1、Designation: E415 15Standard Test Method forAnalysis of Carbon and Low-Alloy Steel by Spark AtomicEmission Spectrometry1This standard is issued under the fixed designation E415; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the y
2、ear 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 simultaneous determinationof 21 alloying and residual elements in carbon and low-al
3、loysteels by spark atomic emission vacuum spectrometry in themass fraction ranges shown Note 1.ElementComposition Range, %ApplicableRange,Mass Fraction%AQuantitative Range,Mass Fraction %BAluminum 0 to 0.093 0.006 to 0.093Antimony 0 to 0.027 0.006 to 0.027Arsenic 0 to 0.1 0.003 to 0.1Boron 0 to 0.00
4、7 0.0004 to 0.007Calcium 0 to 0.003 0.002 to 0.003Carbon 0 to 1.1 0.02 to 1.1Chromium 0 to 8.2 0.007 to 8.14Cobalt 0 to 0.20 0.006 to 0.20Copper 0 to 0.5 0.006 to 0.5Manganese 0 to 2.0 0.03 to 2.0Molybdenum 0 to 1.3 0.007 to 1.3Nickel 0 to 5.0 0.006 to 5.0Niobium 0 to 0.12 0.003 to 0.12Nitrogen 0 to
5、 0.015 0.01 to 0.055Phosphorous 0 to 0.085 0.006 to 0.085Silicon 0 to 1.54 0.02 to 1.54Sulfur 0 to 0.055 0.001 to 0.055Tin 0 to 0.061 0.005 to 0.061Titanium 0 to 0.2 0.001 to 0.2Vanadium 0 to 0.3 0.003 to 0.3Zirconium 0 to 0.05 0.01 to 0.05AApplicable range in accordance with Guide E1763 for results
6、 reported inaccordance with Practice E1950.BQuantitative range in accordance with Practice E1601.NOTE 1The mass fraction ranges of the elements listed have beenestablished through cooperative testing2of reference materials.1.2 This test method covers analysis of specimens having adiameter adequate t
7、o overlap and seal the bore of the sparkstand opening. The specimen thickness can vary significantlyaccording to the design of the spectrometer stand, but athickness between 10 mm and 38 mm has been found to bemost practical.1.3 This test method covers the routine control analysis iniron and steelma
8、king operations and the analysis of processedmaterial. It is designed for chill-cast, rolled, and forgedspecimens. Better performance is expected when referencematerials and specimens are of similar metallurgical conditionand composition. However, it is not required for all applica-tions of this sta
9、ndard.1.4 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. Refere
10、nced Documents2.1 ASTM Standards:3E29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE305 Practice for Establishing and Controlling AtomicEmission Spectrochemical An
11、alytical CurvesE350 Test Methods for Chemical Analysis of Carbon Steel,Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, andWrought IronE406 Practice for Using Controlled Atmospheres in Spec-trochemical AnalysisE1019 Test Methods for Determination of Carbon, Sulfur,Nitrogen, and Oxygen in Steel
12、, Iron, Nickel, and CobaltAlloys by Various Combustion and Fusion TechniquesE1329 Practice for Verification and Use of Control Charts inSpectrochemical AnalysisE1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical MethodE1763 Guide for Interpretation and
13、Use of Results from1This 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, 2015. Published March 2016. Ori
14、ginallyapproved in 1971. Last previous edition approved in 2014 as E415 14. DOI:10.1520/E0415-15.2Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:E01-1122. ContactASTM CustomerService at serviceastm.org.3For referenced ASTM stand
15、ards, 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
16、 19428-2959. United States1Interlaboratory Testing of Chemical Analysis Methods(Withdrawn 2015)4E1806 Practice for Sampling Steel and Iron for Determina-tion of Chemical CompositionE1950 Practice for Reporting Results from Methods ofChemical AnalysisE2972 Guide for Production, Testing, and Value Ass
17、ignmentof In-House Reference Materials for Metals, Ores, andOther Related Materials2.2 Other ASTM DocumentsASTM MNL 7 Manual on Presentation of Data and ControlChart Analysis53. Terminology3.1 For definitions of terms used in this test method, refer toTerminologyE135.4. Summary of Test Method4.1 A c
18、apacitor discharge is produced between the flat,ground surface of the disk specimen and a conically shapedelectrode. The discharge is terminated at a predeterminedintensity time integral of a selected iron line, or at a predeter-mined time, and the relative radiant energies of the analyticallines ar
19、e recorded. The most sensitive lines of arsenic, boron,carbon, nitrogen, phosphorus, sulfur, and tin lie in the vacuumultraviolet region. The absorption of the radiation by air in thisregion is overcome by evacuating the spectrometer or by use ofa vacuum ultraviolet (VUV) transparent gas and flushin
20、g thespark chamber with argon.5. Significance and Use5.1 This test method for the spectrometric analysis of metalsand alloys is primarily intended to test such materials forcompliance with compositional specifications. It is assumedthat all who use this test method will be analysts capable ofperform
21、ing common laboratory procedures skillfully andsafely. It is expected that work will be performed in a properlyequipped laboratory.6. Apparatus6.1 Sampling Devices:6.1.1 Refer to Practice E1806 for devices and practices tosample liquid and solid iron and steel.6.2 Excitation Source, capable of provi
22、ding electrical pa-rameters to spark a sample. See 11.1 for details.6.3 Spark Chamber, automatically flushed with argon. Thespark chamber shall be mounted directly on the spectrometerand shall be provided with a spark stand to hold a flat specimenand a lower counter electrode of rod form.6.3.1 Follo
23、w the manufacturers recommendations forcleaning the spark chamber. During continuous operation, thistypically should be done every 24 h. Follow the manufacturersrecommendations for cleaning the entrance lens or window(verifier data or other reference sample intensity data cantypically indicate when
24、this is necessary).6.4 Spectral LinesTable 1 lists spectral lines and internalstandards usable for carbon and low alloy steel. The spectrom-eter must be able to measure at least one of the listed spectrallines for each of the listed elements. Spectral lines other thanthose listed in Table 1 may be u
25、sed provided it can be shownexperimentally that equivalent precision and accuracy areobtained.6.5 Measuring System, spectrometer capable of convertinglight intensities to measurable electrical signals. The measuringsystem may consist of one of the following configurations:6.5.1 A photomultiplier (PM
26、T) array having individualvoltage adjustments, capacitors in which the output of eachphotomultiplier is stored, a voltage measuring system toregister the voltages on the capacitors either directly orindirectly, and the necessary switching arrangements to pro-vide the desired sequence of operation.6.
27、5.2 A semiconductor detector array (CCD or CMOS),pixel selection electronics to reset the pixels and to transportthe voltage of an individual pixel to one or more output portsof the detector arrays, and a voltage measuring system toregister the voltage of said output ports.6.5.3 A hybrid design usin
28、g both photomultipliers andsemiconductor arrays.6.6 Optical PathIf the instrument is operated using aVUV transparent gas, check the manufacturers suggested gaspurity. It may be necessary to have a gas purification systemconsisting of a circulation pump and a cleaning cartridge tokeep the O2(g) resid
29、ual 500 ng/g and H2O (g) residual1 g g and remove impurities of nitrogen and hydrocarbons.If the instrument is using a vacuum pump, it should be capableof maintaining a vacuum of 3.33 Pa (25 m Hg) or less.NOTE 2A pump with a displacement of at least 0.23 m3/min (8ft3/min) is usually adequate.6.7 Gas
30、 System, consisting of an argon supply with pressureand flow regulation.Automatic sequencing shall be provided toactuate the flow at a given rate for a specific time interval. Theflow rate may be manually or automatically set. The argonsystem shall be in accordance with Practice E406.7. Reagents and
31、 Materials7.1 Counter ElectrodesThe counter electrodes can besilver or thoriated tungsten rods, or other material, provided itcan be shown experimentally that equivalent precision and biasare obtained. The rods can vary in diameter from 1.5 mm to 6.5mm (depending on the instrument design) and typica
32、lly aremachined to a 90 or 120 angled tip.7.1.1 A black deposit will collect on the tip of the electrode.This deposit should be removed between specimens (typicallywith a wire brush). If not removed, it can reduce the overallintensity of the spectral radiation or transfer slight amounts ofcontaminat
33、ion between specimens, or both. The number ofacceptable burns on an electrode varies from one instrument toanother, and should be established in each laboratory.NOTE 3It has been reported that thousands of burns can be performedon a thoriated tungsten electrode before replacement is necessary.4The l
34、ast approved version of this historical standard is referenced onwww.astm.org.5ASTM Manual Series, ASTM International, 8th edition, 2010.E415 152TABLE 1 Internal Standard and Analytical LinesElementWavelength,nmLineClassificationAPossibleInterferenceBAluminum 396.15 I Mo394.40 I V, Mn, Mo, Ni308.22
35、I V, MnAntimony 217.6 I Ni, Nb, Mn, WArsenic 189.04 I V, Cr197.20 I Mo, W193.76 I MnBoron 345.13 II182.64 I S, Mn, Mo182.59 I W, Mn, CuCalcium 393.37 II396.85 II NbCarbon 165.81 I Cr193.09 I AlChromium 312.26 II V313.21 II425.44 I298.92 II Mn, V, Ni, Nb, Mo267.72 II Mn, Mo, WCobalt 345.35 I Cr, Mo22
36、8.62 II Ni, Cr258.03 II Fe, Mn, WCopper 212.3 II Si324.75 I Mn, Nb327.40 I Nb224.26 II W, Ni213.60 II Mo, Cr510.55 I W136.14 II157.40 II172.24 II174.28 II179.34 I182.88 II205.13 I216.20 I217.81 I218.65 II226.76 II235.12 II239.15 I277.21 I281.33 I285.18 I296.69 II297.05 I299.95 I300.81 I303.74 I304.7
37、6 IIron (IS) 305.91 I316.79 I517.16 I321.33 II487.21 I458.38 II413.70 I410.75 I383.63 I363.83 I339.93 I328.68 I308.37 I282.33 I249.59 IE415 153TABLE 1 ContinuedElementWavelength,nmLineClassificationAPossibleInterferenceB226.76 II218.65 II216.20 I193.53 II190.48 I187.75 II149.65 II271.44 II273.07 IIC
38、o492.39 ILead 405.75 I MnManganese 293.31 II Cr, Mo, Ni255.86 II Zr263.82 II Al, WMolybdenum 379.83 IIMn202.03 II277.54 I Cu, V, Co, Mn281.61 II Mn386.41 I V, CrNickel 471.44 I227.73 II341.48 I352.45 I231.60 II Co, Ti227.02 II Nb, W243.79 II Co, Fe, NiNiobium 313.08 II Ti, V319.50 II Mo, Al, VNitrog
39、en 149.26 I Fe, Ti, Si, Mn, Cu, Ni and nitrideforming elements such as TiPhosphorus 178.29 I MoSilicon 288.16 I Mo, Cr, W251.61 I Fe, V212.41 I Mo, Ni, V, Cu, Nb390.55 I Cr, Cu, W, TiSulfur 180.73 I MnTin 147.52 II189.99 II Mn, Mo, AlTitanium 308.80 I Cu, Co337.28 II NbTungsten 324.20 II Nb400.88 I2
40、02.99 II Ti, V, Mn220.50 II CoVanadium 437.92 I310.23 II Fe, Mo, Nb, NiZirconium 468.78 I349.62 II343.82 II W206.19 II WAThe numerals I or II in the line classification column indicate that the line has been classified in a term array and definitely assigned to the normal atom (I) or to the singlyio
41、nized atom (II).BInterferences are dependent upon instrument design, spectrum line choices, and excitation conditions, and those listed require confirmation based upon specimensselected especially to demonstrate suspected interferences.E415 1547.2 Inert Gas, Argon, in accordance with Practice E406.8
42、. Reference Materials8.1 Certified Reference Materials (CRMs)These are avail-able from the National Institute of Standards and Technology(NIST) and other sources and span all or part of the massfraction ranges listed in 1.1. They are used to calibrate thespectrometer for the elements of interest or
43、to validate theperformance of the test method. It is not recommended to useCRMs as verifiers or to establish the repeatability of thechemical measurement process.NOTE 4Certified Reference Materials manufactured by NIST aretrademarked with the name, “Standard Reference Material.”8.2 Reference Materia
44、ls (RMs)These are available frommultiple suppliers or can be developed in house. ReferenceMaterials are typically used in control procedures (verifiers)and in drift correction (standardization) of the spectrometer,and they may be useful in calibrations. These referencematerials shall be homogenous a
45、nd contain appropriate massfractions of each element for the intended purpose. Refer toGuide E2972 for production of your own reference materials.8.3 Several issues can impact the selection and use ofCRMs and RMs:8.3.1 Samples and reference materials may exhibit differ-ences in metallurgical structu
46、re, in particular having differentsizes, compositions, and distributions of inclusions. Inhomo-geneous distribution of inclusions can worsen repeatability ofindividual measurements of elements found in the inclusions.Some inclusions may be removed during preburn steps prior tointegration of intensit
47、ies, causing low results. Typical samplescan be used to determine repeatability of individual measure-ments to yield estimates consistent with performance for actualsamples.8.3.2 For certain elements, there may be no availablereference materials with metallurgical structure similar totypical samples
48、. Therefore, calibrations may be biased. It isrecommended to validate results using typical samples ana-lyzed using Test Methods E350 and E1019.9. Preparation of Specimens and Reference Materials9.1 The specimens and reference materials shall be preparedin the same manner. A specimen cut from a larg
49、e samplesection shall be of sufficient size and thickness for preparationand to properly fit the spectrometer stand. A 10-mm to 38-mmthick specimen is normally most practical.9.2 Ensure that the specimens are free from voids and pits inthe region to be measured (Note 5). Initially, grind the surfacewith a 50-grit to 80-grit abrasive belt or disc (wet or dry) ormill the surface. If wet grinding, perform the final grind with adry abrasive belt or disc. A finer abrasive grinding media (forexample, 120-grit) may be used for the final grind, but is notessential.
