ASTM_E_2465_-_13.pdf

Designation:E246513Standard Test Method forAnalysis of Ni-Base Alloys by Wavelength Dispersive X-RayFluorescence Spectrometry1This standard is issued under the fixed designation E2465;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 test method covers the analysis of Ni-base alloysby wavelength dispersive X-ray Fluorescence Spectrometry forthe determination of the following elements:ElementComposition RangeManganese0.06%to 1.6%Phosphorus0.008%to 0.015%Silicon0.08%to 0.6%Chromium1.6%to 22%Nickel23%to 77%Aluminum0.20%to 1.3%Molybdenum0.03%to 10%Copper0.007%to 2.5%Titanium0.11%to 3.0%Niobium0.55%to 5.3%Iron0.17%to 46%Tungsten0.06%to 0.50%Cobalt0.04%to 0.35%NOTE1Unless exceptions are noted,concentration ranges can beextended by the use of suitable reference materials.Once these elementranges are extended they must be verified by some experimental means.This could include but not limited to Gage Repeatability and Reproduc-ibility studies and/or Inter-laboratory Round Robin studies.Once thesestudies are completed,they will satisfy the ISO 17025 requirements forcapability.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 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 to determine theapplicability of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:2E135 Terminology Relating to Analytical Chemistry forMetals,Ores,and Related MaterialsE305 Practice for Establishing and Controlling AtomicEmission Spectrochemical Analytical CurvesE1361 Guide for Correction of Interelement Effects inX-Ray Spectrometric AnalysisE1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical MethodE1622 Practice for Correction of Spectral Line Overlap inWavelength-Dispersive X-Ray Spectrometry(Withdrawn2006)32.2 Other Documents:ISO 17025 General requirements for the competence oftesting and calibration laboratories2.3 U.S.Government Standards:410 CFR Part 19 Notices,Instructions and Reports to Work-ers:Inspection and Investigations10 CFR Part 20 Standards for Protection Against Radiation3.Terminology3.1 DefinitionsFor definitions of terms used in this testmethod,refer to Terminology E135.4.Summary of Test Method4.1 The test specimen is finished to a clean,uniform surface,then irradiated with an X-ray beam of high energy.Thesecondary X-rays produced are dispersed by means of crystalsand the intensities are measured by suitable detectors atselected wavelengths.The outputs of the detectors in voltagepulses are counted.Radiation measurements are made based onthe time required to reach a fixed number of counts,or on thetotal counts obtained for a fixed time(generally expressed incounts or kilocounts per unit time).4.2 Concentrations of the elements are determined by relat-ing the measured radiation of unknown specimens to analyticalcurves prepared with suitable reference materials.Either afixed-channel(simultaneous)spectrometer or a sequential1This test method is under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals,Ores,and Related Materials and is the directresponsibility of Subcommittee E01.08 on Ni and Co and High TemperatureAlloys.Current edition approved June 1,2013.Published July 2013.Originally approvedin 2006.Last previous edition approved in 2011 as E2465 111.DOI:10.1520/E2465-13.2For 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.3The last approved version of this historical standard is referenced onwww.astm.org.4Available from the U.S.Nuclear Regulatory Commission,Public DocumentRoom,One White Flint North,11555 Rockville Pike,Rockville,MD 20852-2738,http:/www.nrc.gov.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 spectrometer,or an instrument combining both fixed-channelsand one or more goniometers shall be used.5.Significance and Use5.1 This procedure is suitable for manufacturing control andfor verifying that the product meets specifications.It providesrapid,multi-element determinations with sufficient accuracy toassure product quality.The analytical performance data in-cluded may be used as a benchmark to determine if similarX-ray spectrometers provide equivalent precision andaccuracy,or if the performance of a particular spectrometer haschanged.6.Interferences6.1 Interelement effects,or matrix effects,exist fo