ASTM_E_1621_-_13.pdf

Designation:E162113Standard Guide forElemental Analysis by Wavelength Dispersive X-RayFluorescence Spectrometry1This standard is issued under the fixed designation E1621;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 guide provides guidelines for developing anddescribing analytical procedures using a wavelength dispersiveX-ray spectrometer for elemental analysis of solid metals,ores,and related materials.Material forms discussed herein includesolids,powders,and solid forms prepared by chemical andphysical processes such as borate fusion and pressing ofbriquettes.1.2 Liquids are not discussed in this guide because they aremuch less frequently encountered in metals and mining labo-ratories.However,aqueous liquids can be processed by boratefusion to create solids specimens,and X-ray spectrometers canbe equipped to handle liquids directly.1.3 Some provisions of this guide may be applicable to theuse of an energy dispersive X-ray spectrometer.1.4 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.5 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:2E135 Terminology Relating to Analytical Chemistry forMetals,Ores,and Related MaterialsE1257 Guide for Evaluating Grinding Materials Used forSurface Preparation in Spectrochemical AnalysisE1329 Practice for Verification and Use of Control Charts inSpectrochemical AnalysisE1361 Guide for Correction of Interelement Effects inX-Ray Spectrometric AnalysisE1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical MethodE2857 Guide for Validating Analytical Methods3.Terminology3.1 DefinitionsFor definitions of terms used in this guide,refer to Terminologies E135 and the terminology section ofE1361.4.Summary of Guide4.1 Important aspects of test equipment for wavelengthdispersive X-ray fluorescence spectrometry are discussed in-cluding equipment components and accessories,reagents,andmaterials.Key aspects of the application of X-ray spectrometryto materials analysis are discussed including interferences andcorrection options,specimen preparation by a variety ofprocedures,and materials and accessories for presentation ofspecimens for measurement in spectrometers.Key elements ofmeasurement procedures,calibrations procedures,and resultreporting are explained.4.2 In an X-ray spectrometric test method,the test specimenis prepared with a clean,uniform,flat surface.It may beprepared by grinding,polishing,or lathing a metal surface orby fusing or briquetting a powder.This surface is irradiatedwith a primary source of X-rays.The secondary X-raysproduced in the specimen are dispersed according to theirwavelength by means of crystals or synthetic multilayers.Theircount rates at selected wavelengths,hereinafter calledintensities,are measured by suitable detector systems.Amounts of the elements are determined from the measuredintensities using analytical curves prepared with suitable cali-brants.4.3 Important aspects of background estimation are coveredin an appendix to the guide.5.Significance and Use5.1 X-ray fluorescence spectrometry can provide an accu-rate and precise determination of metallic and many non-metallic elements in a wide variety of solid and liquid1This guide is under the jurisdiction of ASTM Committee E01 on AnalyticalChemistry for Metals,Ores,and Related Materials and is the direct responsibility ofSubcommittee E01.20 on Fundamental Practices.Current edition approved Oct.1,2013.Published November 2013.Originallyapproved in 1994.Last previous edition approved in 2005 as E1621 05.DOI:10.1520/E1621-13.2For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 materials.This guide covers the information that should beincluded in an X-ray spectrometric analytical method andprovides direction to the analyst for determining the optimumconditions needed to achieve acceptable accuracy.5.2 The accuracy of a determination is a function of thecalibration scheme,the sample preparation,and the samplehomogeneity.Close attention to all aspects of these areas isnecessary to achieve acceptable results.5.3 All concepts discussed in this guide are explored indetail in a number of