1、Designation: E2209 02 (Reapproved 2006)2E2209 13Standard Test Method forAnalysis of High Manganese Steel Using by Spark AtomicEmission Spectrometry1This standard is issued under the fixed designation E2209; the number immediately following the designation indicates the year oforiginal adoption or, i
2、n 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 NOTEUpdated Section 2 Referenced Documents in December 2006.2 NOTEAdded research report foot
3、note to Section 16 editorially in April 2009.1. Scope1.1 This test method provides for the analysis of high manganese steel by spark atomic emission spectrometry using thepoint-to-plane technique for the following elements in the concentration ranges shown:Elements Concentration Range, %Elements Con
4、position 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 (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 method was tested.2 The
5、se concentrationcomposition ranges can be extended to higherconcentrationscompositions by the use of suitable reference materials. Sulfur is not included because differences in results between laboratories exceededacceptable limits at all analyte levels.1.2 This test method may involve hazardous mat
6、erials, operations, and equipment. This standard does not purport to addressall of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriatesafety and health practices and determine the applicability of regulatory limitations
7、 prior to use.2. Referenced Documents2.1 ASTM Standards:3A128/A128M Specification for Steel Castings, Austenitic ManganeseE135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials1 This test method is under the jurisdiction of ASTM Committee E01 on Analytical Chemistr
8、y for Metals, Ores, and Related Materials and is the direct responsibility ofSubcommittee E01.01 on Iron, Steel, and Ferroalloys.Current edition approved Nov. 1, 2006Nov. 15, 2013. Published November 2006January 2013. Originally approved in 2002. Last previous edition approved in 20022009as E2209 02
9、.E2209 02 (Reapproved 2006)2. DOI: 10.1520/E2209-02R06E02.10.1520/E2209-13.2 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:E01-1035.3 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer S
10、ervice at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the prev
11、ious version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM In
12、ternational, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1E158 Practice for Fundamental Calculations to Convert Intensities into Concentrations in Optical Emission SpectrochemicalAnalysis (Withdrawn 2004)4E172 Practice for Describing and Specifying the Excitati
13、on Source in Emission Spectrochemical Analysis (Withdrawn 2001)4E305 Practice for Establishing and Controlling Atomic Emission Spectrochemical Analytical CurvesE353 Test Methods for Chemical Analysis of Stainless, Heat-Resisting, Maraging, and Other Similar Chromium-Nickel-IronAlloysE406 Practice fo
14、r Using Controlled Atmospheres in Spectrochemical AnalysisE876 Practice for Use of Statistics in the Evaluation of Spectrometric Data (Withdrawn 2003)4E1019 Test Methods for Determination of Carbon, Sulfur, Nitrogen, and Oxygen in Steel, Iron, Nickel, and Cobalt Alloys byVarious Combustion and Fusio
15、n TechniquesE1059 Practice for Designating Shapes and Sizes of Nongraphite Counter Electrodes (Withdrawn 2013)4E1329 Practice for Verification and Use of Control Charts in Spectrochemical AnalysisE1601 Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Meth
16、odE1806 Practice for Sampling Steel and Iron for Determination of Chemical Composition2.2 Other Document:ASTM Manual on Presentation of Data and Control Chart Analysis, ASTM MNL 7A, seventh revision, 2002.MNL 7 ASTMManual on Presentation of Data and Control Chart Analysis, 8th Edition, 2010.3. Termi
17、nology3.1 For definition of terms used in this method, refer to Terminology E135.4. Summary of Test Method4.1 A controlled discharge is produced between the flat surface of the specimen and the counter electrode. The radiant energiesof selected analytical lines are converted into electrical energies
18、 by photo-multiplierphotomultiplier tubes and stored on capacitors.This discharge is terminated after a fixed exposureintegration time.At the end of the exposure period, the charge on each capacitoris measured,measured and converted to concentration.mass fraction percent.5. Significance and Use5.1 T
19、he chemical composition of high manganese steel alloys must be determined accurately to ensure the desired metallurgicalproperties. This procedure is suitable for manufacturing control and inspection testing.6. Interferences6.1 Interferences may vary with spectrometer design and excitation character
20、istics. Direct spectral interferences may be presenton one or more of the wavelengths listed in a method. Frequently, these interferences may be determined and proper correctionsmade by the use of various reference materials. The composition of the sample being analyzed should match closely thecompo
21、sition of one or more of the reference materials used to prepare and control the calibration curve that is employed.Alternatively, mathematical corrections may be used to solve for interelement effects (refer to Practice effects. E158). Variousmathematical correction procedures are commonly utilized
22、. Any of these are acceptable that will achieve analytical accuracyequivalent to that provided by this method.7. Apparatus7.1 Sample Preparation Equipment:7.1.1 Sample Mold, to produce chilled cast samples approximately 38 mm (112 in.) in diameter that are homogeneous, free ofvoids or porosity in th
23、e region to be excited, and representative of the material to be analyzed. Refer to Practice E1806 for steelsampling procedures.7.1.2 Immersion Sampler, to take a sample from the bath or from the metal stream when pouring can be used. The sample shouldproduce a sample of the same dimensions as liste
24、d in 7.1.1.7.1.3 Surface Grinder or Sander With Abrasive Belts or Disk, capable of providing a flat uniform surface on the referencematerials and specimens. The following table shows the various methods of sample preparation used in the Inter-Laboratory Study(ILS):Type of Grinding Preparation Belt a
25、nd/or DiskGrinding Medium Aluminum Oxide, ZirconiumOxideGrit of Grinding Medium 36 to 180NOTE 2Silicon carbide grinding medium may be used but it was not utilized by the laboratories in the Inter-Laboratory Study (ILS).4 The last approved version of this historical standard is referenced on www.astm
26、.org.E2209 1327.2 Excitation Source, capable of providing a triggered capacitor discharge having the source parameters meeting therequirements of 11.1.7.3 Excitation Stand, suitable for mounting in optical emission alignment, a flat surface for the specimen in opposition to acounter electrode. This
27、stand shall provide an atmosphere of argon. The electrode and argon are described in 8.1 and 8.2.7.4 Spectrometer, having sufficient resolving power and linear dispersion to separate clearly the analytical lines from other linesin the spectrum of a specimen in the spectral region 170.0 nm to 450 nm.
28、 The spectrometer shall have a dispersion of at least 2nm/mm and a focal length of at least 0.5 m. Gas purged spectrometers are an alternative to vacuum systems.7.5 Measuring System, consisting of photo-multiplierphotomultiplier tubes having individual voltage adjustment, capacitors onwhich the outp
29、ut of each photo-multiplierphotomultiplier tube is stored and an electronic system to measure voltages on thecapacitors either directly or indirectly, and the necessary switching arrangements to provide the desired sequence of operation.7.6 Vacuum Pump, if required, capable of maintaining a vacuum o
30、f approximately 3 Pa. There are some equipmentmanufactures that will purge the optical portion of the spectrometer with argon or other inert gas rather than pull a vacuum on theoptics. Either vacuum optics or purged optics are required to determine carbon and phosphorus in this method.7.7 FlushingGa
31、s System, consisting of an argon tanks,supply, a pressure regulator, and a gas flow meter. Automatic sequencingshall be provided to actuate the flow of argon at a given flow rate for a given time interval and to start the excitation at the endof the required flush period. The flushinggas system shal
32、l be in accordance with Practice E406.8. Reagents and Materials8.1 Argon, either gaseous or liquid, must be of sufficient purity to permit proper excitation of the analytical lines of interest.Argon of 99.998 % purity has been found satisfactory. Refer to Practice E406.8.2 Counter ElectrodeA Tungste
33、n or Thoriated Tungsten rod ground to a 15, 30, 4515, 30, 45 or 90 angle conical tip,which conforms to Practice E1059, was found satisfactory. Other material may be used provided it can be shown experimentallythat equivalent precision and bias are obtained.9. Reference Materials9.1 Certified Referen
34、ce Materials, for high manganese steel are commercially available.9.2 Calibrants shall be certified reference materials from recognized certification agencies. They shall cover the concentration-composition ranges of the elements to be determined and shall include all of the specific types of alloys
35、 being analyzed. TheTABLE 1 WavelengthsElement Wavelength(nm) LineClassification PossibleInterferencesAAluminum 394.4 I V, Mn, Mo396.152 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
36、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 Mo, Cr, W251.61 I Fe, VSulfur 180.73 I MnA Interferences are dependent upon instrument design, and excitation conditions,and those listed r
37、equire confirmation based upon specimens designed to demon-strate interferences. This standard method does not purport to address theinterferences that these lines may have. Care should be taken to address theinterferences when calibrating the instrument.E2209 133calibrants shall be homogeneous and
38、free of voids and porosity. The metallurgical history of the calibrants should be similar to thatof the specimens being analyzed. Refer to Test Methods E353 and E1019 for chemical analysis of high manganese steel alloys.9.2.1 In selecting calibrants, use caution with compositions that are unusual. O
39、ne element may influence the radiant energy ofanother element. Tests should be made to determine if interrelations exist between elements in the calibrants.10. Preparation of Calibrants and Specimens10.1 Rough grind, either wet or dry, with a coarse grinding belt or disk. The final grind of the spec
40、imen must be the same gritas the calibrants. Dry the specimens, if wet, for proper excitation in the argon atmosphere. Make sure Ensure that the specimensare homogeneous and free from voids and pits in the region to be excited. Cast specimens from molten metal into a suitable moldand cool. Immersion
41、 and stream samplers are also suitable for use. Prepare the surface of the specimens and reference materialsin a similar manner.11. Excitation and Exposure Instrument Parameters11.1 Electrical ParametersBe certain the spectrometer is in optical alignment and has been calibrated according to themanuf
42、acturers instructions.Electrical parameters within the following ranges were found acceptable.11.1.1 Electrical ParametersElectrical parameters within the following ranges were found acceptable.Triggered Capacitor DischargeCapacitance, :F 2.5 to 15Inductance, :H 50 to 70Resistance, residual to 5Pote
43、ntial, V 940 to 1000Peak Current, A 100 to 275Current pulse duration, :s 130 to 250Number of discharges/s 60 to 120Triggered Capacitor DischargeCapacitance, :F 2.5 to 15Inductance, :H 50 to 70Resistance, residual to 5Potential, V 940 to 1000Peak Current, A 100 to 275Current pulse duration, :s 130 to
44、 250Number of discharges/s 60 to 12011.2 Spectrometer Configurations:Spectrometer ParametersFocal Length 0.5 m to 1.2 mDispersion 0.5 nm/mm to 2.16 nm/mmVacuum 1 Pa to 25 Pa11.3 ExposureExcitation Conditions:Exposure ConditionsFlush Time 2 to 5 sPreburn 10 to 30 sExposure 5 to 20 sFlush Time 2 s to
45、5 sPreburn 10 s to 30 sExposure 5 s to 20 s11.4 Initiation CircuitThe initiator circuit parameters shall be adequate to uniformly trigger the capacitor discharge. Thevalues for these parameters will vary with the instrument. Normal values found to be adequate are listed as follows:Capacitance (d-c c
46、harged) :F 1.2Inductance, :H residualResistance, residualPotential, V 42511.4.1 Other Electrical ParametersExcitation units, on which the precise parameters given in 11.1.111.1 and 11.4 are notavailable, may be used provided that it can be shown experimentally that equivalent precision and accuracy
47、are obtained.11.5 Electrode SystemInsert the counter electrode in the lower electrode position. Adjust the analytical gap to 3, 4, 5, 3 mm,4 mm, 5 mm, or 7 mm depending on the manufacturers recommendations for that particular instrument.11.6 Discharge SourceMost capacitor discharge sources in todays
48、 spectrometers are either the directional self-initiatingcapacitor discharge sourcetype or a triggered capacitor discharge source. Refer to Practice type.E172 for a more detailedexplanation of these sources.12. Preparation of Instrumentation12.1 Prepare the spectrometer in accordance with the manufa
49、cturers instructions.NOTE 3It is not within the scope of this method to prescribe all details of equipment to be used. Equipment varies between laboratories.E2209 13413. Calibration, Standardization, and Verification13.1 CalibrationUsing the conditions given in 11.3, excite the calibrants and potential standardants drift correction samplesin a random sequence, bracketing these burns with excitations of any materials intended for use as verifiers. (A verifier may beused as a calibrant even though it is burned only as a verifier.) There should b
