ASTM E2209-02(2006)e2
(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 test 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 0.15 Carbon (C)0.3 to 1.4 Chromium (Cr)0.25 to 2.00 Manganese (Mn)8.0 to 16.2 Molybdenum (Mo)0.03 to 2.0 Nickel (Ni)0.05 to 4.0 Phosphorus (P)0.025 to 0.06 Silicon (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 (Reapproved2006)
Standard Test Method for
Analysis of High Manganese Steel Using Atomic Emission
Spectrometry
This standard is issued under the fixed designation E2209; 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 (´) indicates an editorial change since the last revision or reapproval.
´ NOTE—Updated Section 2 Referenced Documents in December 2006.
´ NOTE—Added research report footnote to Section 16 editorially in April 2009.
1. Scope E135 Terminology Relating to Analytical Chemistry for
Metals, Ores, and Related Materials
1.1 This test method provides for the analysis of high
E158 Practice for Fundamental Calculations to Convert
manganese steel by atomic emission spectrometry using the
Intensities into Concentrations in Optical Emission Spec-
point-to-plane technique for the following elements in the
trochemical Analysis (Withdrawn 2004)
concentration ranges shown:
E172 Practice for Describing and Specifying the Excitation
Elements Concentration Range, %
SourceinEmissionSpectrochemicalAnalysis(Withdrawn
Aluminum (Al) 0.02 to 0.15 2001)
Carbon (C) 0.3 to 1.4
E305 Practice for Establishing and Controlling Atomic
Chromium (Cr) 0.25 to 2.00
Emission Spectrochemical Analytical Curves
Manganese (Mn) 8.0 to 16.2
Molybdenum (Mo) 0.03 to 2.0 E353 Test Methods for Chemical Analysis of Stainless,
Nickel (Ni) 0.05 to 4.0
Heat-Resisting, Maraging, and Other Similar Chromium-
Phosphorus (P) 0.025 to 0.06
Nickel-Iron Alloys
Silicon (Si) 0.25 to 1.5
E406 Practice for Using Controlled Atmospheres in Spec-
NOTE 1—The ranges represent the actual levels at which this method
2 trochemical Analysis
was tested. These concentration ranges can be extended to higher
E876 Practice for Use of Statistics in the Evaluation of
concentrations by the use of suitable reference materials. Sulfur is not
included because differences in results between laboratories exceeded Spectrometric Data (Withdrawn 2003)
acceptable limits at all analyte levels.
E1019 Test Methods for Determination of Carbon, Sulfur,
1.2 This test method may involve hazardous materials, Nitrogen, and Oxygen in Steel, Iron, Nickel, and Cobalt
operations, and equipment. This standard does not purport to Alloys by Various Combustion and Fusion Techniques
address all of the safety concerns, if any, associated with its E1059 Practice for Designating Shapes and Sizes of Non-
use. It is the responsibility of the user of this standard to graphite Counter Electrodes
establish appropriate safety and health practices and deter- E1601 Practice for Conducting an Interlaboratory Study to
mine the applicability of regulatory limitations prior to use. Evaluate the Performance of an Analytical Method
E1806 Practice for Sampling Steel and Iron for Determina-
2. Referenced Documents
tion of Chemical Composition
2.2 Other Document:
2.1 ASTM Standards:
ASTM Manual on Presentation of Data and Control Chart
A128/A128M Specification for Steel Castings, Austenitic
Analysis, ASTM MNL 7A, seventh revision, 2002.
Manganese
3. Terminology
This test method is under the jurisdiction of ASTM Committee E01 on
3.1 For definition of terms used in this method, refer to
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
Terminology E135.
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
Current edition approved Nov. 1, 2006. Published November 2006. Originally
4. Summary of Test Method
approved in 2002. Last previous edition approved in 2002 as E2209 – 02. DOI:
10.1520/E2209-02R06E02.
4.1 A controlled discharge is produced between the flat
Supporting data have been filed at ASTM International Headquarters and may
surface of the specimen and the counter electrode. The radiant
be obtained by requesting Research Report RR:E01-1035.
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 last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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E2209 − 02 (2006)
energies of selected analytical lines are converted into electri- other lines in the spectrum of a specimen in the spectral region
calenergiesbyphoto-multipliertubesandstoredoncapacitors. 170.0 to 450 nm. The spectrometer shall have a dispersion of
This discharge is terminated after a fixed exposure time.At the at least 2 nm/mm and a focal length of at least 0.5 m. Gas
end of the exposure period, the charge on each capacitor is purged spectrometers are an alternative to vacuum systems.
measured, and converted to concentration.
7.5 Measuring System, consisting of photo-multiplier tubes
having individual voltage adjustment, capacitors on which the
5. Significance and Use
output of each photo-multiplier tube is stored and an electronic
5.1 The chemical composition of high manganese steel
system to measure voltages on the capacitors either directly or
alloys must be determined accurately to ensure the desired
indirectly, and the necessary switching arrangements to pro-
metallurgical properties. This procedure is suitable for manu-
vide the desired sequence of operation.
facturing control and inspection testing.
7.6 Vacuum Pump, if required, capable of maintaining a
vacuum of approximately 3 Pa. There are some equipment
6. Interferences
manufactures that will purge the optical portion of the spec-
6.1 Interferences may vary with spectrometer design and
trometerwithargonorotherinertgasratherthanpullavacuum
excitation characteristics. Direct spectral interferences may be
on the optics. Either vacuum optics or purged optics are
present on one or more of the wavelengths listed in a method.
required to determine carbon and phosphorus in this method.
Frequently, these interferences may be determined and proper
7.7 Flushing System, consisting of argon tanks, a pressure
correctionsmadebytheuseofvariousreferencematerials.The
regulator, and a gas flow meter.Automatic sequencing shall be
composition of the sample being analyzed should match
provided to actuate the flow of argon at a given flow rate for a
closely the composition of one or more of the reference
given time interval and to start the excitation at the end of the
materials used to prepare and control the calibration curve that
required flush period. The flushing system shall be in accor-
is employed. Alternatively, mathematical corrections may be
dance with Practice E406.
used to solve for interelement effects (refer to Practice E158).
Various mathematical correction procedures are commonly
8. Reagents and Materials
utilized. Any of these are acceptable that will achieve analyti-
8.1 Argon, either gaseous or liquid, must be of sufficient
cal accuracy equivalent to that provided by this method.
purity to permit proper excitation of the analytical lines of
7. Apparatus interest.Argon of 99.998 % purity has been found satisfactory.
Refer to Practice E406.
7.1 Sample Preparation Equipment:
7.1.1 Sample Mold,toproducechilledcastsamplesapproxi- 8.2 Counter Electrode—A Tungsten or Thoriated Tungsten
rod ground to a 15, 30, 45 or 90° angle conical tip, which
mately 38 mm (1 ⁄2 in.) in diameter that are homogeneous, free
of voids or porosity in the region to be excited, and represen- conforms to Practice E1059, was found satisfactory.
tative of the material to be analyzed. Refer to Practice E1806
TABLE 1 Wavelengths
for steel sampling procedures.
Wavelength Line Possible
7.1.2 Immersion Sampler, to take a sample from the bath or
Element
A
(nm) Classification Interferences
from the metal stream when pouring can be used. The sample
Aluminum 394.4 I V, Mn, Mo
should produce a sample of the same dimensions as listed in
396.152 I Mo
7.1.1. Carbon 193.09 I Al
Chromium 298.92 II Mn, V, Ni, Nb, Mo
7.1.3 Surface Grinder or Sander With Abrasive Belts or
267.72 II Mn, Mo, V
Disk, capable of providing a flat uniform surface on the
425.435 I
Iron (Internal Standard) 273.07 I
reference materials and specimens. The following table shows
271.44 II
the various methods of sample preparation used in the Inter-
Manganese 263.81 II
Laboratory Study (ILS):
290.02 II
293.31 II Cr
Type of Grinding Preparation Belt and/or Disk
Molybdenum 202.03 II
Grinding Medium Aluminum Oxide, Zirconium
263.876 II
Oxide
281.61 II Al, Mn
Grit of Grinding Medium 36 to 180
386.41 I V, Cr
NOTE 2—Silicon carbide grinding medium may be used but it was not
Nickel 231.60 II Co, Ti
218.54 II
utilized by the laboratories in the Inter-Laboratory Study (ILS).
352.45 I
7.2 Excitation Source, capable of providing a triggered
341.476 I
Phosphorus 178.29 I Mo
capacitor discharge having the source parameters meeting the
Silicon 212.41 I
requirements of 11.1.
288.16 I Mo, Cr, W
251.61 I Fe, V
7.3 Excitation Stand, suitable for mounting in optical emis-
Sulfur 180.73 I Mn
sion alignment, a flat surface for the specimen in opposition to
A
Interferences are dependent upon instrument design, and excitation conditions,
a counter electrode. This stand shall provide an atmosphere of
and those listed require confirmation based upon specimens designed to demon-
argon. The electrode and argon are described in 8.1 and 8.2.
strate interferences. This standard method does not purport to address the
interferences that these lines may have. Care should be taken to address the
7.4 Spectrometer, having sufficient resolving power and
interferences when calibrating the instrument.
linear dispersion to separate clearly the analytical lines from
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E2209 − 02 (2006)
9. Reference Materials 11.4.1 Other Electrical Parameters—Excitation units, on
which the precise parameters given in 11.1.1 and 11.4 are not
9.1 Certified Reference Materials, for high manganese steel
available, may be used provided that it can be shown experi-
are commercially available.
mentally that equivalent precision and accuracy are obtained.
9.2 Calibrants shall be certified reference materials from
11.5 Electrode System—Insert the counter electrode in the
recognized certification agencies. They shall cover the concen-
lower electrode position.Adjust the analytical gap to 3, 4, 5, or
tration ranges of the elements to be determined and shall
7 mm depending on the manufacturer’s recommendations for
include all of the specific types of alloys being analyzed. The
that particular instrument.
calibrantsshallbehomogeneousandfreeofvoidsandporosity.
The metallurgical history of the calibrants should be similar to 11.6 Discharge Source—Most capacitor discharge sources
that of the specimens being analyzed. Refer to Test Methods intoday’sspectrometersareeitherthedirectionalself-initiating
E353 and E1019 for chemical analysis of high manganese steel capacitor discharge source or a triggered capacitor discharge
alloys. source. Refer to Practice E172 for a more detailed explanation
9.2.1 In selecting calibrants, use caution with compositions of these sources.
that are unusual. One element may influence the radiant energy
12. Preparation of Instrumentation
of another element. Tests should be made to determine if
interrelations exist between elements in the calibrants.
12.1 Prepare the spectrometer in accordance with the manu-
facturer’s instructions.
10. Preparation of Calibrants and Specimens
NOTE3—Itisnotwithinthescopeofthismethodtoprescribealldetails
of equipment to be used. Equipment varies between laboratories.
10.1 Rough grind, either wet or dry, with a coarse grinding
belt or disk. The final grind of the specimen must be the same
13. Calibration, Standardization, and Verification
grit as the calibrants. Dry the specimens, if wet, for proper
13.1 Calibration—Usingtheconditionsgivenin11.3,excite
excitation in the argon atmosphere. Make sure that the speci-
the calibrants and potential standardants in a random sequence,
mens are homogeneous and free from voids and pits in the
bracketing these burns with excitations of any materials
region to be excited. Cast specimens from molten metal into a
intended for use as verifiers. (A verifier may be used as a
suitable mold and cool. Immersion and stream samplers are
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
11.1 Be certain the spectrometer is in optical alignment and
E305 and E158.
has been calibrated according to the manufacturer’s instruc-
13.2 Standardization—Following the manufacturer’s
tions.
recommendations, standardize on an initial setup and anytime
11.1.1 Electrical Parameters—Electrical parameters within
thatisknownorsuspectedthatreadingshaveshifted.Makethe
the following ranges were found acceptable.
necessary corrections either by adjusting the controls on the
Triggered Capacitor Discharge
readout or by applying mathematical corrections. Standardiza-
Capacitance, :F 2.5 to 15
Inductance, :H 50 to 70
tion shall be done anytime verifications indicate that readings
Resistance, Σ residual to 5
have gone out of statistical control.
Potential, V 940 to 1000
Peak Current, A 100 to 275
13.3 Verification—Shall be done at least at the beginning of
Current pulse duration, :s 130 to 250
any analytical work. Analyze verifiers in replicate to confirm
Number of discharges/s 60 to 120
that they read within expected confidence interval, as defined
11.2 Spectrometer Configurations:
in 13.4. The replication shall be the same as recommended in
Spectrometer Parameters
14.2.
Focal Length 0.5 m to 1.2 m
13.3.1 Check the verification after standardizing. If confir-
Dispersion 0.5 to 2.16 nm/mm
Vacuum 1 to 25 Pa
mation is not obtained, standardize again and/or investigate
why confirmation is not obtained. Standardization is confirmed
11.3 Exposure Conditions:
if the results are within two standard deviations from the mean
Exposure Conditions
Flush Time 2 to 5 s of the standard.
Preburn 10 to 30 s
13.3.2 Repeat the verification at least every4horifthe
Exposure 5 to 20 s
instrument has been idle for more than 1 h. If readings are not
11.4 Initiation Circuit—The initiator circuit parameters
in conformance, repeat the standardization.
shall be adequate to uniformly trigger the ca
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