1、Designation: E415 08E415 14Standard Test Method forAtomic Emission Vacuum Spectrometric Analysis of Carbonand Low-Alloy Steel by Spark Atomic EmissionSpectrometry1This standard is issued under the fixed designation E415; the number immediately following the designation indicates the year oforiginal
2、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 simultaneous determination of 20 alloyin
3、g and residual elements in carbon and low-alloy steelsin the concentration by spark atomic emission vacuum spectrometry in the mass fraction ranges shown (Note 1).Concentration Range, %Composition Range, %Element Applicable Range,Mass Fraction %AQuantitative Range,Mass Fraction %BAluminum 0 to 0.075
4、 0.02 to 0.075Arsenic 0 to 0.1 0.05 to 0.1Boron 0 to 0.007 0.002 to 0.007Calcium 0 to 0.003 0.001 to 0.003Carbon 0 to 1.1 0.08 to 1.1Chromium 0 to 2.25 0.02 to 2.25Cobalt 0 to 0.18 0.008 to 0.18Copper 0 to 0.5 0.04 to 0.5Manganese 0 to 2.0 0.10 to 2.0Molybdenum 0 to 0.6 0.03 to 0.6Nickel 0 to 5.0 0.
5、02 to 5.0Niobium 0 to 0.085 0.02 to 0.085Nitrogen 0 to 0.015 0.004 to 0.015Phosphorous 0 to 0.085 0.02 to 0.085Silicon 0 to 1.15 0.07 to 1.15Sulfur 0 to 0.055 0.01 to 0.055Tin 0 to 0.045 0.01 to 0.045Titanium 0 to 0.2 0.004 to 0.2Vanadium 0 to 0.3 0.004 to 0.3Zirconium 0 to 0.05 0.02 to 0.05A Applic
6、able range in accordance with Guide E1763 for results reported in accordance with Practice E1950.B Quantitative range in accordance with Practice E1601.NOTE 1The concentration mass fraction ranges of the elements listed have been established through cooperative testing2 of reference materials.Includ
7、ed, in addition to the original data of Test Method E415 71, are data from cooperative testing of a broader range of reference materials to expandthe element concentration mass fraction ranges.1.2 This test method covers analysis of specimens having a diameter adequate to overlap and seal the bore o
8、f the spark standopening (to effect an argon seal). opening. The specimen thickness can vary significantly according to the design of thespectrometer stand, but a thickness between 10 mm and 38 mm has been found to be most practical.1.3 This test method covers the routine control analysis in iron an
9、d 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 applications o
10、f this standard.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 June 1, 2008March 1, 2014. Published July
11、 2008April 2014. Originally approved in 1971. Last previous edition approved in 20052008 asE415 99a (2005).E415 08. DOI: 10.1520/E0415-08.2 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report: RR:E2-1004.This document is not an ASTM st
12、andard 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 editions as appropriate. In all ca
13、ses 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 States11.4 This standard does not purport to address all of the safety concerns, if an
14、y, 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 to use.2. Referenced Documents2.1 ASTM Standards:3E135 Terminology Relating to Analytical Chemistry for
15、 Metals, Ores, and Related MaterialsE158 Practice for Fundamental Calculations to Convert Intensities into Concentrations in Optical Emission SpectrochemicalAnalysis (Withdrawn 2004)4E305 Practice for Establishing and Controlling Atomic Emission Spectrochemical Analytical CurvesE350 Test Methods for
16、 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, Nickel, and Cobalt Alloys b
17、yVarious 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 Results from Interlaborato
18、ry Testing of Chemical Analysis MethodsE1806 Practice for Sampling Steel and Iron for Determination of Chemical CompositionE1950 Practice for Reporting Results from Methods of Chemical Analysis2.2 Other ASTM DocumentsASTM MNL 7 Manual on Presentation of Data and Control Chart Analysis43. Terminology
19、3.1 For definitions of terms used in this test method, refer to Terminology E135.4. Summary of Test Method4.1 A capacitor discharge 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 integra
20、l of a selected iron line, or at a predetermined time, and therelative radiant energies of the analytical lines are recorded. The 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
21、region is overcomeby evacuating the spectrometer and flushing the spark chamber with argon.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
22、all who use this test method will be analysts capable of performingcommon 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 liqui
23、d and solid iron and steel.6.2 Excitation Source, capable of providing electrical 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
24、flat specimen and a lower counter electrode of rod form.NOTE 2Follow the manufacturers recommendations for cleaning the excitation chamber (during continuous operation, this typically should be doneevery 24 h). Follow the manufacturers recommendations for cleaning the entrance lens or window (verifi
25、er data or other reference sample intensity datacan typically indicate when this is necessary).6.3.1 Follow the manufacturers recommendations for cleaning the spark chamber (during continuous operation, this typicallyshould be done every 24 h). Follow the manufacturers recommendations for cleaning t
26、he entrance lens or window (verifier dataor other reference sample intensity data can typically indicate when this is necessary).3 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume informatio
27、n, refer to the standards Document Summary page on the ASTM website.4 The last approved version of this historical standard is referenced on www.astm.org.4 MNL 7A Manual on Presentation of Data and Control Chart Analysis, ASTM Manual Series, ASTM International, 7th ed., 2002. ASTM Manual Series, AST
28、MInternational, 8th edition, 2010.E415 1426.4 Spectrometer, having a reciprocal linear dispersion of 0.60 nm/mm, or better, in the first order and a focal length of 0.75m to 3 m. Its approximate range shall be from 120.0145.0 nm to 400.0 nm. Masks shall be provided in the spectrometer to eliminatesc
29、attered radiation. The spectrometer shall be provided with an air inlet and a vacuum outlet. The spectrometer shall be operatedat a vacuum of 3.33 Pa (25 m of mercury) or below. The primary slit width can range from 20 m to 50 m. Secondary slit widthscan vary (normally between 37 m and 200 m) depend
30、ing on the element wavelength and possible interfering wavelengths.6.5 Measuring System, consisting of photomultipliers (Note 2) having individual voltage adjustments, capacitors in which theoutput of each photomultiplier is stored, a voltage measuring system to register the voltages on the capacito
31、rs either directly orindirectly, and the necessary switching arrangements to provide the desired sequence of operation.NOTE 2Spectrometers equipped with CCD and/or CID detectors may be used provided the user can verify that the data obtained are equivalent tothe precision and bias statistics in this
32、 method.6.6 Vacuum Pump, capable of maintaining a vacuum of 3.33 Pa (25 m Hg) or less.NOTE 3A 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 sequencing shall be provided toact
33、uate the flow at a given rate for a specific time interval. The flow rate may be manually or automatically controlled. The argonsystem shall be in accordance with Practice E406.7. Reagents and Materials7.1 Counter ElectrodesThe counter electrodes can be silver or thoriated tungsten rods, or other ma
34、terial, provided it can beshown experimentally that equivalent precision and bias is obtained. The rods can vary in diameter from 1.5 mm to 6.5 mm(depending on the instrument manufacturer) and typically are machined to a 90 90 or 120 120 angled tip.NOTE 4A black deposit will collect on the tip of th
35、e electrode. This deposit should be removed between specimens (typically with a wire brush). Ifnot removed, it can reduce the overall intensity of the spectral radiation or transfer slight amounts of contamination between specimens, or both. Thenumber of acceptable excitations on an electrode varies
36、 from one instrument to another, and should be established in each laboratory. It has been reportedthat thousands of excitations can be performed on a thoriated tungsten electrode before replacement is necessary.7.1.1 Ablack deposit will collect on the tip of the electrode. This deposit should be re
37、moved 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 excitations on an electrode varies from one instrument to another, andsh
38、ould be established in each laboratory.NOTE 4It has been reported that thousands of excitations 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 Certified Reference Materials (CRMs)Thes
39、e are available from the National Institute of Standards and Technology (NIST)and other sources and span all or part of the concentration mass fraction ranges listed in 1.1. They are used to calibrate thespectrometer for the elements of interest or to validate the performance of the test method. It
40、is not recommended to use CRMsas verifiers or to establish the repeatability of the chemical measurement process. Differences can occur between CRMs andproduction samples prepared by the sampling procedures recommended in this test method. Certain elements (for example, sulfur)calibrations may need
41、to be corrected with values from reference materials made by normal production sampling techniques andanalyzed by Test Methods E350 and E1019.NOTE 5Certified Reference Materials manufactured by NIST are trademarked with the name, “Standard Reference Materials, SRMs.”8.2 Reference Materials (RMs)Thes
42、e are available from multiple suppliers or can be developed in house. RMs are typicallyused to control (verifiers) and drift correct (standardants) the spectrometer. These reference materials shall be homogenous andcontain appropriate concentrationscompositions of each element to be controlled or dr
43、ift corrected, or both.9. Preparation of Specimens and Reference Materials9.1 The specimens and reference materials must be prepared in the same manner. A specimen cut from a large sample sectionmust be of sufficient size and thickness for preparation and to properly fit the spectrometer stand. A 10
44、-mm to 38-mm thickspecimen is normally most practical.9.2 Ensure the specimens are free from voids and pits in the region to be excited (Note 6). Initially grind the surface with a50-grit to 80-grit abrasive belt or disc (wet or dry). Perform the final grind with a dry abrasive belt or disc.Afiner a
45、brasive grindingmedia (for example, 120-grit) may be used for the final grind, but is not essential (essential. Note 7).NOTE 6Specimen porosity is undesirable because it leads to the improper “diffuse-type” rather than the desired “concentrated-type” discharge. Thespecimen surface should be kept cle
46、an because the specimen is the electron emitter, and electron emission is inhibited by oily, dirty surfaces.NOTE 7Reference materials and specimens must be refinished dry on an abrasive belt or disc before being re-excited on the same areaE415 1439.2.1 Reference materials and specimens must be refin
47、ished dry on an abrasive belt or disc before being re-excited on the samearea.TABLE 1 Internal Standard and Analytical LinesElement Wavelength, nm LineClassificationA Possible InterferenceBAluminum 394.40 I V, Mn, Mo, Ni308.22 I V, MnArsenic 197.20 I Mo, W193.76 I MnBoron 182.64 I S, Mn, Mo182.59 I
48、W, Mn, CuCalcium 396.85 II NbCarbon 193.09 I AlChromium 298.92 II Mn, V, Ni, Nb, Mo267.72 II Mn, Mo, WCobalt 345.35 I Cr, Mo228.62 II Ni, CrCopper 327.40 I Nb213.60 II Mo, CrIron (IS) 271.44 II273.07 II CoManganese 293.31 II Cr, Mo, Ni255.86 II ZrMolybdenum 379.83 II Mn277.54 I Cu, V, Co, Mn386.41 I
49、 V, CrNickel 231.60 II Co, Ti227.02 II Nb, WNiobium 319.50 II Mo, Al, VNitrogen 149.26 I Fe, Ti, Si, Mn, Cu, Niand nitride formingelements such as TiPhosphorus 178.29 I MoSilicon 288.16 I Mo, Cr, W251.61 I Fe, VSulfur 180.73 I MnTin 189.99 II Mn, Mo, AlTitanium 337.28 II Nb324.20 II NbVanadium 310.23 II Fe, Mo, Nb, Ni311.07 II Mn, Ti, FeZirconium 343.82 II WA The numerals I or II in the line classification column indicate that the line hasbeen classified in a term array and definitely assigned to the normal atom (I) or tothe singly ionized atom (I
