ASTM_E_1010_-_16.pdf

Designation:E101016Standard Practice forPreparation of Disk Specimens of Steel and Iron byRemelting for Spectrochemical Analysis1This standard is issued under the fixed designation E1010;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 practice describes the preparation of disk speci-mens of steel and iron by melting chunks,chips,drillings,turnings,wire,or powder briquets with an electric arc in anargon atmosphere.Solidification of the specimen takes place inthe crucible in an argon atmosphere.The disk obtained issuitable for quantitative spectrochemical analysis.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.Specific warningstatements are given in 6.2.1,Section 8,and 10.1.2.1.2.Referenced Documents2.1 ASTM Standards:2E135 Terminology Relating to Analytical Chemistry forMetals,Ores,and Related MaterialsE876 Practice for Use of Statistics in the Evaluation ofSpectrometric Data(Withdrawn 2003)33.Terminology3.1 For definitions of terms used in this procedure,refer toTerminology E135.4.Summary of Practice4.1 The sample of steel or iron is placed in a water-cooledcopper crucible.The furnace is flushed with argon at acontrolled rate of flow.An arc is struck between the electrodeand the sample material and is maintained until the melting iscomplete.The molten specimen is allowed to solidify in thecrucible in an argon atmosphere.After solidification,thespecimen is removed from the crucible and prepared forspectrochemical analysis.4.2 Partial losses of some elements may be experiencedduring the melting of the disk specimen.This procedure,ifcarefully followed,will provide consistent losses.Elementallosses can be determined by correlating the analysis of thecharge material with the spectrochemical analysis of theremelted specimen.5.Significance and Use5.1 Most spectrochemical instruments employed for analyz-ing steel and iron require a solid specimen with a flat surfacelarge enough for analytical excitation and measurement proce-dures.This practice describes a procedure for convertingunusual types of steel and iron samples to satisfactory spec-trochemical specimens.6.Apparatus6.1 Melting Furnace,4consisting of a chamber that containsthe following:6.1.1 Crucible,of copper and water-cooled,in whichsamples of steel or iron are melted,then solidified to formspecimens for spectrochemical analysis.6.1.2 Electrode Holder,water-cooled and of negativepolarity,that can be moved up and down easily,and may haveprovisions for circular motion and adjusting the arc gap to afixed spacing.6.1.3 Viewing Window,composed of dark welding-typeglass with an inner-protective glass that is impervious to heatand splatter from the molten metal.6.2 DC Electric Power Generator,to supply electric currentand voltage equivalent to that required for electric arc welding.It may be a rotating dc generator or a static rectifier withprovisions to adjust the current in the 0 A to 600 A range.1This practice is under the jurisdiction of ASTM Committee E01 on AnalyticalChemistry for Metals,Ores,and Related Materials and is the direct responsibility ofSubcommittee E01.01 on Iron,Steel,and Ferroalloys.Current edition approved Jan.15,2016.Published March 2016.Originallyapproved in 1984.Last previous edition approved in 2009 as E1010 09.DOI:10.1520/E1010-16.2For 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.4Melting furnaces,manufactured by Cianflone Scientific,228 RIDC Park WestDrive,Pittsburgh,PA 15275,http:/,have been found suitablefor this purpose.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 6.2.1 WarningA safety interlock shall be provided toprevent electrical shocks to the operator when the meltingfurnace is open.6.3 Vacuum Pump,with free air capacity of 50 L/min andvacuum of 350 m,minimum.7.Materials7.1 Inert Gas,argon of at least 99.96%purity.7.2 Electrode,thoriated tungsten or high-purity graphite.8.Hazards8.1 Operating personnel should adhere to the manufactur-ers operating recommendations to avoid electrical shock andphysical harm from light and heat.See 6.2.1 and 10.1.2.1 forspecific warnings.9.Preparation of Samples9.