1、Designation: E 2209 02 (Reapproved 2006)e1Standard Test Method forAnalysis of High Manganese Steel Using Atomic EmissionSpectrometry1This standard is issued under the fixed designation E 2209; the number immediately following the designation indicates the year oforiginal adoption or, in the case of
2、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.e1NOTEUpdated Section 2 Reference Documents in December 2006.1. Scope1.1 This test method provides for the
3、analysis of highmanganese steel by atomic emission spectrometry using thepoint-to-plane technique for the following elements in theconcentration ranges shown:Elements Concentration Range, %Aluminum (Al) 0.02 to 0.15Carbon (C) 0.3 to 1.4Chromium (Cr) 0.25 to 2.00Manganese (Mn) 8.0 to 16.2Molybdenum (
4、Mo) 0.03 to 2.0Nickel (Ni) 0.05 to 4.0Phosphorus (P) 0.025 to 0.06Silicon (Si) 0.25 to 1.5NOTE 1The ranges represent the actual levels at which this methodwas tested.2These concentration ranges can be extended to higherconcentrations by the use of suitable reference materials. Sulfur is notincluded
5、because differences in results between laboratories exceededacceptable limits at all analyte levels.1.2 This test method may involve hazardous materials,operations, and equipment. This standard does not purport toaddress all of the safety concerns, if any, associated with itsuse. It is the responsib
6、ility of the user of this standard toestablish appropriate safety and health practices and deter-mine the applicability of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:3A 128/A 128M Specification for Steel Castings, AusteniticManganeseE 135 Terminology Relating to An
7、alytical Chemistry forMetals, Ores, and Related MaterialsE 158 Practice for Fundamental Calculations to ConvertIntensities into Concentrations in Optical Emission Spec-trochemical Analysis4E 172 Practice for Describing and Specifying the ExcitationSource in Emission Spectrochemical Analysis4E 305 Pr
8、actice for Establishing and Controlling Spectro-chemical Analytical Curves4E 353 Test Methods for Chemical Analysis of Stainless,Heat-Resisting, Maraging, and Other Similar Chromium-Nickel-Iron AlloysE 406 Practice for Using Controlled Atmospheres in Spec-trochemical AnalysisE 876 Practice for Use o
9、f Statistics in the Evaluation ofSpectrometric Data4E 1019 Test Methods for Determination of Carbon, Sulfur,Nitrogen, and Oxygen in Steel and in Iron, Nickel, andCobalt AlloysE 1059 Practice for Designating Shapes and Sizes of Non-graphite Counter ElectrodesE 1601 Practice for Conducting an Interlab
10、oratory Study toEvaluate the Performance of an Analytical MethodE 1806 Practice for Sampling Steel and Iron for Determi-nation of Chemical Composition2.2 Other Document:ASTM Manual on Presentation of Data and Control ChartAnalysis, ASTM MNL 7A, seventh revision, 2002.3. Terminology3.1 For definition
11、 of terms used in this method, refer toTerminology E 135.4. Summary of Test Method4.1 A controlled discharge is produced between the flatsurface of the specimen and the counter electrode. The radiantenergies of selected analytical lines are converted into electri-cal energies by photo-multiplier tub
12、es and stored on capacitors.This discharge is terminated after a fixed exposure time. At theend of the exposure period, the charge on each capacitor ismeasured, and converted to concentration.1This test method is under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores an
13、d Related Materials and is the directresponsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.Current edition approved Nov. 1, 2006. Published November 2006. Originallyapproved in 2002. Last previous edition approved in 2002 as E 2209 02.2Supporting data have been filed at ASTM Internat
14、ional Headquarters and maybe obtained by requesting Research Report RR: E01-1035.3For 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 Document Summary page
15、 onthe ASTM website.4Withdrawn.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5. Significance and Use5.1 The chemical composition of high manganese steelalloys must be determined accurately to ensure the desiredmetallurgical propert
16、ies. This procedure is suitable for manu-facturing control and inspection testing.6. Interferences6.1 Interferences may vary with spectrometer design andexcitation characteristics. Direct spectral interferences may bepresent on one or more of the wavelengths listed in a method.Frequently, these inte
17、rferences may be determined and propercorrections made by the use of various reference materials. Thecomposition of the sample being analyzed should matchclosely the composition of one or more of the referencematerials used to prepare and control the calibration curve thatis employed. Alternatively,
18、 mathematical corrections may beused to solve for interelement effects (refer to Practice E 158).Various mathematical correction procedures are commonlyutilized. Any of these are acceptable that will achieve analyti-cal accuracy equivalent to that provided by this method.7. Apparatus7.1 Sample Prepa
19、ration Equipment:7.1.1 Sample Mold, to produce chilled cast samples approxi-mately 38 mm (112 in) in diameter that are homogeneous, freeof voids or porosity in the region to be excited, and represen-tative of the material to be analyzed. Refer to Practice E 1806for steel sampling procedures.7.1.2 Im
20、mersion Sampler, to take a sample from the bath orfrom the metal stream when pouring can be used. The sampleshould produce a sample of the same dimensions as listed in7.1.1.7.1.3 Surface Grinder or Sander With Abrasive Belts orDisk, capable of providing a flat uniform surface on thereference materia
21、ls and specimens. The following table showsthe various methods of sample preparation used in the Inter-Laboratory Study (ILS):Type of Grinding Preparation Belt and/or DiskGrinding Medium Aluminum Oxide, Zirconium OxideGrit of Grinding Medium 36 to 180NOTE 2Silicon carbide grinding medium may be used
22、 but it was notutilized by the laboratories in the Inter-Laboratory Study (ILS).7.2 Excitation Source, capable of providing a triggeredcapacitor discharge having the source parameters meeting therequirements of 11.1.7.3 Excitation Stand, suitable for mounting in optical emis-sion alignment, a flat s
23、urface for the specimen in opposition toa counter electrode. This stand shall provide an atmosphere ofargon. The electrode and argon are described in 8.1 and 8.2.7.4 Spectrometer, having sufficient resolving power andlinear dispersion to separate clearly the analytical lines fromother lines in the s
24、pectrum of a specimen in the spectral region170.0 to 450 nm. The spectrometer shall have a dispersion ofat least 2 nm/mm and a focal length of at least 0.5 m. Gaspurged spectrometers are an alternative to vacuum systems.7.5 Measuring System, consisting of photo-multiplier tubeshaving individual volt
25、age adjustment, capacitors on which theoutput of each photo-multiplier tube is stored and an electronicsystem to measure voltages on the capacitors either directly orindirectly, and the necessary switching arrangements to pro-vide the desired sequence of operation.7.6 Vacuum Pump, if required, capab
26、le of maintaining avacuum of approximately 3 Pa. There are some equipmentmanufactures that will purge the optical portion of the spec-trometer with argon or other inert gas rather than pull a vacuumon the optics. Either vacuum optics or purged optics arerequired to determine carbon and phosphorus in
27、 this method.7.7 Flushing System, consisting of argon tanks, a pressureregulator, and a gas flow meter. Automatic sequencing shall beprovided to actuate the flow of argon at a given flow rate for agiven time interval and to start the excitation at the end of therequired flush period. The flushing sy
28、stem shall be in accor-dance with Practice E 406.8. Reagents and Materials8.1 Argon, either gaseous or liquid, must be of sufficientpurity to permit proper excitation of the analytical lines ofinterest. Argon of 99.998% purity has been found satisfactory.Refer to Practice E 406.8.2 Counter Electrode
29、A Tungsten or Thoriated Tungstenrod ground to a 15, 30, 45 or 90 angle conical tip, whichconforms to Practice E 1059, was found satisfactory.9. Reference Materials9.1 Certified Reference Materials, for high manganese steelare commercially available.9.2 Calibrants shall be certified reference materia
30、ls fromrecognized certification agencies. They shall cover the concen-tration ranges of the elements to be determined and shallinclude all of the specific types of alloys being analyzed. TheTABLE 1 WavelengthsElementWavelength(nm)LineClassificationPossibleInterferencesAAluminum 394.4 I V, Mn, Mo396.
31、152 I MoCarbon 193.09 I AlChromium 298.92 II Mn, V, Ni, Nb, Mo267.72 II Mn, Mo, V425.435 IIron (Internal Standard) 273.07 I271.44 IIManganese 263.81 II290.02 II293.31 II CrMolybdenum 202.03 II263.876 II281.61 II Al, Mn386.41 I V, CrNickel 231.60 II Co, Ti218.54 II352.45 I341.476 IPhosphorus 178.29 I
32、 MoSilicon 212.41 I288.16 I Mo, Cr, W251.61 I Fe, VSulfur 180.73 I MnAInterferences are dependent upon instrument design, and excitation condi-tions, and those listed require confirmation based upon specimens designed todemonstrate interferences. This standard method does not purport to address thei
33、nterferences that these lines may have. Care should be taken to address theinterferences when calibrating the instrument.E 2209 02 (2006)e12calibrants shall be homogeneous and free of voids and porosity.The metallurgical history of the calibrants should be similar tothat of the specimens being analy
34、zed. Refer to Test MethodsE 353 and E 1019 for chemical analysis of high manganesesteel alloys.9.2.1 In selecting calibrants, use caution with compositionsthat are unusual. One element may influence the radiant energyof another element. Tests should be made to determine ifinterrelations exist betwee
35、n elements in the calibrants.10. Preparation of Calibrants and Specimens10.1 Rough grind, either wet or dry, with a coarse grindingbelt or disk. The final grind of the specimen must be the samegrit as the calibrants. Dry the specimens, if wet, for properexcitation in the argon atmosphere. Make sure
36、that the speci-mens are homogeneous and free from voids and pits in theregion to be excited. Cast specimens from molten metal into asuitable mold and cool. Immersion and stream samplers arealso suitable for use. Prepare the surface of the specimens andreference materials in a similar manner.11. Exci
37、tation and Exposure11.1 Be certain the spectrometer is in optical alignment andhas been calibrated according to the manufacturers instruc-tions.11.1.1 Electrical ParametersElectrical parameters withinthe following ranges were found acceptable.Triggered Capacitor DischargeCapacitance, :F 2.5 to 15Ind
38、uctance, :H 50 to 70Resistance, S residual to 5Potential, V 940 to 1000Peak Current, A 100 to 275Current pulse duration, :s 130 to 250Number of discharges/s 60 to 12011.2 Spectrometer Configurations:Spectrometer ParametersFocal Length 0.5 m to 1.2 mDispersion 0.5 to 2.16 nm/mmVacuum 1 to 25 Pa11.3 E
39、xposure Conditions:Exposure ConditionsFlush Time 2 to 5 sPreburn 10 to 30 sExposure 5 to 20 s11.4 Initiation CircuitThe initiator circuit parametersshall be adequate to uniformly trigger the capacitor discharge.The values for these parameters will vary with the instrument.Normal values found to be a
40、dequate are listed as follows:Capacitance (d-c charged) :F 1.2Inductance, :H residualResistance, S residualPotential, V 42511.4.1 Other Electrical ParametersExcitation units, onwhich the precise parameters given in 11.1.1 and 11.4 are notavailable, may be used provided that it can be shown experi-me
41、ntally that equivalent precision and accuracy are obtained.11.5 Electrode SystemInsert the counter electrode in thelower electrode position. Adjust the analytical gap to 3, 4, 5, or7 mm depending on the manufacturers recommendations forthat particular instrument.11.6 Discharge SourceMost capacitor d
42、ischarge sourcesin todays spectrometers are either the directional self-initiatingcapacitor discharge source or a triggered capacitor dischargesource. Refer to Practice E 172 for a more detailed explanationof these sources.12. Preparation of Instrumentation12.1 Prepare the spectrometer in accordance
43、 with the manu-facturers instructions.NOTE 3It is not within the scope of this method to prescribe all detailsof equipment to be used. Equipment varies between laboratories.13. Calibration, Standardization, and Verification13.1 CalibrationUsing the conditions given in 11.3, ex-cite the calibrants an
44、d potential standardants in a randomsequence, bracketing these burns with excitations of anymaterials intended for use as verifiers. (A verifier may be usedas a calibrant even though it is burned only as a verifier.) Thereshould be at least five calibrants for each element, spanning therequired conc
45、entration range. Make replicate exposures inaccordance with 14.2. Using the averages of the data for eachpoint, determine analytical curves as described in PracticesE 305 and E 158.13.2 StandardizationFollowing the manufacturers rec-ommendations, standardize on an initial setup and anytime thatis kn
46、own or suspected that readings have shifted. Make thenecessary corrections either by adjusting the controls on thereadout or by applying mathematical corrections. Standardiza-tion shall be done anytime verifications indicate that readingshave gone out of statistical control.13.3 VerificationShall be
47、 done at least at the beginning ofany analytical work. Analyze verifiers in replicate to confirmthat they read within expected confidence interval, as definedin 13.4. The replication shall be the same as recommended in14.2.13.3.1 Check the verification after standardizing. If confir-mation is not ob
48、tained, standardize again and/or investigatewhy confirmation is not obtained. Standardization is confirmedif the results are within two standard deviations from the meanof the standard.13.3.2 Repeat the verification at least every4horiftheinstrument has been idle for more than 1 h. If readings are n
49、otin conformance, repeat the standardization.13.4 The confidence interval will be established from ob-servations of the repeatability of the verifiers and determiningthe confidence interval for some acceptable confidence level asprescribed in Practice E 876 or by establishing the upper andlower limit of a control chart as prescribed in ASTM ManualMNL 7A. The latter is the preferable approach since it alsomonitors the consistency of the statistics of the measurementsand provides a means of maintaining a record of performance.14. Measurement Procedure for Excitation
