ASTM E2209-02(2006)e1
(Test Method)Standard Test Method for Analysis of High Manganese Steel Using Atomic Emission Spectrometry
Standard Test Method for Analysis of High Manganese Steel Using Atomic Emission Spectrometry
SIGNIFICANCE AND USE
The chemical composition of high manganese steel alloys must be determined accurately to ensure the desired metallurgical properties. This procedure is suitable for manufacturing control and inspection testing.
SCOPE
1.1 This method provides for the analysis of high manganese steel by atomic emission spectrometry using the point-to-plane technique for the following elements in the concentration ranges shown:ElementsConcentration 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 1.5
Note 1—The ranges represent the actual levels at which this method was tested. These concentration ranges can be extended to higher concentrations by the use of suitable reference materials. Sulfur is not included because differences in results between laboratories exceeded acceptable limits at all analyte levels.
1.2 This test method may involve hazardous materials, operations, and equipment. This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Designation:E2209–02(Reapproved 2006)
Standard Test Method for
Analysis of High Manganese Steel Using Atomic Emission
Spectrometry
This standard is issued under the fixed designation E 2209; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
e NOTE—Updated Section 2 Reference Documents in December 2006.
1. Scope E 158 Practice for Fundamental Calculations to Convert
Intensities into Concentrations in Optical Emission Spec-
1.1 This test method provides for the analysis of high
trochemical Analysis
manganese steel by atomic emission spectrometry using the
E 172 Practice for Describing and Specifying the Excitation
point-to-plane technique for the following elements in the
Source in Emission Spectrochemical Analysis
concentration ranges shown:
E 305 Practice for Establishing and Controlling Spectro-
Elements Concentration Range, %
chemical Analytical Curves
Aluminum (Al) 0.02 to 0.15
E 353 Test Methods for Chemical Analysis of Stainless,
Carbon (C) 0.3 to 1.4
Heat-Resisting, Maraging, and Other Similar Chromium-
Chromium (Cr) 0.25 to 2.00
Nickel-Iron Alloys
Manganese (Mn) 8.0 to 16.2
Molybdenum (Mo) 0.03 to 2.0
E 406 Practice for Using Controlled Atmospheres in Spec-
Nickel (Ni) 0.05 to 4.0
trochemical Analysis
Phosphorus (P) 0.025 to 0.06
Silicon (Si) 0.25 to 1.5 E 876 Practice for Use of Statistics in the Evaluation of
Spectrometric Data
NOTE 1—The ranges represent the actual levels at which this method
E 1019 Test Methods for Determination of Carbon, Sulfur,
was tested. These concentration ranges can be extended to higher
Nitrogen, and Oxygen in Steel and in Iron, Nickel, and
concentrations by the use of suitable reference materials. Sulfur is not
included because differences in results between laboratories exceeded
Cobalt Alloys
acceptable limits at all analyte levels.
E 1059 Practice for Designating Shapes and Sizes of Non-
graphite Counter Electrodes
1.2 This test method may involve hazardous materials,
E 1601 Practice for Conducting an Interlaboratory Study to
operations, and equipment. This standard does not purport to
Evaluate the Performance of an Analytical Method
address all of the safety concerns, if any, associated with its
E 1806 Practice for Sampling Steel and Iron for Determi-
use. It is the responsibility of the user of this standard to
nation of Chemical Composition
establish appropriate safety and health practices and deter-
2.2 Other Document:
mine the applicability of regulatory limitations prior to use.
ASTM Manual on Presentation of Data and Control Chart
2. Referenced Documents
Analysis, ASTM MNL 7A, seventh revision, 2002.
2.1 ASTM Standards:
3. Terminology
A 128/A 128M Specification for Steel Castings, Austenitic
3.1 For definition of terms used in this method, refer to
Manganese
Terminology E 135.
E 135 Terminology Relating to Analytical Chemistry for
Metals, Ores, and Related Materials
4. Summary of Test Method
4.1 A controlled discharge is produced between the flat
This test method is under the jurisdiction of ASTM Committee E01 on surface of the specimen and the counter electrode. The radiant
Analytical Chemistry for Metals, Ores and Related Materials and is the direct
energies of selected analytical lines are converted into electri-
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
calenergiesbyphoto-multipliertubesandstoredoncapacitors.
Current edition approved Nov. 1, 2006. Published November 2006. Originally
This discharge is terminated after a fixed exposure time.At the
approved in 2002. Last previous edition approved in 2002 as E 2209 – 02.
Supporting data have been filed at ASTM International Headquarters and may
end of the exposure period, the charge on each capacitor is
be obtained by requesting Research Report RR: E01-1035.
measured, and converted to concentration.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. Withdrawn.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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E2209–02 (2006)
5. Significance and Use system to measure voltages on the capacitors either directly or
indirectly, and the necessary switching arrangements to pro-
5.1 The chemical composition of high manganese steel
vide the desired sequence of operation.
alloys must be determined accurately to ensure the desired
7.6 Vacuum Pump, if required, capable of maintaining a
metallurgical properties. This procedure is suitable for manu-
vacuum of approximately 3 Pa. There are some equipment
facturing control and inspection testing.
manufactures that will purge the optical portion of the spec-
trometerwithargonorotherinertgasratherthanpullavacuum
6. Interferences
on the optics. Either vacuum optics or purged optics are
6.1 Interferences may vary with spectrometer design and
required to determine carbon and phosphorus in this method.
excitation characteristics. Direct spectral interferences may be
7.7 Flushing System, consisting of argon tanks, a pressure
present on one or more of the wavelengths listed in a method.
regulator, and a gas flow meter.Automatic sequencing shall be
Frequently, these interferences may be determined and proper
provided to actuate the flow of argon at a given flow rate for a
correctionsmadebytheuseofvariousreferencematerials.The
given time interval and to start the excitation at the end of the
composition of the sample being analyzed should match
required flush period. The flushing system shall be in accor-
closely the composition of one or more of the reference
dance with Practice E 406.
materials used to prepare and control the calibration curve that
is employed. Alternatively, mathematical corrections may be
8. Reagents and Materials
used to solve for interelement effects (refer to Practice E 158).
8.1 Argon, either gaseous or liquid, must be of sufficient
Various mathematical correction procedures are commonly
purity to permit proper excitation of the analytical lines of
utilized. Any of these are acceptable that will achieve analyti-
interest. Argon of 99.998% purity has been found satisfactory.
cal accuracy equivalent to that provided by this method.
Refer to Practice E 406.
8.2 Counter Electrode—A Tungsten or Thoriated Tungsten
7. Apparatus
rod ground to a 15, 30, 45 or 90° angle conical tip, which
7.1 Sample Preparation Equipment:
conforms to Practice E 1059, was found satisfactory.
7.1.1 Sample Mold,toproducechilledcastsamplesapproxi-
mately 38 mm (1 ⁄2 in) in diameter that are homogeneous, free
9. Reference Materials
of voids or porosity in the region to be excited, and represen-
9.1 Certified Reference Materials, for high manganese steel
tative of the material to be analyzed. Refer to Practice E 1806
are commercially available.
for steel sampling procedures.
9.2 Calibrants shall be certified reference materials from
7.1.2 Immersion Sampler, to take a sample from the bath or
recognized certification agencies. They shall cover the concen-
from the metal stream when pouring can be used. The sample
tration ranges of the elements to be determined and shall
should produce a sample of the same dimensions as listed in
include all of the specific types of alloys being analyzed. The
7.1.1.
7.1.3 Surface Grinder or Sander With Abrasive Belts or
TABLE 1 Wavelengths
Disk, capable of providing a flat uniform surface on the
Wavelength Line Possible
reference materials and specimens. The following table shows
Element
A
(nm) Classification Interferences
the various methods of sample preparation used in the Inter-
Aluminum 394.4 I V, Mn, Mo
Laboratory Study (ILS):
396.152 I Mo
Type of Grinding Preparation Belt and/or Disk
Carbon 193.09 I Al
Grinding Medium Aluminum Oxide, Zirconium Oxide
Chromium 298.92 II Mn, V, Ni, Nb, Mo
Grit of Grinding Medium 36 to 180
267.72 II Mn, Mo, V
425.435 I
NOTE 2—Silicon carbide grinding medium may be used but it was not
Iron (Internal Standard) 273.07 I
utilized by the laboratories in the Inter-Laboratory Study (ILS).
271.44 II
Manganese 263.81 II
7.2 Excitation Source, capable of providing a triggered
290.02 II
capacitor discharge having the source parameters meeting the
293.31 II Cr
requirements of 11.1. Molybdenum 202.03 II
263.876 II
7.3 Excitation Stand, suitable for mounting in optical emis-
281.61 II Al, Mn
sion alignment, a flat surface for the specimen in opposition to
386.41 I V, Cr
a counter electrode. This stand shall provide an atmosphere of Nickel 231.60 II Co, Ti
218.54 II
argon. The electrode and argon are described in 8.1 and 8.2.
352.45 I
7.4 Spectrometer, having sufficient resolving power and
341.476 I
Phosphorus 178.29 I Mo
linear dispersion to separate clearly the analytical lines from
Silicon 212.41 I
other lines in the spectrum of a specimen in the spectral region
288.16 I Mo, Cr, W
170.0 to 450 nm. The spectrometer shall have a dispersion of
251.61 I Fe, V
Sulfur 180.73 I Mn
at least 2 nm/mm and a focal length of at least 0.5 m. Gas
A
purged spectrometers are an alternative to vacuum systems. Interferences are dependent upon instrument design, and excitation condi-
tions, and those listed require confirmation based upon specimens designed to
7.5 Measuring System, consisting of photo-multiplier tubes
demonstrate interferences. This standard method does not purport to address the
having individual voltage adjustment, capacitors on which the
interferences that these lines may have. Care should be taken to address the
output of each photo-multiplier tube is stored and an electronic interferences when calibrating the instrument.
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E2209–02 (2006)
calibrantsshallbehomogeneousandfreeofvoidsandporosity. 11.6 Discharge Source—Most capacitor discharge sources
The metallurgical history of the calibrants should be similar to intoday’sspectrometersareeitherthedirectionalself-initiating
that of the specimens being analyzed. Refer to Test Methods capacitor discharge source or a triggered capacitor discharge
E 353 and E 1019 for chemical analysis of high manganese source. Refer to Practice E 172 for a more detailed explanation
steel alloys. of these sources.
9.2.1 In selecting calibrants, use caution with compositions
12. Preparation of Instrumentation
that are unusual. One element may influence the radiant energy
12.1 Prepare the spectrometer in accordance with the manu-
of another element. Tests should be made to determine if
facturer’s instructions.
interrelations exist between elements in the calibrants.
NOTE 3—Itisnotwithinthescopeofthismethodtoprescribealldetails
10. Preparation of Calibrants and Specimens
of equipment to be used. Equipment varies between laboratories.
10.1 Rough grind, either wet or dry, with a coarse grinding
13. Calibration, Standardization, and Verification
belt or disk. The final grind of the specimen must be the same
grit as the calibrants. Dry the specimens, if wet, for proper 13.1 Calibration—Using the conditions given in 11.3, ex-
excitation in the argon atmosphere. Make sure that the speci- cite the calibrants and potential standardants in a random
mens are homogeneous and free from voids and pits in the sequence, bracketing these burns with excitations of any
region to be excited. Cast specimens from molten metal into a materials intended for use as verifiers. (Averifier may be used
suitable mold and cool. Immersion and stream samplers are as a calibrant even though it is burned only as a verifier.)There
also suitable for use. Prepare the surface of the specimens and should be at least five calibrants for each element, spanning the
reference materials in a similar manner. required concentration range. Make replicate exposures in
accordance with 14.2. Using the averages of the data for each
11. Excitation and Exposure
point, determine analytical curves as described in Practices
E 305 and E 158.
11.1 Be certain the spectrometer is in optical alignment and
has been calibrated according to the manufacturer’s instruc- 13.2 Standardization—Following the manufacturer’s rec-
ommendations, standardize on an initial setup and anytime that
tions.
11.1.1 Electrical Parameters—Electrical parameters within is known or suspected that readings have shifted. Make the
necessary corrections either by adjusting the controls on the
the following ranges were found acceptable.
readout or by applying mathematical corrections. Standardiza-
Triggered Capacitor Discharge
Capacitance, :F 2.5 to 15
tion shall be done anytime verifications indicate that readings
Inductance, :H 50 to 70
have gone out of statistical control.
Resistance, S residual to 5
13.3 Verification—Shall be done at least at the beginning of
Potential, V 940 to 1000
Peak Current, A 100 to 275
any analytical work. Analyze verifiers in replicate to confirm
Current pulse duration, :s 130 to 250
that they read within expected confidence interval, as defined
Number of discharges/s 60 to 120
in 13.4. The replication shall be the same as recommended in
11.2 Spectrometer Configurations:
14.2.
Spectrometer Parameters
13.3.1 Check the verification after standardizing. If confir-
Focal Length 0.5 m to 1.2 m
mation is not obtained, standardize again and/or investigate
Dispersion 0.5 to 2.16 nm/mm
why confirmation is not obtained. Standardization is confirmed
Vacuum 1 to 25 Pa
if the results are within two standard deviations from the mean
11.3 Exposure Conditions:
of the standard.
Exposure Conditions
13.3.2 Repeat the verification at least every4horifthe
Flush Time 2 to 5 s
Preburn 10 to 30 s instrument has been idle for more than 1 h. If readings are not
Exposure 5 to 20 s
in conformance, repeat the standardization.
13.4 The confidence interval will be established from ob-
11.4 Initiation Circuit—The initiator circuit parameters
servations of the repeatability of the verifiers and determining
shall be adequate to uniformly trigger the capacitor discharge.
the confidence interval for some acceptable confidence level as
The values for these parameters will vary with the instrument.
prescribed in Practice E 876 or by establishing the upper and
Normal values found to be adequate are listed as follows:
lower limit of a control chart as prescribed in ASTM Manual
Capacitance (d-c charged) :F 1.2
Inductance, :H residual
MNL 7A. The latter is the preferable approach since it also
Resistance, S residual
monitors the consistency of the statistics of the measurements
Potential, V 425
and provides a means of main
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