ASTM_C_1605_-_04_2014.pdf

Designation:C160504(Reapproved 2014)Standard Test Methods forChemical Analysis of Ceramic Whiteware Materials UsingWavelength Dispersive X-Ray Fluorescence Spectrometry1This standard is issued under the fixed designation C1605;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 These test methods cover the determination of ten majorelements(SiO2,Al2O3,Fe2O3,MgO,CaO,Na2O,K2O,TiO2,P2O5,MnO,and LOI in ceramic whitewares clays and mineralsusing wavelength dispersive X-ray fluorescence spectrometry(WDXRF).The sample is first ignited,then fused with lithiumtetraborate and the resultant glass disc is introduced into awavelength dispersive X-ray spectrometer.The disc is irradi-ated with X-rays from an X-ray tube.X-ray photons emitted bythe elements in the samples are counted and concentrationsdetermined using previously prepared calibration standards.(1)2In addition to 10 major elements,the method provides agravimetric loss-on-ignition.NOTE1Much of the text of this test method is derived directly fromMajor element analysis by wavelength dispersive X-ray fluorescencespectrometry,included in Ref(1).1.2 Interferences,with analysis by WDXRF,may resultfrom mineralogical or other structural effects,line overlaps,and matrix effects.The structure of the sample,mineralogicalor otherwise,is eliminated through fusion with a suitable flux.Fusion of the sample diminishes matrix effects and produces astable,flat,homogeneous sample for presentation to thespectrometer.Selecting certain types of crystal monochroma-tors eliminates many of the line overlaps and multiorder lineinterferences.A mathematical correction procedure(2)is usedto correct for the absorption and enhancement matrix effects.1.3 Concentrations of the elements in clays and minerals aredetermined independent of the oxidation state and are reportedin the oxidation state in which they most commonly occur inthe earths crust.1.4 Concentration ranges:ElementConcentration range(percent)SiO20.1099.0Al2O30.1058.0Fe2O30.0428.0MgO0.1060.0CaO0.0260.0Na2O0.1530.0K2O0.0230.0TiO20.0210.0P2O50.0550.0MnO0.0115.0LOI(925C)0.01100.01.5 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 safety and health practices and determine the applica-bility of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:3C242 Terminology of Ceramic Whitewares and RelatedProductsC322 Practice for Sampling Ceramic Whiteware ClaysC323 Test Methods for Chemical Analysis of CeramicWhiteware Clays3.Apparatus3.1 Simultaneous X-ray Spectrometer,for example,PhilipsPW1606 or equivalent.3.2 Pt-Au Alloy Crucibles and Molds,(3).3.3 Fluxer,(4)or equivalent).3.4 Two Muffle Furnaces with Rocker AttachmentsAmuffle furnace is not required if the fluxer has automaticoperation with its own heat source.3.5 Hot Plate and Muffle Furnace.1These test methods are under the jurisdiction of ASTM Committee C21 onCeramic Whitewares and Related Productsand are the direct responsibility ofSubcommittee C21.03 on Methods for Whitewares and Environmental Concerns.Current edition approved Dec.1,2014.Published December 2014.Originallyapprovedin2004.Lastpreviouseditionapprovedin2009asC1605 04(2009).DOI:10.1520/C1605-04R14.2The boldface numbers in parentheses refer to the list of references at the end ofthis standard.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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 4.Reagents4.1 Digest the samples in Johnson Matthey Spectroflux 1004or equivalent brand(lithium tetraborate).A blend of lithiumtetraborate(Spectroflux 1004)and lithium metaborate(Spec-troflux 100A4)can be used if a lower fusion point is desired.The flux is ordered in powdered form,lot size as appropriate,and identified by number and date.4.2 Dry the minus 60-mesh material for the lot 2 days at300C and keep in sealed Mason jars.4.3 After drying,perform a loss-on-fusion for each lot offlux from the manufacturer so that an appropriate amount offlux can be weighed out to yield 8.0000 g of lithium tetraborateafter fusion.4.4 Weigh the charges of flux using a Zymark5robot to60.0035 g(60.04%precision).If the Zymark5robot is notavailable the samples can be weighed by hand.4.5 Clean the platinum ware in 50 percent reagent gradeHCl,rinse in deionized water and dry at 140C.Other acidsmay be used instead of HCl,depending on the preference of thelaboratory.4.6 Prepare the LiBr used as a nonwetting agent by neut