ASTM_E_1852_-_13.pdf

Designation:E185213Standard Test Method forDetermination of Low Levels of Antimony in Carbon andLow-Alloy Steel by Graphite Furnace Atomic AbsorptionSpectrometry1This standard is issued under the fixed designation E1852;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 antimonyin carbon and low-alloy steel in the 0.0005%through 0.010%range.1.2 If this test method is used to test materials havingcontents less than 0.001%antimony,users of different labo-ratories will experience more than the usual 5%risk that theirresults will differ by more than 50%relative error.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.2.Referenced Documents2.1 ASTM Standards:2E50 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 MaterialsE1184 Practice for Determination of Elements by GraphiteFurnace Atomic Absorption SpectrometryE1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical MethodE1770 Practice for Optimization of Electrothermal AtomicAbsorption Spectrometric EquipmentE1806 Practice for Sampling Steel and Iron for Determina-tion of Chemical Composition2.2 ISO Standards:3ISO 5725 Precision of Test MethodsDetermination ofRepeatability and Reproducibility for a Standard TestMethod by Inter-Laboratory TestsISO 10698 SteelDetermination of Antimony ContentElectrothermal Atomic Absorption Spectrometric Method3.Terminology3.1 For definitions of terms used in this test method,refer toTerminology E135.4.Summary of Test Method4.1 The sample is dissolved in hydrochloric and nitric acidsand diluted to volume.An appropriate aliquot is injected intothe graphite furnace atomizer of an atomic absorptionspectrometer,which is equipped with a background correction.The sample is dried,pyrolized,and atomized.The absorbanceof the radiation from the external light source is measured andcompared to the absorbance of samples of known composition.NOTE1In general,the deuterium correction system should be able tocorrect for the broad-band background absorbance up to 0.5 to 0.6absorbance units.Zeeman systems should compensate for backgroundlevels as high as 1.0 to 1.5 absorbance units.5.Significance and Use5.1 This test method is utilized for the determination oftrace levels of antimony in carbon and low-alloy steel.It isassumed that the procedure will be performed by trainedanalysts capable of performing common laboratory practicesskillfully and safely.It is expected that the work will beperformed in a properly equipped laboratory and proper wastedisposal procedures will be followed.6.Hazards6.1 For precautions to be observed in the use of certainreagents and equipment in this test method,refer to PracticesE50.1This test method is under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals,Ores,and Related Materials and is the directresponsibility of Subcommittee E01.01 on Iron,Steel,and Ferroalloys.Current edition approved Nov.15,2013.Published January 2014.Originallyapproved in 1996.Last previous edition approved in 2008 as E1852 08.DOI:10.1520/E1852-13.2For 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.3Available from American National Standards Institute(ANSI),25 W.43rd St.,4th Floor,New York,NY 10036,http:/www.ansi.org.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 7.Apparatus7.1 Atomic Absorption Spectrometer with Graphite FurnaceAtomizer,equipped with background corrector and appropriatesignal output device,such as video display screen,digitalcomputer,printer or strip chart recorder,and autosampler.It isrecommended that the instrument meet the following perfor-mance requirements after adjusting the instrument and opti-mizing the furnace heating program as described in PracticeE1770.7.1.1 The characteristic mass determined in accordancewith Practice E1770 for antimony shall be less than 25 pg orwithin the manufacturers tolerance.7.1.2 The precision of the most concentrated blank additionsolution shall not exceed 10%of the mean absorbance of thesame solution.The precision of the least concentrated blankaddition solution(excluding Solution B0)shall not exceed 4%of the mean absorba