ASTM E2209-02(2006)
(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
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.
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 STP 15D, fourth revision, 1976, Part 3,
p. 71
2.1 ASTM Standards:
A 128/A 128M Specification for Steel Castings, Austenitic
3. Terminology
Manganese
3.1 For definition of terms used in this method, refer to
E 135 Terminology Relating to Analytical Chemistry for
Terminology E 135.
Metals, Ores, and Related Materials
4. Summary of Test Method
This test method is under the jurisdiction of ASTM Committee E01 on
4.1 A controlled discharge is produced between the flat
Analytical Chemistry for Metals, Ores and Related Materials and is the direct
surface of the specimen and the counter electrode. The radiant
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
energies of selected analytical lines are converted into electri-
Current edition approved Nov. 1, 2006. Published November 2006. Originally
approved in 2002. Last previous edition approved in 2002 as E 2209 – 02. calenergiesbyphoto-multipliertubesandstoredoncapacitors.
Supporting data have been filed at ASTM International Headquarters and may
This discharge is terminated after a fixed exposure time.At the
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 ASTM website. Withdrawn.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E2209–02 (2006)
end of the exposure period, the charge on each capacitor is 7.5 Measuring System, consisting of photo-multiplier tubes
measured, and converted to concentration. having individual voltage adjustment, capacitors on which the
output of each photo-multiplier tube is stored and an electronic
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.
7.1.2 Immersion Sampler, to take a sample from the bath or
from the metal stream when pouring can be used. The sample
TABLE 1 Wavelengths
should produce a sample of the same dimensions as listed in
Wavelength Line Possible
7.1.1.
Element
A
(nm) Classification Interferences
7.1.3 Surface Grinder or Sander With Abrasive Belts or
Aluminum 394.4 I V, Mn, Mo
Disk, capable of providing a flat uniform surface on the
396.152 I Mo
reference materials and specimens. The following table shows
Carbon 193.09 I Al
the various methods of sample preparation used in the Inter- Chromium 298.92 II Mn, V, Ni, Nb, Mo
267.72 II Mn, Mo, V
Laboratory Study (ILS):
425.435 I
Type of Grinding Preparation Belt and/or Disk
Iron (Internal Standard) 273.07 I
Grinding Medium Aluminum Oxide, Zirconium Oxide
271.44 II
Grit of Grinding Medium 36 to 180
Manganese 263.81 II
290.02 II
NOTE 2—Silicon carbide grinding medium may be used but it was not
293.31 II Cr
utilized by the laboratories in the Inter-Laboratory Study (ILS).
Molybdenum 202.03 II
263.876 II
7.2 Excitation Source, capable of providing a triggered
281.61 II Al, Mn
capacitor discharge having the source parameters meeting the
386.41 I V, Cr
requirements of 11.1. Nickel 231.60 II Co, Ti
218.54 II
7.3 Excitation Stand, suitable for mounting in optical emis-
352.45 I
sion alignment, a flat surface for the specimen in opposition to
341.476 I
Phosphorus 178.29 I Mo
a counter electrode. This stand shall provide an atmosphere of
Silicon 212.41 I
argon. The electrode and argon are described in 8.1 and 8.2.
288.16 I Mo, Cr, W
7.4 Spectrometer, having sufficient resolving power and
251.61 I Fe, V
Sulfur 180.73 I Mn
linear dispersion to separate clearly the analytical lines from
A
other lines in the spectrum of a specimen in the spectral region Interferences are dependent upon instrument design, and excitation condi-
tions, and those listed require confirmation based upon specimens designed to
170.0 to 450 nm. The spectrometer shall have a dispersion of
demonstrate interferences. This standard method does not purport to address the
at least 2 nm/mm and a focal length of at least 0.5 m. Gas
interferences that these lines may have. Care should be taken to address the
purged spectrometers are an alternative to vacuum systems. interferences when calibrating the instrument.
E2209–02 (2006)
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. 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
that are unusual. One element may influence the radiant energy
12. Preparation of Instrumentation
of another element. Tests should be made to determine if
12.1 Prepare the spectrometer in accordance with the manu-
interrelations exist between elements in the calibrants.
facturer’s instructions.
10. Preparation of Calibrants and Specimens NOTE 3—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—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
11.1 Be certain the spectrometer is in optical alignment and
E 305 and E 158.
has been calibrated according to the manufacturer’s instruc-
13.2 Standardization—Following the manufacturer’s rec-
tions.
ommendations, standardize on an initial setup and anytime that
11.1.1 Electrical Parameters—Electrical parameters within
is known or suspected that readings have shifted. Make the
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
tion shall be done anytime verifications indicate that readings
Inductance, :H 50 to 70
Resistance, S residual to 5
have gone out of statistical control.
Potential, V 940 to 1000
13.3 Verification—Shall be done at least at the beginning of
Peak Current, A 100 to 275
any analytical work. Analyze verifiers in replicate to confirm
Current pulse duration, :s 130 to 250
Number of discharges/s 60 to 120
that they read within expected confidence interval, as defined
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
Dispersion 0.5 to 2.16 nm/mm
mation is not obtained, standardize again and/or investigate
Vacuum 1 to 25 Pa
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 of the standard.
Flush Time 2 to 5 s
13.3.2 Repeat the verification at least every4horifthe
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.
11.4 Initiation Circuit—The initiator circuit parameters
13.4 The confidence interval will be established from ob-
shall be adequate to uniformly trigger the capacitor discharge.
servations of the repeatability of the verifiers and determining
The values for these parameters will vary with the instrument.
the confidence interval for some acceptable confidence level as
Normal values found to be adequate are listed as follows:
prescribed in Practice E 876 or by establishing the upper and
Capacitance (d-c charged) :F 1.2
lower limit of a control chart as prescribed in ASTM Manual
Inductance, :H residual
STP 15D. The latter is the preferable appr
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