TM_A_751
14
NOTICE:This standard has either been superseded and replaced by a new version or withdrawn.Contact ASTM International(www.astm.org)for the latest informationDesignation:A751-14NTERNATIONALStandardTest Methods,Practices,and Terminology forChemical Analysis of Steel Products1This standard is issued under the fixed designation A751: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(e)indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S.Department of Defense.INTRODUCTIONThese test methods,practices,and terminology were prepared to answer the need for a singledocument that would include all aspects of obtaining and reporting the chemical analysis of steel,stainless steel,and related alloys.Such subjects as definitions of terms and product(check)analysisvariations(tolerances)required clarification.Requirements for sampling,meeting specified limits,andtreatment of data usually were not clearly established in product specifications.It is intended that these test methods,practices,and terminology will contain all requirements forthe determination of chemical composition of steel,stainless steel,or related alloys so that productspecifications will need contain only special modifications and exceptions.1.Scope*priate safety and health practices and determine the applica-1.1 These test methods,practices,and terminology coverbility of regulatory limitations prior to use.definitions,reference methods,practices,and guides relating tothe chemical analysis of steel.stainless steel.and related2.Referenced Documentsalloys.It includes both wet chemical and instrumental tech-2.1 ASTM Standards:2niques.E29 Practice for Using Significant Digits in Test Data to1.2 Directions are provided for handling chemicalDetermine Conformance with Specificationsrequirements,product analyses,residual elements,and refer-E50 Practices for Apparatus,Reagents,and Safety Consid-ence standards,and for the treatment and reporting of chemicalerations for Chemical Analysis of Metals,Ores,andanalysis data.Related MaterialsE60 Practice for Analysis of Metals,Ores,and Related1.3 These test methods,practices,and terminology applyMaterials by Spectrophotometryonly to those product standards which include these testE322 Test Method for Analysis of Low-Alloy Steels andmethods,practices,and terminology,or parts thereof,as aCast Irons by Wavelength Dispersive X-Ray Fluorescencerequirement.Spectrometry1.4 In cases of conflict,the product specification require-E350 Test Methods for Chemical Analysis of Carbon Steel,ments shall take precedence over the requirements of these testLow-Alloy Steel,Silicon Electrical Steel,Ingot Iron,andmethods,practices,and terminology.Wrought Iron1.5 Attention is directed to ISO/IEC 17025 when there mayE352 Test Methods for Chemical Analysis of Tool Steels andbe a need for information on criteria for evaluation of testingOther Similar Medium-and High-Alloy Steelslaboratories.E353 Test Methods for Chemical Analysis of Stainless,Heat-Resisting.Maraging,and Other Similar Chromium-1.6 This standard does not purport to address all of theNickel-Iron Alloyssafety concerns,if any,associated with its use.It is theE354 Test Methods for Chemical Analysis of High-responsibility of the user of this standard to establish appro-Temperature,Electrical,Magnetic,and Other Similar Iron,Nickel,and Cobalt AlloysThese test methods,practices,and terminology are under the jurisdiction ofASTM Committee A01 on Steel,Stainless Steel and Related Alloys and are thedirect responsibility of Subcommittee A01.13 on Mechanical and Chemical Testingand Processing Methods of Steel Products and Processes.2 For referenced ASTM standards,visit the ASTM website,www.astm.org.orCurrent edition approved March 1,2014.Published April 2014.Originallycontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMapproved in 1977.Last previous edition approved in 2011 as A751-11.DOI:Standards volume information,refer to the standards Document Summary page on10.1520/A0751-14.the ASTM website.*A Summary of Changes section appears at the end of this standardCopyright ASTM Intemational,100 Barr Harbor Drive,PO Box C700.West Conshohocken.PA 19428-2959.United StatesA751-14E415 Test Method for Atomic Emission Vacuum Spectro-document include precision statements with reproducibility data with themetric Analysis of Carbon and Low-Alloy Steelexception of Test Methods E50.E548 Guide for General Criteria Used for Evaluating Labo-3.1.1.3 product analysis tolerances(Note 2)-a permissibleratory Competence(Withdrawn 2002)3variation over the maximum limit or under the minimum limitE572 Test Method for Analysis of Stainless and Alloy Steelsof a specified element and applicable only to product analyses,by Wavelength Dispersive X-Ray Fluorescence Spectrom-not cast or heat analyses.etryNoTE 2-The term analysis toleranceis often misunderstood.It doesE743 Guide for Spectrochemical Laboratory Quality Assur-not apply to cast or heat analyses determined to show conformance toance(Withdrawn 1998)specified chemical limits.It applies only to product analysis and becomesE851 Practice for Evaluation of Spectrochemical Laborato-meaningful only when the heat analysis of an element falls close to one ofries(Withdrawn 1998)3the specified limits.For example,stainless steel UNS 30400 limits forE882 Guide for Accountability and Quality Control in thechromium are 18.00 to 20.00%A heat that the producer reported as18.01%chromium may be found to show 17.80%chromium by a userChemical Analysis Laboratoryperforming a product analysis.If the product analysis tolerance for such aE1019 Test Methods for Determination of Carbon,Sulfur.chromium level is 0.20%,the product analysis of 17.80%chromiumNitrogen,and Oxygen in Steel,Iron,Nickel,and Cobaltwould be acceptable.A product analysis of 17.79%would not beAlloys by Various Combustion and Fusion Techniquesacceptable.E1085 Test Method for Analysis of Low-Alloy Steels by3.1.1.4 proprietary analytical method-a non-standard ana-X-Ray Fluorescence Spectrometrylytical method,not published by ASTM,utilizing referenceE1086 Test Method for Atomic Emission Vacuum Spectro-standards traceable to the National Institute of Standards andmetric Analysis of Stainless Steel by Point-to-Plane Ex-Technology(NIST)(when available)or other sources refer-citation Techniqueenced in Section 10.E1097 Guide for Determination of Various Elements by3.1.1.5 referee analysis-performed using ASTM methodsDirect Current Plasma Atomic Emission Spectrometrylisted in 9.1.1 and NIST reference standards or methods andE1184 Practice for Determination of Elements by Graphitereference standards agreed upon between parties.The selectionFurnace Atomic Absorption Spectrometryof a laboratory to perform the referee analysis shall be a matterE1282 Guide for Specifying the Chemical Compositions andof agreement between the supplier and the purchaser.Selecting Sampling Practices and Quantitative Analysis3.1.1.6 certified reference material-a specimen of materialMethods for Metals.Ores.and Related Materialsspecially prepared,analyzed,and certified for chemical contentE1329 Practice for Verification and Use of Control Charts inunder the jurisdiction of a recognized standardizing agency orSpectrochemical Analysisgroup,such as the National Institute of Standards andE1806 Practice for Sampling Steel and Iron for Determina-Technology,for use by analytical laboratories as an accuratetion of Chemical Compositionbasis for comparison.Reference samples should bear sufficient2.2 ISO Standards:resemblance to the material to be analyzed so that no signifi-ISO/IEC 17025 General Requirements for the Competencecant differences are required in procedures or corrections(forof Testing and Calibration Laboratoriesexample,for interferences or inter-element effects).3.1.1.7 working reference materials-reference materials3.Terminologyused for routine analytical control and traceable to NIST3.1 Definitions:standards and other recognized standards when appropriate3.1.1 Pertaining to Analyses:standards are available.3.1.1.1 cast or heat(formerly ladle)analysis-applies to3.1.2 Pertaining to Elements:chemical analyses representative of a heat of steel as reported3.1.2.1 intentionally added unspecified element-an elementto the purchaser and determined by analyzing a test sample,added in controlled amounts at the option of the producer topreferably obtained during the pouring of the steel,for theobtain desirable characteristics.elements designated in a specification.3.1.2.2 residual element-a specified or unspecified3.1.1.2 product,check or verification analysis-a chemicalelement,not intentionally added,originating in raw materials,analysis of the semifinished or finished product,usually for therefractories,or air.purpose of determining conformance to the specification re-3.1.2.3 specified element-an element controlled to a speci-quirements.The range of the specified composition applicablefied range,maximum or minimum,in accordance with theto product analysis is normally greater than that applicable torequirements of the product specification.heat analysis in order to take into account deviations associated3.1.2.4 trace element-a residual element that may occur inwith analytical reproducibility(Note 1)and the heterogeneityvery low concentrations,generally less than 0.01%of the steel.4.Concerning the Specification of Chemical CompositionNorE 1-All of the chemical analysis procedures referenced in thisRequirements4.1 It is recommended that Guide E1282 be consulted as a3The last approved version of this historical standard is referenced onguide for specifying the chemical compositions for steels.www.astm.org.4Available from American National Standards Institute(ANSD),25 W.43rd St.4.2 The recommended practice for specifying chemical4th Floor.New York,NY 10036,http:/position limits is to limit the number of significant figuresA751-14for each element so that the number of figures to the right of the6.3 Product analysis tolerances,where available,are givendecimal point conforms to the following:in the individual material specifications or in the generalChemicalMaximum Number of Figures torequirement specifications.Concentrationthe Right of the Decimal PointUp to 0.010%,incl.0.XXXX or may be expressed as ppm7.Unspecified Elements(Note 4)Over 0.010%toO.XXX0.10%,incl.7.1 Reporting analyses of unspecified elements is permitted.0ver0.10%to3.0%.0.XXincl.NoTE 4-All commercial metals contain small amounts of variousOver 3.0%0.Xelements in addition to those which are specified.It is neither practical nor4.3 For those cases in which the composition range spansnecessary to specify limits for every unspecified element that might bepresent,despite the fact that the presence of many of these elements iseither 0.10 or 3.0%the number of figures to the right of theoften routinely determined by the producer.decimal is to be determined by that indicated by the upperlimit.7.2 Analysis limits shall be established for specific elementsrather than groups of elements such as“all others,”“rare4.4 Technical considerations may dictate the employment ofearths,”and“balance,”less than the number of figures to the right of the decimal aspreviously recommended.8.SamplingNorE 3-The recommendations should be employed to reduce the8.1 Cast or Heat Analyses:number of significant figures,such as from 18.00 to 18.0%but a8.1.1 Samples shall be taken,insofar as possible,during thesignificant figure should never be added unless there is a technical reasoncasting of a heat,at a time which,in the producers judgment,for so doing.best represents the composition of the cast.5.Cast or Heat Analysis8.1.2 In case the heat analysis samples or analyses are lost5.1 The producer shall perform analyses for those elementsor inadequate,or when it is evident that the sample does notspecified in the material specification.The results of suchtruly represent the heat,representative samples may be takenanalyses shall conform to the requirements specified in thefrom the semifinished or finished product,in which case suchmaterial specification.samples may be analyzed to satisfy the specified requirements5.1.1 For multiple heats,either individual heat or castThe analysis shall meet the specified limits for heat analysis.analysis or an average heat or cast analysis shall be reported.If8.2 Check,Product,or Verification Analyses-Unless other-significant variations in heat or cast size are involved,awise specified,the latest revision of Practice E1806 shall beweighted average heat or cast analysis,based on the relativeused as a guide for samplingquantity of metal in each heat or cast,shall be reported.5.1.2 For consumable electrode remelted material,a heat is9.Test Methodsdefined as all the ingots remelted by the same process from a9.1 This section lists some test methods that have beenprimary heat.The heat analysis shall be obtained from onefound acceptable for chemical analysis of steels.remelted ingot,or the product of one remelted ingot,from eachprimary melt.If this heat analysis does not meet the heat9.1.1 The following ASTM wet chemical test methods havebeen found acceptable as referee test methods and as a base foranalysis requirements of the specification,one sample from thestandardizing instrumental analysis techniques:product of each remelted ingot shall be analyzed,and theanalyses shall meet the heat analysis requirements.TestMethodsGeneral Description5.2 If the test samples taken for the heat analysis are lost,E350the basic wet chemical procedure for steelsinadequate,or not representative of the heat,a product analysisE352wet chemical procedure for tool steelsE353wet chemical procedure for stainless steelsof the semifinished or finished product may be used to establishE354wet chemical procedure for high nickel steelsthe heat analysis.E1019determination of carbon,sulfur,nitrogen,oxygen,and5.2.1 If a product analysis is made to establish the heathydrogen,in steel and in iron,nickel,and cobalt alloysanalysis,the product analysis shall meet the specified limits for9.1.2 The following ASTM instrumental test methods,heat analysis and the product analysis tolerances described inpractices,and guides may be employed for chemical analysisSection 6 do not apply.of steels or may be useful as a guide in the calibration andstandardization of instrumental equipment for routine sampling6.Product Analysis Requirementsand analysis of steels:6.1 For product analysis,the range of the specified chemicalStandardGeneral Descriptioncomposition is normally greater(designated product analysisE50apparatus,reagents,and safetyE60tolerances)than that applicable to heat analyses to take intophotometric and spectrophotometric workspectrographic analysis of steels(rod-to-rod technique)account deviations associated with analytical reproducibilityspectrographic analysis of acid-soluble aluminumand the heterogeneity of the steel.If several determinations ofE322x-ray fluorescence for steelsany element in the heat are made,they may not vary bothspectrometric analysis of stainless steelsE415vacuum spectrometric analysis of steelsabove and below the specified range.spectrographic determination of silicon and aluminum in6.2 Product analysis tolerances may not be used to deter-high-purity ironE572x-ray emission spectrometric analysis of stainless steelsmine conformance to the specified heat or cast analysis unlessflame atomic absorptionpermitted by the individual material specification.E882accountability and quality controlA751-14E1019-determination of carbon,sulfur,nitrogen,oxygen,and hy-TABLE 2 Normal Elements and Ranges for Stainless Steelsdrogen in steel and in iron,nickel,and cobalt alloysUsing Spark Emission SpectroscopyE1085x-ray emission spectrometric analysis of low alloy steels0.004-5.00.005-2.0E1086optical emission vacuum spectrometric analysis of stain-s0.0005-0.10.005-2.5less steel by the point-to plane excitation technique0.00200.30.0054.0E1097Codirect current plasma spectroscopyMN0.005-15.00.001-0.20E1184graphite furnace atomic absorption0.001-1.5W0.005-3.0E1282selecting sampling practices and analysis methodsSi0.005-5.0Pb0.002-0.05E1329verification and use of control charts90.01-26.00.00050.05E1806samplingNi0.01-36.0Ca0.00020.019.2 The following are some of the commonly accepted90.001-5.50.001-0.01Mo0.005-8.0e0.001-0.2techniques employed for routine chemical analysis of steels.Cu0.005-4.0Z0.001-0.1These routine analyses are the basis for the producersqualityCb0.005-3.00.005-0.5control/assurance programs.Proprietary methods are permis-sible provided the results are equivalent to those obtained fromstandard methods when applicable.9.2.1 Analysis of stainless steels using x-ray fluorescence9.3 There are additional common techniques often used forchemical analysis of standards for instrument analysis such as:spectroscopy(XRF).See Table 1 for normal elements andpolarographic analysis,ion exchange separations,ranges for stainless steels.radioactivation,and mass spectrometry.9.2.2 Analysis of stainless steels using spark emissionspectroscopy(OES).See Table 2 for normal elements and10.Reference Materialsranges for stainless steels.9.2.3 Analysis of solutions using an atomic absorption10.1 For referee analyses,reference standards of a recog-spectrophotometer.nized standardizing agency shall be employed with preference9.2.4 Analysis of solutions using an inductively coupledgiven to NIST standard reference materials when applicable(NIST does not produce reference standards suitable for allplasma emission spectrometer.9.2.5 Determination of carbon or sulfur,or both,by com-elements or all alloys.3)bustion(in oxygen)and measurement of CO2 or SO2,or both,10.1.1 When standard reference materials for certain alloysby thermal conductivity or infrared detectors.are not available from NIST,reference materials may beproduced by employing ASTM standard procedures and NISTElement RangesElement Rangesstandard reference materials to the extent that such procedures0.002-5.00.0005-0.19.2.6 Determination of nitrogen and oxygen by fusion(in aand reference standards are available.Several independentlaboratories should be used for certification of these standardshelium atmosphere)and measurement of N2 by thermal con-ductivity and oxygen by measurement of CO by infrared orand their results statistically reviewed and merged.10.1.2 Methods not published by ASTM such as a definitivethermal conductivity detectors.analytical method may be used when the method is validatedElement Rangesby analyzing certified reference materials along with theN20.00050.3020.0008-0.02candidate reference material.Examples of definitive analytical9.2.7 Analysis of solutions using inductively coupledmethods include gravimetric,coulometry,titrimetric based onplasma emission spectroscopy(ICP)or direct plasma emissionnormality,and mass spectrometryspectroscopy(DCP).Normal elements and ranges for stainless10.2 Working reference materials may be used for routinesteels are as follows:analytical control.Element Ranges%B0.00020.0111.Significant Numbers0.00020.01Mg0.00020.0111.1 Laboratories shall report each element to the same0.0010.2number of significant numbers as used in the pertinent material0.0010.1specifications.0.0050.5La0.0010.0111.2 When a chemical determination yields a greater num-ber of significant numbers than is specified for an element,theresult shall be rounded in accordance with Section 12.12.Rounding ProcedureTABLE 1 Normal Elements and Ranges for Stainless SteelsUsing X-Ray Fluorescence Spectroscopy12.1 To determine conformance with the specificationElement RangesElement Rangesrequirements,an observed value or calculated value shall be0.005-15.0Cu0.005-4.0rounded in accordance with Practice E29 to the nearest unit inP0.001-0.15Cb0.005-3.0the last right-hand place of values listed in the table ofSi0.005-5.00.005-2.0Cr0.01-26.00.005-2.5chemical requirements.Ni0.01-36.0Co0.005-4.0Al0.002-5.50.002-0.20Mo0.005-8.00.005-3.03 Some sources of reference materials are listed in ASTM Data Series PublicationNo.DS2,issued 1963.A751-1412.2 In the special case of rounding the number5when13.1.1 Description of the material tested,for example,heatno additional numbers other than0”follow the“5”,roundingnumber,grade of material,product specification.shall be done in the direction of the specification analysis limits13.1.2 Test method(s)or unambiguous description of theif following Practice E29 would cause rejection of material.nonstandard method(s)used.13.Records14.Keywords13.1 In addition to the test data requested,the test records14.I cast analysis:chemical analysis;heat analysis;productshall contain the following information as appropriate:analysis:reference materialsAPPENDIX(Nonmandatory Information)X1.QUALITY ASSURANCE FOR VALIDITY OF ANALYTICAL RESULTSX1.1 The requirements embodied in Guide E548,ISO/X1.3.1 Replication of sampling and testing to improve theIEC 17025,and E851 provide generic requirements for pro-precision of results:duction of valid chemical-analysis results.X1.3.2 Use of reference materials is crucial to accurateresults;X1.2 Additional pertinent standards for improving the com-petency of chemical analysis laboratories are included inX1.3.3 Instrumentation that is appropriate and properlyGuides E743 and E882.maintained:andX1.3.4 Personnel who are properly trained,ethical chemistsX1.3 Keys to improving validity of chemical analyticalor technicians and who work with properly documented,results are as follows:current standards.