ASTM_F_1710_-_08.pdf

Designation:F171008Standard Test Method forTrace Metallic Impurities in Electronic Grade Titanium byHigh Mass-Resolution Glow Discharge Mass Spectrometer1This standard is issued under the fixed designation F1710;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 determination of concentra-tions of trace metallic impurities in high purity titanium.1.2 This test method pertains to analysis by magnetic-sectorglow discharge mass spectrometer(GDMS).1.3 The titanium matrix must be 99.9 weight%(3N-grade)pure,or purer,with respect to metallic impurities.There mustbe no major alloy constituent,for example,aluminum or iron,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 effect the reliability of high puritytitanium 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 MaterialsE173 Practice for Conducting Interlaboratory Studies ofMethods for Chemical Analysis of Metals(Withdrawn1998)3E180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals(Withdrawn 2009)3E691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodE1257 Guide for Evaluating Grinding Materials Used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,not covered in Terminology E135,is indicated in 3.2.3.2 Definitions:3.2.1 campaigna series of analyses of similar specimensperformed in the same manner in one working session,usingone GDMS setup.3.2.1.1 DiscussionAs a practical matter,cleaning of theion source specimen cell is often the boundary event separatingone analysis campaign from the next.3.2.2 reference samplematerial accepted as suitable foruse as a calibration/sensitivity reference standard by all partiesconcerned with the analyses.3.2.3 specimena suitably sized piece cut from a referenceor test sample,prepared for installation in the GDMS ionsource,and analyzed.3.2.4 test samplematerial titanium to be analyzed for tracemetallic impurities by this GDMS method.3.2.4.1 DiscussionGenerally the test sample is extractedfrom a larger batch(lot,casting)of product and is intended tobe 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 beam1This 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 1996.Last previous edition approved in 2002 as F1710 97(02).DOI:10.1520/F1710-08.2For 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.3The last approved version of this historical standard is referenced onwww.astm.org.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 through a double-focusing magnetic-sector mass separationapparatus.The mass spectrum,that is,the ion current,iscollected as magnetic field or acceleration voltage,or both,isscanned.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.4.2.1 If the source of interfering contributions to the mea-sured ion current at Micannot be determined una