g gadolinium oxide to performimpurity calculations in sections 14-17GADOLINIUM CONTENT IN GADOLINIUM OXIDEBY IMPURITY CORRECTION METHOD14. Scope14.1 The percent gadolinium oxide content of powders,exclusive of volatiles, is determined by calculat
26、ion after thematerial has been analyzed to determine the total impurities.15. Summary of Test Method15.1 The total gadolinium content of gadolinium oxidepowders is determined by calculation after the sample has beenanalyzed by the following procedures:15.1.1 Loss of Weight on Ignition, Sections 7-13
27、.15.1.2 Impurity Elements by ICP-MS or ICP-AES, ele-ments as specified in C 88816. 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 u
28、sed as the concentration of thatelement in the following calculations.16.2 Calculate the percent gadolinium oxide as follows:G 5 100 2 IS! 1024! 1 ILI!100! (2)where:G = percent gadolinium oxideC889062IS= total g spectrographic impurities as oxides, per gramgadolinium oxide powder sample,ILI= gram lo
29、ss-on-ignition impurity per gram gadoliniumoxide powder sample,17. Precision 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 ta
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33、he address shown below.This standard is copyrighted by ASTM International, 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).C889063
