ASTM_E_1447_-_09.pdf

Designation:E144709Standard Test Method forDetermination of Hydrogen in Titanium and Titanium Alloysby Inert Gas Fusion Thermal Conductivity/Infrared DetectionMethod1This standard is issued under the fixed designation E1447;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 applies to the determination of hydro-gen in titanium and titanium alloys in concentrations from0.0006%to 0.0260%.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 determine the applica-bility of regulatory limitations prior to use.For specifichazards,see Section 9.2.Referenced Documents2.1 ASTM Standards:2C696 Test Methods for Chemical,Mass Spectrometric,andSpectrochemical Analysis of Nuclear-Grade Uranium Di-oxide Powders and PelletsE50 Practices for Apparatus,Reagents,and Safety Consid-erations for Chemical Analysis of Metals,Ores,andRelated MaterialsE135 Terminology Relating to Analytical Chemistry forMetals,Ores,and Related MaterialsE1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical MethodE1914 Practice for Use of Terms Relating to the Develop-ment and Evaluation of Methods for Chemical Analysis3.Terminology3.1 DefinitionsFor definitions of terms used in this testmethod,see Terminology E135 and E1914.4.Summary of Test Method4.1 The specimen,contained in a small,single-use graphitecrucible,is fused under a flowing carrier gas atmosphere.Hydrogen present in the sample is released as molecularhydrogen into the flowing gas stream.The hydrogen is sepa-rated from other liberated gases such as carbon monoxide andfinally measured in a thermal conductivity cell.4.2 Alternatively,hydrogen is converted to water by passingthe gas stream over heated copper oxide and subsequentlymeasuring in an appropriate infrared(IR)cell.4.3 This test method is written for use with commercialanalyzers equipped to perform the above operations automati-cally and is calibrated using reference materials of knownhydrogen content.5.Significance and Use5.1 This test method is intended to test for compliance withcompositional specifications.It is assumed that all who use thistest method will be trained analysts capable of performingcommon laboratory procedures skillfully and safely.It isexpected that the work will be performed in a properlyequipped laboratory.6.Interferences6.1 The elements ordinarily present in titanium and itsalloys do not interfere.7.Apparatus7.1 Fusion and Measurement ApparatusAutomatic hydro-gen determinator,consisting of an electrode furnace or induc-tion furnace;analytical gas stream impurity removal systems;auxiliary purification systems and either a thermal conductivitycell hydrogen measurement system or an infrared hydrogenmeasurement system(Note 1).NOTE1The apparatus and analysis system have been previouslydescribed in the Apparatus and Apparatus and Equipment sections of TestMethods C696.Several models of commercial analyzers are available andpresently in use in industry.Each has its own unique design characteristicsand operational requirements.Consult the instrument manufacturersinstructions for operational details.1This test method is under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals,Ores,and Related Materials and is the directresponsibility of Subcommittee E01.06 on Ti,Zr,W,Mo,Ta,Nb,Hf,Re.Current edition approved March 1,2009.Published March 2009.Originallyapproved in 1992.Last previous edition approved in 2005 as E1447 05.DOI:10.1520/E1447-09.2For 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 7.2 Graphite CruciblesThe crucibles are machined fromhigh-purity graphite.Use the size crucibles recommended bythe manufacturer of the instrument.7.3 Crucible TongsCapable of handling recommendedcrucibles.7.4 Tweezers or ForcepsFor contamination-free samplehandling.8.Reagents and Materials8.1 Acetone,low-residue reagent grade or higher purity.8.2 Sodium Hydroxide on Clay Base,commonly known asAscarite II.8.3 High-Purity Carrier Gas(99.99%)Argon,nitrogen,or helium(Note 2).NOTE2Carrier gases vary by instrument model and include high-purity argon,nitrogen,and helium.Consult instrument manufacturersinstructions for proper gas recommendation.8.