ASTM_C_1508_-_01_2011.pdf

Designation:C150801(Reapproved 2011)Standard Test Method forDetermination of Bromine and Chlorine in UF6and UranylNitrate by X-Ray Fluorescence(XRF)Spectroscopy1This standard is issued under the fixed designation C1508;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 method covers the determination of bromine(Br)and chlorine(Cl)in uranium hexafluoride(UF6)and uranylnitrate solution.The method as written covers the determina-tion of bromine in UF6over the concentration range of 0.2 to8 g/g,uranium basis.The chlorine in UF6can be determinedover the range of 4 to 160 g/g,uranium basis.Higherconcentrations may be covered by appropriate dilutions.Thedetection limit for Br is 0.2 g/g uranium basis and for Cl is 4g/g uranium basis.1.2 This standard may involve hazardous materials,opera-tions and equipment.This standard does not purport to addressall of the safety concerns,if any,associated with its use.It isthe responsibility of the user of this standard to establishappropriate safety and health practices and determine theapplicability of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:2C761 Test Methods for Chemical,Mass Spectrometric,Spectrochemical,Nuclear,and Radiochemical Analysis ofUranium HexafluorideC787 Specification for Uranium Hexafluoride for Enrich-mentC788 Specification for Nuclear-Grade Uranyl Nitrate Solu-tion or CrystalsC1118 Guide for Selecting Components for Wavelength-Dispersive X-Ray Fluorescence(XRF)Systems(With-drawn 2011)3D1193 Specification for Reagent Water3.Summary of Test Method3.1 A sample of hydrolyzed UF6(uranyl fluoride)or uranylnitrate solution is treated with sodium nitrite to reduce oxidizedforms of bromine and chlorine(bromates and chlorates)to theirrespective halide ions.Addition of silver nitrate precipitates thesilver halides.Spike recoveries can be improved by theaddition of potassium iodide causing coprecipitation of thehalides.The halides are collected on filter paper and areanalyzed by X-ray fluorescence using two different crystal/detector systems.4.Significance and Use4.1 The method is designed to show whether or not thetested materials meet the specifications as given in Specifica-tions C787 and C788.5.Interferences5.1 Plastic equipment must be used throughout the methodfor uranyl fluoride as the hydrofluoric acid in the uranylfluoride leaches chloride from glassware causing a high bias.5.2 Low recoveries may occur as the precipitate can bedifficult to transfer quantitatively to the filter paper.A surfac-tant can be added(optional step)to minimize the adhesion ofthe precipitate to the walls of the beakers and the funnel.6.Apparatus6.1 X-Ray Spectrometer,see Guide C1118 for the selectionof the X-ray Spectrometer.6.2 Plastic Vacuum Filtration Apparatus,for 47 mm diam-eter filter paper.6.3 Filter Paper,0.45 micron,47 mm diameter.46.4 Beakers,polypropylene,250 mL.6.5 Stirring Rods,plastic or Teflon.6.6 X-ray Sample Support,Rings.Inner diameter approxi-mately 40 mm.1This test method is under the jurisdiction ofASTM Committee C26 on NuclearFuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods ofTest.Current edition approved June 1,2011.Published June 2011.Originallyapproved in 2001.Last previous edition approved in 2006 as C1508 01(2006).DOI:10.1520/C1508-01R1.2For 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.3The last approved version of this historical standard is referenced onwww.astm.org.4The filter must be Cl and Br free.Millipore membrane filter type HABP()has been successfully used.An alternate is 15A from S.C.B,BP6,RN86,07130 Soyons France.Any other equivalent is acceptable.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 7.Reagents7.1 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.5Other 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.7.2 Purity of WaterUnless otherwise indicated,referencesto water shall be understood to mean reagent water conformingto Specification D1193,Type I.7.3 Ammonium Hydroxide,NH4OH,concentrated,specificgravity 0.90.7.4 Ammonium Hydroxide Solution,1+3(3.7 M).Dilute 1part NH4OH with 3 parts water.7.5 Surfactant,bromine and chlorine free.6(Optional).7.6 Surfacta