1、Designation: E415 15E415 17Standard 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
2、, 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 simultaneous determination of 21 alloying and residual elements in carbon an
3、d low-alloy steelsby spark atomic emission vacuum spectrometry in the mass 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
4、0 to 0.007 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 0.12Nitr
5、ogen 0 to 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 0.05A Applicable range in accordance with Guide E1763 f
6、or results reported in accordance with Practice E1950.B Quantitative range in accordance with Practice E1601.NOTE 1The mass fraction ranges of the elements listed have been established through cooperative testing2 of reference materials.1.2 This test method covers analysis of specimens having a diam
7、eter adequate to overlap and seal the bore of the spark standopening. The specimen thickness can vary significantly according to the design of the spectrometer stand, but a thickness between10 mm and 38 mm has been found to be most practical.1.3 This test method covers the routine control analysis i
8、n iron and steelmaking operations and the analysis of processedmaterial. It is designed for chill-cast, rolled, and forged specimens. Better performance is expected when reference materials andspecimens are of similar metallurgical condition and composition. However, it is not required for all appli
9、cations of this standard.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior
10、 to use.1 This test method is under the jurisdiction of ASTM Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials and is the direct responsibility ofSubcommittee E01.01 on Iron, Steel, and Ferroalloys.Current edition approved Nov. 15, 2015May 15, 2017. Published March 2016Ju
11、ne 2017. Originally approved in 1971. Last previous edition approved in 20142015 asE415 14.E415 15. DOI: 10.1520/E0415-15.2 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:E01-1122. Contact ASTM CustomerService at serviceastm.or
12、g.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior e
13、ditions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States11.5 This international standard was developed
14、in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1
15、 ASTM Standards:3E29 Practice for Using Significant Digits in Test Data to Determine Conformance with SpecificationsE135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related MaterialsE305 Practice for Establishing and Controlling Atomic Emission Spectrochemical Analytical Curve
16、sE350 Test Methods for Chemical Analysis of Carbon Steel, Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, and WroughtIronE406 Practice for Using Controlled Atmospheres in Spectrochemical AnalysisE1019 Test Methods for Determination of Carbon, Sulfur, Nitrogen, and Oxygen in Steel, Iron, Nicke
17、l, and Cobalt Alloys byVarious Combustion and Fusion TechniquesE1329 Practice for Verification and Use of Control Charts in Spectrochemical AnalysisE1601 Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical MethodE1763 Guide for Interpretation and Use of Resu
18、lts from Interlaboratory Testing of Chemical Analysis Methods (Withdrawn2015)4E1806 Practice for Sampling Steel and Iron for Determination of Chemical CompositionE1950 Practice for Reporting Results from Methods of Chemical AnalysisE2972 Guide for Production, Testing, and Value Assignment of In-Hous
19、e Reference Materials for Metals, Ores, and OtherRelated Materials2.2 Other ASTM DocumentsASTM MNL 7 Manual on Presentation of Data and Control Chart Analysis53. Terminology3.1 For definitions of terms used in this test method, refer to TerminologyE135.4. Summary of Test Method4.1 A capacitor discha
20、rge is produced between the flat, ground surface of the disk specimen and a conically shaped electrode.The discharge is terminated at a predetermined intensity time integral of a selected iron line, or at a predetermined time, and therelative radiant energies of the analytical lines are recorded. Th
21、e most sensitive lines of arsenic, boron, carbon, nitrogen,phosphorus, sulfur, and tin lie in the vacuum ultraviolet region. The absorption of the radiation by air in this region is overcomeby evacuating the spectrometer or by use of a vacuum ultraviolet (VUV) transparent gas and flushing the spark
22、chamber withargon.5. Significance and Use5.1 This test method for the spectrometric analysis of metals and alloys is primarily intended to test such materials forcompliance with compositional specifications. It is assumed that all who use this test method will be analysts capable of performingcommon
23、 laboratory procedures skillfully and safely. It is expected that work will be performed in a properly equipped laboratory.6. Apparatus6.1 Sampling Devices:6.1.1 Refer to Practice E1806 for devices and practices to sample liquid and solid iron and steel.6.2 Excitation Source, capable of providing el
24、ectrical parameters to spark a sample. See 11.1 for details.6.3 Spark Chamber, automatically flushed with argon. The spark chamber shall be mounted directly on the spectrometer andshall be provided with a spark stand to hold a flat specimen and a lower counter electrode of rod form.6.3.1 Follow the
25、manufacturers recommendations for cleaning the spark chamber. During continuous operation, this typicallyshould be done every 24 h. Follow the manufacturers recommendations for cleaning the entrance lens or window (verifier dataor other reference sample intensity data can typically indicate when thi
26、s is necessary).6.4 Spectral LinesTable 1 lists spectral lines and internal standards usable for carbon and low alloy steel. The spectrometermust be able to measure at least one of the listed spectral lines for each of the listed elements. Spectral lines other than those listedin Table 1 may be used
27、 provided it can be shown experimentally that equivalent precision and accuracy are obtained.3 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document S
28、ummary page on the ASTM website.4 The last approved version of this historical standard is referenced on www.astm.org.5 ASTM Manual Series, ASTM International, 8th edition, 2010.E415 172TABLE 1 Internal Standard and Analytical LinesElement Wavelength, nm LineClassificationA PossibleInterferenceBAlum
29、inum 396.15 I Mo394.40 I V, Mn, Mo, Ni308.22 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,
30、Mo267.72 II Mn, Mo, WCobalt 345.35 I Cr, Mo228.62 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 I2
31、96.69 II297.05 I299.95 I300.81 I303.74 I304.76 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 1736.5 Measuring System, spectrometer capable of converting light intensities to measurable electrical signals. The
32、 measuringsystem may consist of one of the following configurations:TABLE 1 ContinuedElement Wavelength, nm LineClassificationA PossibleInterferenceB226.76 II218.65 II216.20 I193.53 II190.48 I187.75 II149.65 II271.44 II273.07 II Co492.39 ILead 405.75 I MnManganese 293.31 II Cr, Mo, Ni255.86 II Zr263
33、.82 II Al, WMolybdenum 379.83 II Mn202.03 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, VNitrogen 149.26 I Fe, Ti, Si, Mn, Cu, Ni and nitrideforming elements such a
34、s 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 I202.99 II Ti, V, Mn220.50 II CoVanadium 437.92 I310.23 II Fe, Mo, Nb,
35、NiZirconium 468.78 I349.62 II343.82 II W206.19 II WA The 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 singlyionized atom (II).B Interferences are dependent upon instrument design
36、, spectrum line choices, and excitation conditions, and those listed require confirmation based upon specimensselected especially to demonstrate suspected interferences.E415 1746.5.1 A photomultiplier (PMT) array having individual voltage adjustments, capacitors in which the output of eachphotomulti
37、plier is stored, a voltage measuring system to register the voltages on the capacitors either directly or indirectly, and thenecessary switching arrangements to provide the desired sequence of operation.6.5.2 Asemiconductor detector array (CCD or CMOS), pixel selection electronics to reset the pixel
38、s and to transport the voltageof an individual pixel to one or more output ports of the detector arrays, and a voltage measuring system to register the voltageof said output ports.6.5.3 A hybrid design using both photomultipliers and semiconductor arrays.6.6 Optical PathIf the instrument is operated
39、 using a VUV transparent gas, check the manufacturers suggested gas purity.It may be necessary to have a gas purification system consisting of a circulation pump and a cleaning cartridge to keep the O2 (g)residual 500 ng/g and H2O (g) residual 1 gg and remove impurities of nitrogen and hydrocarbons.
40、 If the instrument is usinga vacuum pump, it should be capable of 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 (8 ft3/min) is usually adequate.6.7 Gas System, consisting of an argon supply with pressure and flow regulation. Automatic sequ
41、encing shall be provided toactuate the flow at a given rate for a specific time interval. The flow rate may be manually or automatically set. The argon systemshall be in accordance with Practice E406.7. Reagents and Materials7.1 Counter ElectrodesThe counter electrodes can be silver or thoriated tun
42、gsten rods, or other material, provided it can beshown experimentally that equivalent precision and bias are obtained. The rods can vary in diameter from 1.5 mm to 6.5 mm(depending on the instrument design) and typically are machined to a 90 or 120 angled tip.7.1.1 Ablack deposit will collect on the
43、 tip of the electrode. This deposit should be removed between specimens (typically witha wire brush). If not removed, it can reduce the overall intensity of the spectral radiation or transfer slight amounts of contaminationbetween specimens, or both. The number of acceptable burns on an electrode va
44、ries from one instrument to another, and shouldbe established in each laboratory.NOTE 3It has been reported that thousands of burns can be performed on a thoriated tungsten electrode before replacement is necessary.7.2 Inert Gas, Argon, in accordance with Practice E406.8. Reference Materials8.1 Cert
45、ified Reference Materials (CRMs)These are available from the National Institute of Standards and Technology (NIST)and other sources and span all or part of the mass fraction ranges listed in 1.1. They are used to calibrate the spectrometer for theelements of interest or to validate the performance o
46、f the test method. It is not recommended to use CRMs as verifiers or toestablish the repeatability of the chemical measurement process.NOTE 4Certified Reference Materials manufactured by NIST are trademarked with the name, “Standard Reference Material.”8.2 Reference Materials (RMs)These are availabl
47、e from multiple suppliers or can be developed in house. Reference Materialsare typically used in control procedures (verifiers) and in drift correction (standardization) of the spectrometer, and they may beuseful in calibrations. These reference materials shall be homogenous and contain appropriate
48、mass fractions of each element forthe intended purpose. Refer to Guide E2972 for production of your own reference materials.8.3 Several issues can impact the selection and use of CRMs and RMs:8.3.1 Samples and reference materials may exhibit differences in metallurgical structure, in particular havi
49、ng different sizes,compositions, and distributions of inclusions. Inhomogeneous distribution of inclusions can worsen repeatability of individualmeasurements of elements found in the inclusions. Some inclusions may be removed during preburn steps prior to integration ofintensities, causing low results. Typical samples can be used to determine repeatability of individual measurements to yieldestimates consistent with performance for actual samples.8.3.2 For certain elements, there may be no available reference materials with metallurgical structure simil
