ASTM_C_1342_-_96.pdf

Designation:C 1342 96Standard Practice forFlux Fusion Sample Dissolution1This standard is issued under the fixed designation C 1342;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(e)indicates an editorial change since the last revision or reapproval.1.Scope1.1 This practice covers flux fusion sample decompositionand dissolution for the determination of SiO2as well as manyother oxides in glasses,ceramics,and raw materials.Thesolutions are analyzed by atomic spectroscopy methods.Ana-lyte concentrations ranging from trace to major levels can bemeasured in these solutions,depending on the sample weightsand dilution volumes used during preparation.1.2 This standard does not purport to address all the safetyconcerns,if any,associated with its use.It is the responsibilityof the user of this standard to establish appropriate safety andhealth practices and determine the applicability of regulatorylimitations prior to use.Specific precautionary statements aregiven in Section 8.2.Referenced Documents2.1 ASTM Standards:C 1109 Test Method for Analysis of Aqueous Leachatesfrom Nuclear Waste Materials Using Inductively CoupledPlasma-Atomic Emission Spectrometry2C 1111 Test Method for Determining Elements in WasteStreams by Inductively Coupled Plasma-Atomic EmissionSpectroscopy2C 1220 Test Method for Static Leaching of MonolithicWaste Forms for Disposal of Radioactive Waste2C 1285 Test Methods for Determining Chemical Durabilityof Nuclear Waste Glasses:The Product Consistency Test(PCT)2C 1317 Practice for Dissolution of Silicate orAcid ResistantMatrix Samples2D 1193 Specifications for Reagent Water33.Summary of Practice3.1 A ground sample is weighed into a platinum crucible,and an appropriate amount of alkaline flux(Na2CO3andNa2B4O7)is added.The mixture is fused in a muffle furnace(950C for 25 min),cooled to room temperature,dissolvedwith hydrochloric acid,and diluted to an appropriate volumefor subsequent analysis.3.2 With appropriate sample preparation,the solution result-ing from this procedure can be analyzed for trace metals byinductively coupled plasma-atomic emission spectroscopy(ICP-AES),inductively coupled plasma-mass spectrometry(ICP-MS),and flame atomic absorption spectroscopy.4.Significance and Use4.1 This practice describes a method for fusing and dissolv-ing silicate and refractory matrix samples for subsequentanalysis for trace metals and radionuclides.Glass vitrificationplant feeds and product can be characterized using thisdissolution method,followed by the appropriate analysis of theresulting solutions as described in Test Methods C 1109 andC 1111.4.2 This practice has been used to analyze round robinsimulated nuclear waste glass samples.4.3 This practice can be used for bulk analysis of glasssamples as described in Test Methods C 1220 and C 1285.4.4 This practice is a companion to Practice C 1317.Theseprocedures can be used to dissolve borosilicate glasses con-taining nuclear wastes for subsequent analysis.5.Technical Precautions5.1 This procedure is not useful for the determination ofboron or sodium since these elements are contained in the fluxmaterial.5.2 The user is cautioned that with analysis by ICP emis-sion,flame atomic absorption,and ICP-MS,the high sodiumconcentrations from the flux may cause interferences.5.3 Elements that form volatile species under these alkalinefusion conditions may be lost during the fusion process(that is,As and Sb).6.Apparatus6.1 Platinum Crucibles,30 mL.6.2 Balance,analytical type,precision to 0.1 mg.6.3 Furnace,with heating capacity to 1000C.6.4 Crucible Tongs(cannot be made of iron,unless usingplatinum-clad tips).6.5 Polytetrafluoroethylene(PTFE)Beaker,125-mL capac-ity.6.6 Magnetic Stir Bar,PTFE-coated(0.32 to 0.64 cm).6.7 Magnetic Stirrer.6.8 Mortar and Pestle,agate or alumina(or equivalentgrinding apparatus).6.9 Sieves,100 mesh.1This practice is under the jurisdiction of ASTM Committee C-26 on NuclearFuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods ofTest.Current edition approved July 10,1996.Published September 1996.2Annual Book of ASTM Standards,Vol 12.01.3Annual Book of ASTM Standards,Vol 11.01.1AMERICAN SOCIETY FOR TESTING AND MATERIALS100 Barr Harbor Dr.,West Conshohocken,PA 19428Reprinted from the Annual Book of ASTM Standards.Copyright ASTMNOTICE:Thisstandardhaseitherbeensupersededandreplacedbyanewversionordiscontinued.ContactASTMInternational(www.astm.org)forthelatestinformation.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.47.2 Purity of WaterUnless otherwise indicated,referencesto water shall be understood to mean at least Type II reagentwater in c