1、Designation: E 415 99a (Reapproved 2005)Standard Test Method forOptical Emission Vacuum Spectrometric Analysis of Carbonand Low-Alloy Steel1This standard is issued under the fixed designation E 415; the number immediately following the designation indicates the year oforiginal adoption or, in the ca
2、se 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.1. Scope1.1 This test method covers the simultaneous determinationof 20 alloying and residual element
3、s in carbon and low-alloysteels in the concentration ranges shown (Note 1).Concentration Range, %Element Applicable Range, %AQuantitative Range, %BAluminum 0 to 0.075 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 1.1C
4、hromium 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 0.02 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
5、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 0.05AApplicable range in accordance with Guide E 1763 for results reported inaccordance with Practice E 1950.BQuantitative range in accordance wit
6、h Practice E 1601.NOTE 1The concentration ranges of the elements listed have beenestablished through cooperative testing2of reference materials. Included,in addition to the original data of Test Method E 415 71, are data fromcooperative testing of a broader range of reference materials to expand the
7、element concentration ranges.1.2 This test method covers analysis of specimens having adiameter adequate to overlap the bore of the spark standopening (to effect an argon seal). The specimen thicknessshould be between 10 and 38 mm.1.3 This test method covers the routine control analysis ofpreliminar
8、y and ladle tests from either basic oxygen, open-hearth, or electric furnaces and analysis of processed material.It is designed for either chill-cast or rolled and forged speci-mens. The reference materials and specimens should be ofsimilar metallurgical condition and composition.1.4 This standard d
9、oes 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 St
10、andards:3E30 Test Methods for Chemical Analysis of Steel, CastIron, Open-Hearth Iron, and Wrought Iron4E 135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE 158 Practice for Fundamental Calculations to ConvertIntensities into Concentrations in Optical Emission Sp
11、ec-trochemical Analysis4E 305 Practice for Establishing and Controlling Spectro-chemical Analytical CurvesE 350 Test Methods for Chemical Analysis of Carbon Steel,Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, andWrought IronE 406 Practice for Using Controlled Atmospheres in Spec-trochemical
12、 AnalysisE 1019 Test Methods for Determination of Carbon, Sulfur,Nitrogen, and Oxygen in Steel and in Iron, Nickel, andCobalt AlloysE 1329 Practice for Verification and Use of Control Chartsin Spectrochemical AnalysisE 1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance
13、of an Analytical MethodE 1763 Guide for Interpretation and Use of Results fromInterlaboratory Testing of Chemical Analysis MethodsE 1806 Practice for Sampling Steel and Iron for Determi-nation of Chemical Composition1This test method is under the jurisdiction of ASTM Committee E01 onAnalytical Chemi
14、stry for Metals, Ores and Related Materials and is the directresponsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.Current edition approved Jan. 1, 2005. Published March 2005. Originallyapproved in 1971. Last previous edition approved in 1999 as E 415 99a.2Supporting data have been f
15、iled at ASTM International Headquarters and maybe obtained by requesting Research Report RR: E2-1004.3For 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 D
16、ocument Summary page onthe ASTM website.4Withdrawn.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.E 1950 Practice for Reporting Results from Methods ofChemical Analysis3. Terminology3.1 For definitions of terms used in this test met
17、hod, refer toTerminology E 135.4. Summary of Test Method4.1 The most sensitive lines of arsenic, boron, carbon,nitrogen, phosphorus, sulfur, and tin lie in the vacuum ultra-violet region. The absorption of the radiation by air in thisregion is overcome by evacuating the spectrometer and flush-ing th
18、e spark chamber with argon. A capacitor discharge isproduced between the flat, ground surface of the disk specimenand a conically shaped electrode. The discharge is terminatedat a predetermined intensity time integral of a selected ironline, or at a predetermined time, and the relative radiantenergi
19、es or concentrations of the analytical lines are recorded.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 b
20、e analysts capable ofperforming common laboratory procedures skillfully andsafely. It is expected that work will be performed in a properlyequipped laboratory.6. Apparatus6.1 Sample Preparation Equipment:6.1.1 Sample Mold, capable of producing castings that arehomogeneous and free from voids and por
21、osity. Refer toPractice E 1806 for steel sampling procedures. The followingmold types have been found to produce acceptable samples:6.1.1.1 Cast Iron MoldA mold 70 mm (234 in.) deep, 64mm (212 in.) in diameter at the top of the mold, and 57 mm(214 in.) in diameter at the bottom of the mold. The wall
22、thickness of the mold is approximately 32 mm (114 in.).6.1.1.2 Refractory Mold RingA mold that has a minimuminside diameter of 32 mm (114 in.) and a minimum height of 25mm (1 in.). The ring is placed on a flat surface of a copper plateapproximately 50 mm (2 in.) thick.6.1.1.3 Book-Type Steel or Copp
23、er Mold, to produce achill-cast disk 64 mm (212 in.) in diameter and 13 mm (12 in.)thick.6.2 Excitation Source, capable of providing a triggeredcapacitor discharge having source parameters meeting therequirements of 11.1.6.3 Spark Chamber, automatically flushed with argon. Thespark chamber shall be
24、mounted directly on the spectrometer,and shall be provided with a spark stand to hold a flat specimenand a lower electrode of rod form.NOTE 2Clean the excitation chamber when the counter electrode isreplaced. Clean the lens or protective window after approximately 200 to300 excitations to minimize t
25、ransmission losses.6.4 Spectrometer, having a reciprocal linear dispersion of0.60 nm/mm, or better, in the first order and a focal length of0.75 to 3 m. Its approximate range shall be from 120.0 to 400.0nm. Masks shall be provided in the spectrometer to eliminatescattered radiation. The spectrometer
26、 shall be provided with anair inlet and a vacuum outlet. The spectrometer shall beoperated at a vacuum of 25 m of mercury or below. Theprimary slit width is 20 to 50 m. Secondary slit width is 50 to200 m.6.5 Measuring System, consisting of photomultipliers hav-ing individual voltage adjustments, cap
27、acitors in which theoutput of each photomultiplier is stored, a voltage measuringsystem to register the voltages on the capacitors either directlyor indirectly, and the necessary switching arrangements toprovide the desired sequence of operation.6.6 Vacuum Pump, capable of maintaining a vacuum of 25
28、m Hg.NOTE 3A pump with a displacement of at least 0.23 m3/min (8ft3/min) is usually adequate.6.7 Flushing System, consisting of argon tanks, a pressureregulator, and a gas flowmeter. Automatic sequencing shall beprovided to actuate the flow of argon at a given flow rate for agiven time interval and
29、to start the excitation at the end of theflush period. Means of changing the flow rate of argon shall beprovided. The flushing system shall be in accordance withPractice E 406.7. Reagents and Materials7.1 Counter ElectrodesThe counter electrodes shall be6.4-mm (14-in.) in diameter, hard-drawn, fine,
30、 silver rods,1.5-mm (116-in.) thoriated, tungsten rods, or other materialprovided it can be shown experimentally that equivalentprecision and bias is obtained. Machine the rods to a 90 or 120cone.NOTE 4A black deposit builds up on the tip of the electrode, thusreducing the overall intensity of the s
31、pectral radiation. In general thiscondition will not affect analytical performance for the first 40 or 50excitations, after which time a freshly prepared counter electrode shouldbe installed. The number of acceptable excitations on an electrode variesfrom one instrument to another, and should be est
32、ablished in eachlaboratory. With a thoriated tungsten electrode, it has been reported that ahundred or more excitations can usually be made before replacement.7.2 Inert Gas, Argon, in accordance with Practice E 406.8. Reference Materials8.1 Certified Reference Materials (CRMs) are availablefrom the
33、National Institute of Standards and Technology andother sources. These cover all or part of the concentrationranges listed in 1.1. They are valuable in establishing prelimi-nary working curves and determining the precision of theinstrument. However, because of differences between theseCRMs and the p
34、roduction specimens prepared by the samplingprocedures recommended for this test method, curves based onCRMs may (in very unusual circumstances) need to becorrected with values from reference materials made by normalproduction sampling techniques and analyzed in accordancewith Test Methods E30, E 35
35、0, and E 1019.8.2 Reference MaterialsPeriodically check the instrumentfor drift. For this purpose, verifiers and standardants areemployed. These reference materials shall be homogeneousand contain appropriate amounts of each element, covering theconcentration range of elements contained in the speci
36、mens.E 415 99a (2005)29. Preparation of Specimens and Reference Materials9.1 Use cast or rolled and forged samples. Cut a 13 to25-mm (12 to 1-in.) thick slice from the sample or obtain aninitial smooth flat surface by machining at least 1.3 mm (0.05in.) off the original surface using a lathe or grin
37、der. Makecertain that the specimens are homogeneous and free fromvoids and pits in the region to be excited (Note 5). Rough grindthe cut surface by grinding on a belt surfacer, either wet or dry,with 50 to 80-grit abrasive belt. Obtain the final surface by drygrinding. A finer abrasive belt, such as
38、 120-grit, may be usedfor final dry grinding, but is not essential (Note 6).NOTE 5Specimen porosity is undesirable because it leads to theimproper “diffuse-type” rather than the desired “concentrated-type” dis-charge. The specimen surface should be kept clean because the specimenis the electron emit
39、ter, and electron emission is inhibited by oily, dirtysurfaces.NOTE 6Reference materials and specimens shall be refinished dry ona belt sander before being re-excited on the same area.10. Preparation of ApparatusNOTE 7The instructions given in this test method apply to mostspectrometers; however, so
40、me settings and adjustments may need to bevaried, and additional preparation of the equipment may be required. It isnot within the scope of an ASTM test method to prescribe the minutedetails of the apparatus preparation, which may differ not only for eachmanufacturer, but also for different equipmen
41、t from the same manufac-turer. For a description of and further details of operation of a particularspectrometer, refer to the manufacturers handbook.10.1 Program the spectrometer to accommodate the internalstandard lines and one of the analytical lines for each elementlisted in Table 1.NOTE 8The li
42、nes listed in Table 1 have proven satisfactory for theelements and concentration ranges described in the scope. Other internalstandard and analytical lines, such as those listed in Table 2, may be usedprovided that it can be shown experimentally that equivalent precision andaccuracy are obtained.10.
43、2 Position or test the position of the spectrometer exitslits to ensure that peak radiation passes through each slit andis incident on the photomultiplier. This shall be done initiallyand as often as necessary thereafter to maintain proper align-ment.NOTE 9The manner and frequency of positioning or
44、checking theposition of the exit slits will depend on factors such as: the type ofspectrometer, the variety of analytical problems encountered, and thefrequency of use. Each laboratory should establish a suitable checkprocedure.11. Excitation and Exposure11.1 Electrical Parameters (Note 10):11.1.1 S
45、elect excitation parameters within the followingrangesTriggered Capacitor DischargeCapacitance, F 10to15Inductance, H 50to70Resistance, V 3to5Potential, V 940 to 1000Current, A, r-f 0.3 to 0.8Number of discharge/s 60NOTE 10When parameter values are established, maintain themcarefully. The variation
46、of the power supply voltage shall not exceed65 % and preferably should be held within 62%.11.1.2 Initiation CircuitThe initiator circuit parametersshall be adequate to uniformly trigger the capacitor discharge.Nominal values found to be adequate are listed as follows:TABLE 1 Internal Standard and An
47、alytical LinesElement Wavelength, nmLineClassificationAPossible 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 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
48、.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 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, Nia
49、nd 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 WAThe 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 (II).BInterferences are dependent upon instrument design, spectrum line choices,and excitation conditions, and those
