1、Designation: E 415 08Standard Test Method forAtomic 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 case of revision, the
2、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 determinationof 20 alloying and residual elements in carbon and low-a
3、lloysteels 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 1.1Chromium 0 to 2.25 0.0
4、2 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 to 1.15Sulfur 0 to 0.
5、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 with Practice E 1601.NOT
6、E 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 theelement concentration
7、 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 thickness canvary significantly according to the design of the spectrometerstand, but a thickness between 10 mm and 38 mm has been
8、found to be most practical.1.3 This test method covers the routine control analysis iniron and steelmaking 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
9、 metallurgical conditionand composition. However, it is not required for all applica-tions of this standard.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
10、and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:3E 135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE 158 Practice for Fundamental Calculations to ConvertIntensities into Conc
11、entrations in Optical Emission Spec-trochemical Analysis4E 305 Practice for Establishing and Controlling AtomicEmission Spectrochemical Analytical CurvesE 350 Test Methods for Chemical Analysis of Carbon Steel,Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, andWrought IronE 406 Practice for U
12、sing Controlled Atmospheres in Spec-trochemical 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 In
13、terlaboratory Study toEvaluate the Performance 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 jurisd
14、iction 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 June 1, 2008. Published July 2008. Originally approvedin 1971. Last previous edition approved in
15、2005 as E 415 99a (2005).2Supporting data have been filed 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 ASTMS
16、tandards volume information, refer to the standards Document 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. Terminol
17、ogy3.1 For definitions of terms used in this test method, refer toTerminology E 135.4. Summary of Test Method4.1 A capacitor discharge is produced between the flat,ground surface of the disk specimen and a conically shapedelectrode. The discharge is terminated at a predeterminedintensity time integr
18、al of a selected iron line, or at a predeter-mined time, and the relative radiant energies of the analyticallines are 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 this
19、region is overcome by evacuating the spectrometer and flush-ing the spark 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
20、all who use this test method will be analysts capable ofperforming 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 E 1806 for devices and practices tosample liquid
21、and solid iron and steel.6.2 Excitation Source, capable of providing 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 fl
22、at specimenand a lower counter electrode of rod form.NOTE 2Follow the manufacturers recommendations for cleaning theexcitation chamber (during continuous operation, this typically should bedone every 24 h). Follow the manufacturers recommendations forcleaning the entrance lens or window (verifier da
23、ta or other referencesample intensity data can typically indicate when this is necessary).6.4 Spectrometer, having a reciprocal linear dispersion of0.60 nm/mm, or better, in the first order and a focal length of0.75 m to 3 m. Its approximate range shall be from 120.0 nmto 400.0 nm. Masks shall be pr
24、ovided in the spectrometer toeliminate scattered radiation. The spectrometer shall be pro-vided with an air inlet and a vacuum outlet. The spectrometershall be operated at a vacuum of 3.33 Pa (25 m of mercury)or below. The primary slit width can range from 20 mto50m. Secondary slit widths can vary (
25、normally between 37 mand 200 m) depending on the element wavelength andpossible interfering wavelengths.6.5 Measuring System, consisting of photomultipliers hav-ing individual voltage adjustments, capacitors in which theoutput of each photomultiplier is stored, a voltage measuringsystem to register
26、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 3.33Pa (25 m Hg) or less.NOTE 3A pump with a displacement of at least 0.23 m3/min (8ft3/min) is usuall
27、y adequate.6.7 Gas 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 controlled. Theargon system shall be in accordance with Prac
28、tice E 406.7. Reagents and Materials7.1 Counter ElectrodesThe counter electrodes can besilver or thoriated tungsten rods, or other material, provided itcan be shown experimentally that equivalent precision and biasis obtained. The rods can vary in diameter from 1.5 mm to 6.5mm (depending on the inst
29、rument manufacturer) and typicallyare machined to a 90 or 120 angled tip.NOTE 4A black deposit will collect on the tip of the electrode. Thisdeposit should be removed between specimens (typically with a wirebrush). If not removed, it can reduce the overall intensity of the spectralradiation or trans
30、fer slight amounts of contamination between specimens,or both. The number of acceptable excitations on an electrode varies fromone instrument to another, and should be established in each laboratory. Ithas been reported that thousands of excitations can be performed on athoriated tungsten electrode
31、before replacement is necessary.7.2 Inert Gas, Argon, in accordance with Practice E 406.8. 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 concen-tration ranges
32、 listed in 1.1. They are used to calibrate thespectrometer for the elements of interest or to validate theperformance of the test method. It is not recommended to useCRMs as verifiers or to establish the repeatability of thechemical measurement process. Differences can occur betweenCRMs and producti
33、on samples prepared by the samplingprocedures recommended in this test method. Certain el-ements (for example, sulfur) calibrations may need to becorrected with values from reference materials made by normalproduction sampling techniques and analyzed by Test MethodsE 350 and E 1019.NOTE 5Certified R
34、eference Materials manufactured by NIST aretrademarked with the name, “Standard Reference Materials, SRMs.”8.2 Reference Materials (RMs)These are available frommultiple suppliers or can be developed in house. RMs aretypically used to control (verifiers) and drift correct (standar-dants) the spectrom
35、eter. These reference materials shall behomogenous and contain appropriate concentrations of eachelement to be controlled or drift corrected, or both.9. Preparation of Specimens and Reference Materials9.1 The specimens and reference materials must be preparedin the same manner. A specimen cut from a
36、 large samplesection must be of sufficient size and thickness for preparationE415082and to properly fit the spectrometer stand. A 10 mm to 38-mmthick specimen is normally most practical.9.2 Ensure the specimens are free from voids and pits in theregion to be excited (Note 6). Initially grind the sur
37、face with a50-grit to 80-grit abrasive belt or disc (wet or dry). Perform thefinal grind with a dry abrasive belt or disc. A finer abrasivegrinding media (for example, 120-grit) may be used for thefinal grind, but is not essential (Note 7).NOTE 6Specimen porosity is undesirable because it leads to t
38、heimproper “diffuse-type” rather than the desired “concentrated-type” dis-charge. The specimen surface should be kept clean because the specimenis the electron emitter, and electron emission is inhibited by oily, dirtysurfaces.NOTE 7Reference materials and specimens must be refinished dry onan abras
39、ive belt or disc before being re-excited on the same area10. Preparation of ApparatusNOTE 8The instructions given in this test method apply to mostspectrometers; however, some settings and adjustments may need to bevaried, and additional preparation of the equipment may be required. It isnot within
40、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 equipment from the same manufac-turer. For a description of and further details of operation of a particularspectrometer, refer to the
41、manufacturers handbook.10.1 Program the spectrometer to accommodate the internalstandard lines and one of the analytical lines for each elementlisted in Table 1. Multiple lines may be used for a givenelement (for example, nickel) depending on the concentrationrange and the individual spectrometer so
42、ftware.NOTE 9The lines 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 andaccura
43、cy are obtained.10.2 Test the positioning of the spectrometer entrance slit toensure that peak radiation is entering the spectrometer cham-ber. This shall be done initially and as often as necessary tomaintain proper entrance slit alignment. Follow the manufac-turers recommended procedures. The labo
44、ratory will deter-mine the frequency of positioning the alignment based oninstrument performance.10.3 Exit slit positioning and alignment is normally per-formed by the manufacturer at spectrometer assembly. Undernormal circumstances, further exit slit alignment is not neces-sary (Note 10).NOTE 10The
45、 manner and frequency of positioning or 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 utilizing qualified service engi
46、neers.11. Excitation and Exposure11.1 Electrical Parameters (Note 11):11.1.1 Excitation parameters are normally established bythe spectrometer manufacturer. The following ranges are his-torical guidelines and newer instruments may vary from these.Triggered Capacitor DischargeCapacitance, F 10to15Ind
47、uctance, H 50to70Resistance, V 3to5Potential, V 940 to 1000TABLE 1 Internal Standard and Analytical 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.
48、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 V, CrNickel 231.60 I
49、I 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 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 depen
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