1、Designation: E 2209 02 (Reapproved 2006)2Standard 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 r
2、evision, 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.1NOTEUpdated Section 2 Referenced Documents in December 2006.2NOTEAdded research report footnote to Section 1
3、6 editorially in April 2009.1. Scope1.1 This test method provides for the 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)
4、0.3 to 1.4Chromium (Cr) 0.25 to 2.00Manganese (Mn) 8.0 to 16.2Molybdenum (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 higherconcent
5、rations by the use of suitable reference materials. Sulfur is notincluded 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 o
6、f the safety concerns, if any, associated with itsuse. It is the responsibility 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 Specificati
7、on for Steel Castings, AusteniticManganeseE 135 Terminology Relating to Analytical 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 Spe
8、cifying the ExcitationSource in Emission Spectrochemical Analysis4E 305 Practice for Establishing and Controlling AtomicEmission Spectrochemical Analytical CurvesE 353 Test Methods for Chemical Analysis of Stainless,Heat-Resisting, Maraging, and Other Similar Chromium-Nickel-Iron AlloysE 406 Practic
9、e for Using Controlled Atmospheres in Spec-trochemical AnalysisE 876 Practice for Use of Statistics in the Evaluation ofSpectrometric Data4E 1019 Test Methods for Determination of Carbon, Sulfur,Nitrogen, and Oxygen in Steel, Iron, Nickel, and CobaltAlloys by Various Combustion and Fusion Techniques
10、E 1059 Practice for Designating Shapes and Sizes of Non-graphite Counter ElectrodesE 1601 Practice for Conducting an Interlaboratory 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 M
11、anual on Presentation of Data and Control ChartAnalysis, ASTM MNL 7A, seventh revision, 2002.3. Terminology3.1 For definition 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 counte
12、r electrode. The radiantenergies of selected analytical lines are converted into electri-cal energies by photo-multiplier tubes and stored on capacitors.1This test method is under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and Related Materials and is the directr
13、esponsibility 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 International Headquarters and maybe obtained
14、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 onthe ASTM website.4Withdrawn. The la
15、st approved version of this historical standard is referencedon www.astm.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.This discharge is terminated after a fixed exposure time. At theend of the exposure period, the charge on ea
16、ch capacitor ismeasured, and converted to concentration.5. Significance and Use5.1 The chemical composition of high manganese steelalloys must be determined accurately to ensure the desiredmetallurgical properties. This procedure is suitable for manu-facturing control and inspection testing.6. Inter
17、ferences6.1 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 interferences may be determined and propercorrections made by the use of various reference mat
18、erials. 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, mathematical corrections may beused to solve for interelement effects (refer to Practice
19、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 Preparation Equipment:7.1.1 Sample Mold, to produce chilled cast samples approxi-mately 38 mm (
20、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 Immersion Sampler, to take a sample from the bath orfrom the metal stream when pouring can
21、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 materials and specimens. The following table showsthe various methods of sample preparation used
22、 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 but it was notutilized by the laboratories in the Inter-Laboratory Study (ILS).7.2 Excit
23、ation 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 surface for the specimen in opposition toa counter electrode. This stand shall provide an
24、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 spectrum of a specimen in the spectral region170.0 to 450 nm. The spectrometer shall have
25、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 voltage adjustment, capacitors on which theoutput of each photo-multiplier tube is stored and
26、 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, capable of maintaining avacuum of approximately 3 Pa. There are some equipmentmanufactures tha
27、t 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 this method.7.7 Flushing System, consisting of argon tanks, a pressureregulator, and a g
28、as 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 system shall be in accor-dance with Practice E 406.8. Reagents and Materials8.1 Argon, eith
29、er 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 ElectrodeA Tungsten or Thoriated Tungstenrod ground to a 15, 30, 45 or 90 angle conical tip, whic
30、hconforms to Practice E 1059, was found satisfactory.9. Reference Materials9.1 Certified Reference Materials, for high manganese steelare commercially available.TABLE 1 WavelengthsElementWavelength(nm)LineClassificationPossibleInterferencesAAluminum 394.4 I V, Mn, Mo396.152 I MoCarbon 193.09 I AlChr
31、omium 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 MoSilicon 212.41 I288.16 I M
32、o, 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 theinterferences that these lines
33、 may have. Care should be taken to address theinterferences when calibrating the instrument.E 2209 02 (2006)229.2 Calibrants shall be certified reference materials fromrecognized certification agencies. They shall cover the concen-tration ranges of the elements to be determined and shallinclude all
34、of the specific types of alloys being analyzed. Thecalibrants shall be homogeneous and free of voids and porosity.The metallurgical history of the calibrants should be similar tothat of the specimens being analyzed. Refer to Test MethodsE 353 and E 1019 for chemical analysis of high manganesesteel a
35、lloys.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 between elements in the calibrants.10. Preparation of Calibrants and Specimens10.1 Rough grind,
36、 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 that the speci-mens are homogeneous and free from voids and pits in theregion to be excit
37、ed. 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. Excitation and Exposure11.1 Be certain the spectrometer is in optical alignment andhas been c
38、alibrated 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 15Inductance, :H 50 to 70Resistance, S residual to 5Potential, V 940 to 1000Peak Current, A 10
39、0 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 Exposure Conditions:Exposure ConditionsFlush Time 2 to 5 sPreburn 10 to 30 sExposure 5 to
40、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 adequate are listed as follows:Capacitance (d-c charged) :F 1.2Inductance, :H residualResi
41、stance, 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-mentally that equivalent precision and accuracy are obtained.11.5 Electrode SystemInsert th
42、e 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 discharge sourcesin todays spectrometers are either the directional self-initiatingcapacit
43、or 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 with the manu-facturers instructions.NOTE 3It is not within the scope of this method to
44、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 and potential standardants in a randomsequence, bracketing these burns with excitations of
45、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 concentration range. Make replicate exposures inaccordance with 14.2. Using the averages of t
46、he 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 known or suspected that readings have shifted. Make thenecessary corrections either by adju
47、sting 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 done at least at the beginning ofany analytical work. Analyze verifiers in replicate to
48、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 obtained, standardize again and/or investigatewhy confirmation is not obtained. Standardiza
49、tion 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 notin 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
