ASTM_F_1593_-_08.pdf

Designation:F159308Standard Test Method forTrace Metallic Impurities in Electronic Grade Aluminum byHigh Mass-Resolution Glow-Discharge Mass Spectrometer1This standard is issued under the fixed designation F1593;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 measuring the concentrations oftrace metallic impurities in high purity aluminum.1.2 This test method pertains to analysis by magnetic-sectorglow discharge mass spectrometer(GDMS).1.3 The aluminum matrix must be 99.9 weight%(3N-grade)pure,or purer,with respect to metallic impurities.Theremust be no major alloy constituent,for example,silicon orcopper,greater than 1000 weight ppm in concentration.1.4 This test method does not include all the informationneeded to complete GDMS analyses.Sophisticated computer-controlled laboratory equipment skillfully used by an experi-enced operator is required to achieve the required sensitivity.This test method does cover the particular factors(for example,specimen preparation,setting of relative sensitivity factors,determination of sensitivity limits,etc.)known by the respon-sible technical committee to affect the reliability of high purityaluminum analyses.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 MaterialsE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodE1257 Guide for Evaluating Grinding Materials Used forSurface Preparation in Spectrochemical Analysis3.Terminology3.1 Terminology in this test method is consistent withTerminology E135.Required terminology specific to this testmethod and not covered in Terminology E135 is indicatedbelow.3.2 campaigna series of analyses of similar specimensperformed in the same manner in one working session,usingone GDMS setup.As a practical matter,cleaning of the ionsource specimen cell is often the boundary event separatingone analysis campaign from the next.3.3 reference sample material accepted as suitable for useas a calibration/sensitivity reference standard by all partiesconcerned with the analyses.3.4 specimena suitably sized piece cut from a reference ortest sample,prepared for installation in the GDMS ion source,and analyzed.3.5 test sample material(aluminum)to be analyzed fortrace metallic impurities by this GDMS test method.Generallythe test sample is extracted from a larger batch(lot,casting)ofproduct and is intended to be representative of the batch.4.Summary of the Test Method4.1 A specimen is mounted as the cathode in a plasmadischarge cell.Atoms subsequently sputtered from the speci-men surface are ionized,and then focused as an ion beamthrough a double-focusing magnetic-sector mass separationapparatus.The mass spectrum,that is,the ion current,iscollected as magnetic field,or acceleration voltage is scanned,or both.4.2 The ion current of an isotope at mass Miis the totalmeasured current,less contributions from all other interferingsources.Portions of the measured current may originate fromthe ion detector alone(detector noise).Portions may be due toincompletely mass resolved ions of an isotope or molecule withmass close to,but not identical with,Mi.In all such instancesthe interfering contributions must be estimated and subtractedfrom the measured signal.1This test method is under the jurisdiction of ASTM Committee F01 onElectronics and is the direct responsibility of Subcommittee F01.17 on SputterMetallization.Current edition approved June 15,2008.Published July 2008.Originallyapproved in 1995.Last previous edition approved in 2002 as F1593 97(2002).DOI:10.1520/F1593-08.2For 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 4.2.1 If the source of interfering contributions to the mea-sured ion current at Micannot be determined unambiguously,the measured current less the interfering contributions fromidentified sources constitutes an upper bound of the detectionlimit for the current due to the isotope.4.3 The composition of the test specimen is calculated fromthe mass spectrum by applying a relative sensitivity factor(RSF(X/M)for each contam