ASTM_C_1110_-_03_2008.pdf

Designation:C 1110 03(Reapproved 2008)Standard Practice forSample Preparation for X-Ray Emission SpectrometricAnalysis of Uranium in Ores Using the Glass Fusion orPressed Powder Method1This standard is issued under the fixed designation C 1110;the number immediately following the designation indicates the year 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 This practice covers the preparation of uranium oresamples to be analyzed by X-ray emission.Two separatetechniques,the glass fusion method or the pressed powdermethod,may be used.1.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.3 This standard does not purport to address all of thesafety problems,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.2.Referenced Documents2.1 ASTM Standards:2E 50 Practices for Apparatus,Reagents,and Safety Consid-erations for Chemical Analysis of Metals,Ores,andRelated MaterialsE 135 Terminology Relating to Analytical Chemistry forMetals,Ores,and Related Materials3.Terminology3.1 Definitions:Refer to Terminology E 135 for terms usedin this practice.4.Summary of Practice4.1 Two types of specimen preparation methods are offered.These are the glass fusion technique and the pressed powdertechnique.The glass fusion specimens are fused and cast intodisks in a platimum-gold alloy crucible in the presence of anoxidizing agent at a preset temperature and time.The pressedpowder specimens are ground in a mill to a specified particlesize and briquetted into a solid specimen possessing a flathomogeneous surface to be analyzed.5.Significance and Use5.1 This practice is useful for the preparation of specimensof ore bodies for the analysis of uranium by X-ray emission.Two separate preparation techniques are described.6.Apparatus6.1 Platimum-Gold Crucible,95%platinum 5%gold,withflat 32-mm diameter bottom.6.2 Muffle Furnace,1200C capacity with controller of610C resolution,or fusion apparatus with similar capabili-ties.NOTE1A fusion apparatus may be substituted for the muffle furnacethroughout this practice.If such is used,follow the manufacturersoperating instructions.6.3 Rotary Swing Mill,with tungsten or boron carbide vials.6.4 Pellet Die,32-mm diameter.6.5 Hydraulic Press,25-ton capacity.6.6 Crucible,porcelain,Coors,30-mL capacity.6.7 Refractory Brick,60 to 70%alumina firebrick.6.8 Analytical Balance,accurate to 60.001 g.7.Reagents and Materials7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society,wheresuch specifications are available.3Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination(see Practices E 50).7.2 Lithium Tetraborate(Li2B4O7),anhydrous,spectro-graphic grade.1This practice is under the jurisdiction of ASTM Committee C26 on NuclearFuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods ofTest.Current edition approved Dec.1,2008.Published January 2009.Originallyapproved in 1988.Last previous edition approved in 2003 as C 1110 03.2For 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.3Reagent Chemicals,American Chemical Society Specifications,AmericanChemical Society,Washington,DC.For Suggestions on the testing of reagents notlisted by the American Chemical Society,see Annual Standards for LaboratoryChemicals,BDH Ltd.,Poole,Dorset,U.K.,and the United States Pharmacopeiaand National Formulary,U.S.Pharmacopeial Convention,Inc.(USPC),Rockville,MD.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.Copyright by ASTM Intl(all rights reserved);Thu Apr 16 08:27:09 EDT 2009Downloaded/printed byLaurentian University pursuant to License Agreement.No further reproductions authorized.7.3 Oxidizing Agent,ammonium nitrate(NH4NO3).7.4 Ethanol,anhydrous.7.5 Binding Agent,for example,pelletizing grade graphitepowder,cellulose powder,“Somar Mix,”or equivalent.7.6 Boric Acid,99.9%pure.8.Preparation of Standards and Specimens8.1 Glass Fusion Method:8.1.1 Ignition Loss of Lithium Tetraborate:NOTE2Commercially availabe fused and ground lithium tetraboratemay be used,and only the 105C drying step is required.8.1.1.1 Heat a 95%platinum/5%gold crucible in a mufflefurnace at 1100C for at lea