ASTM E415-99a(2005)
(Test Method)Standard Test Method for Optical Emission Vacuum Spectrometric Analysis of Carbon and Low-Alloy Steel
Standard Test Method for Optical Emission Vacuum Spectrometric Analysis of Carbon and Low-Alloy Steel
SIGNIFICANCE AND USE
This test method for the spectrometric analysis of metals and alloys is primarily intended to test such materials for compliance with compositional specifications. It is assumed that all who use this test method will be analysts capable of performing common laboratory procedures skillfully and safely. It is expected that work will be performed in a properly equipped laboratory.
SCOPE
1.1 This test method covers the simultaneous determination of 20 alloying and residual elements in carbon and low-alloy steels in the concentration ranges shown (Note 1).Note 1
The concentration ranges of the elements listed have been established through cooperative testing of reference materials. Included, in addition to the original data of Test Method E 415 - 71, are data from cooperative testing of a broader range of reference materials to expand the element concentration ranges.
1.2 This test method covers analysis of specimens having a diameter adequate to overlap the bore of the spark stand opening (to effect an argon seal). The specimen thickness should be between 10 and 38 mm.
1.3 This test method covers the routine control analysis of preliminary and ladle tests from either basic oxygen, open-hearth, or electric furnaces and analysis of processed material. It is designed for either chill-cast or rolled and forged specimens. The reference materials and specimens should be of similar metallurgical condition and composition.
1.4 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:E415–99a (Reapproved 2005)
Standard Test Method for
Optical Emission Vacuum Spectrometric Analysis of Carbon
and Low-Alloy Steel
This standard is issued under the fixed designation E 415; 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 hearth, or electric furnaces and analysis of processed material.
It is designed for either chill-cast or rolled and forged speci-
1.1 This test method covers the simultaneous determination
mens. The reference materials and specimens should be of
of 20 alloying and residual elements in carbon and low-alloy
similar metallurgical condition and composition.
steels in the concentration ranges shown (Note 1).
1.4 This standard does not purport to address all of the
Concentration Range, %
A B
safety concerns, if any, associated with its use. It is the
Element Applicable Range, % Quantitative Range, %
responsibility of the user of this standard to establish appro-
Aluminum 0 to 0.075 0.02 to 0.075
priate safety and health practices and determine the applica-
Arsenic 0 to 0.1 0.05 to 0.1
bility of regulatory limitations prior to use.
Boron 0 to 0.007 0.002 to 0.007
Calcium 0 to 0.003 0.001 to 0.003
Carbon 0 to 1.1 0.08 to 1.1
2. Referenced Documents
Chromium 0 to 2.25 0.02 to 2.25
2.1 ASTM Standards:
Cobalt 0 to 0.18 0.008 to 0.18
Copper 0 to 0.5 0.04 to 0.5
E30 Test Methods for Chemical Analysis of Steel, Cast
Manganese 0 to 2.0 0.10 to 2.0
Iron, Open-Hearth Iron, and Wrought Iron
Molybdenum 0 to 0.6 0.03 to 0.6
E 135 Terminology Relating to Analytical Chemistry for
Nickel 0 to 5.0 0.02 to 5.0
Niobium 0 to 0.085 0.02 to 0.085
Metals, Ores, and Related Materials
Nitrogen 0 to 0.015 0.004 to 0.015
E 158 Practice for Fundamental Calculations to Convert
Phosphorous 0 to 0.085 0.02 to 0.085
Silicon 0 to 1.15 0.07 to 1.15 Intensities into Concentrations in Optical Emission Spec-
Sulfur 0 to 0.055 0.01 to 0.055
trochemical Analysis
Tin 0 to 0.045 0.01 to 0.045
E 305 Practice for Establishing and Controlling Spectro-
Titanium 0 to 0.2 0.004 to 0.2
chemical Analytical Curves
Vanadium 0 to 0.3 0.004 to 0.3
Zirconium 0 to 0.05 0.02 to 0.05
E 350 Test Methods for ChemicalAnalysis of Carbon Steel,
Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, and
A
Applicable range in accordance with Guide E 1763 for results reported in Wrought Iron
accordance with Practice E 1950.
E 406 Practice for Using Controlled Atmospheres in Spec-
B
Quantitative range in accordance with Practice E 1601.
trochemical Analysis
NOTE 1—The concentration ranges of the elements listed have been
E 1019 Test Methods for Determination of Carbon, Sulfur,
established through cooperative testing of reference materials. Included,
Nitrogen, and Oxygen in Steel and in Iron, Nickel, and
in addition to the original data of Test Method E 415 – 71, are data from
Cobalt Alloys
cooperative testing of a broader range of reference materials to expand the
E 1329 Practice for Verification and Use of Control Charts
element concentration ranges.
in Spectrochemical Analysis
1.2 This test method covers analysis of specimens having a
E 1601 Practice for Conducting an Interlaboratory Study to
diameter adequate to overlap the bore of the spark stand
Evaluate the Performance of an Analytical Method
opening (to effect an argon seal). The specimen thickness
E 1763 Guide for Interpretation and Use of Results from
should be between 10 and 38 mm.
Interlaboratory Testing of Chemical Analysis Methods
1.3 This test method covers the routine control analysis of
E 1806 Practice for Sampling Steel and Iron for Determi-
preliminary and ladle tests from either basic oxygen, open-
nation of Chemical Composition
This test method is under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores and Related Materials and is the direct
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Jan. 1, 2005. Published March 2005. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1971. Last previous edition approved in 1999 as E 415 – 99a. Standards volume information, refer to the standard’s Document Summary page on
Supporting data have been filed at ASTM International Headquarters and may the ASTM website.
be obtained by requesting Research Report RR: E2-1004. Withdrawn.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E415–99a (2005)
E 1950 Practice for Reporting Results from Methods of nm. Masks shall be provided in the spectrometer to eliminate
Chemical Analysis scattered radiation. The spectrometer shall be provided with an
air inlet and a vacuum outlet. The spectrometer shall be
3. Terminology
operated at a vacuum of 25 µm of mercury or below. The
primary slit width is 20 to 50 µm. Secondary slit width is 50 to
3.1 For definitions of terms used in this test method, refer to
200 µm.
Terminology E 135.
6.5 Measuring System, consisting of photomultipliers hav-
4. Summary of Test Method
ing individual voltage adjustments, capacitors in which the
output of each photomultiplier is stored, a voltage measuring
4.1 The most sensitive lines of arsenic, boron, carbon,
system to register the voltages on the capacitors either directly
nitrogen, phosphorus, sulfur, and tin lie in the vacuum ultra-
or indirectly, and the necessary switching arrangements to
violet region. The absorption of the radiation by air in this
provide the desired sequence of operation.
region is overcome by evacuating the spectrometer and flush-
6.6 Vacuum Pump, capable of maintaining a vacuum of 25
ing the spark chamber with argon. A capacitor discharge is
µm Hg.
produced between the flat, ground surface of the disk specimen
and a conically shaped electrode. The discharge is terminated
NOTE 3—A pump with a displacement of at least 0.23 m /min (8
at a predetermined intensity time integral of a selected iron
ft /min) is usually adequate.
line, or at a predetermined time, and the relative radiant
6.7 Flushing System, consisting of argon tanks, a pressure
energies or concentrations of the analytical lines are recorded.
regulator, and a gas flowmeter. Automatic sequencing shall be
provided to actuate the flow of argon at a given flow rate for a
5. Significance and Use
given time interval and to start the excitation at the end of the
5.1 Thistestmethodforthespectrometricanalysisofmetals
flush period. Means of changing the flow rate of argon shall be
and alloys is primarily intended to test such materials for
provided. The flushing system shall be in accordance with
compliance with compositional specifications. It is assumed
Practice E 406.
that all who use this test method will be analysts capable of
7. Reagents and Materials
performing common laboratory procedures skillfully and
safely. It is expected that work will be performed in a properly
7.1 Counter Electrodes—The counter electrodes shall be
equipped laboratory. 6.4-mm ( ⁄4-in.) in diameter, hard-drawn, fine, silver rods,
1.5-mm ( ⁄16-in.) thoriated, tungsten rods, or other material
6. Apparatus
provided it can be shown experimentally that equivalent
6.1 Sample Preparation Equipment: precisionandbiasisobtained.Machinetherodstoa90or120°
cone.
6.1.1 Sample Mold, capable of producing castings that are
homogeneous and free from voids and porosity. Refer to
NOTE 4—A black deposit builds up on the tip of the electrode, thus
Practice E 1806 for steel sampling procedures. The following
reducing the overall intensity of the spectral radiation. In general this
mold types have been found to produce acceptable samples:
condition will not affect analytical performance for the first 40 or 50
6.1.1.1 Cast Iron Mold—A mold 70 mm (2 ⁄4 in.) deep, 64 excitations, after which time a freshly prepared counter electrode should
be installed. The number of acceptable excitations on an electrode varies
mm (2 ⁄2 in.) in diameter at the top of the mold, and 57 mm
1 from one instrument to another, and should be established in each
(2 ⁄4 in.) in diameter at the bottom of the mold. The wall
laboratory. With a thoriated tungsten electrode, it has been reported that a
thickness of the mold is approximately 32 mm (1 ⁄4 in.).
hundred or more excitations can usually be made before replacement.
6.1.1.2 Refractory Mold Ring—Amold that has a minimum
1 7.2 Inert Gas, Argon, in accordance with Practice E 406.
insidediameterof32mm(1 ⁄4in.)andaminimumheightof25
mm(1in.).Theringisplacedonaflatsurfaceofacopperplate
8. Reference Materials
approximately 50 mm (2 in.) thick.
8.1 Certified Reference Materials (CRMs) are available
6.1.1.3 Book-Type Steel or Copper Mold, to produce a
from the National Institute of Standards and Technology and
1 1
chill-cast disk 64 mm (2 ⁄2 in.) in diameter and 13 mm ( ⁄2 in.)
other sources. These cover all or part of the concentration
thick.
ranges listed in 1.1. They are valuable in establishing prelimi-
6.2 Excitation Source, capable of providing a triggered
nary working curves and determining the precision of the
capacitor discharge having source parameters meeting the
instrument. However, because of differences between these
requirements of 11.1.
CRMs and the production specimens prepared by the sampling
6.3 Spark Chamber, automatically flushed with argon. The
procedures recommended for this test method, curves based on
spark chamber shall be mounted directly on the spectrometer,
CRMs may (in very unusual circumstances) need to be
and shall be provided with a spark stand to hold a flat specimen
correctedwithvaluesfromreferencematerialsmadebynormal
and a lower electrode of rod form.
production sampling techniques and analyzed in accordance
NOTE 2—Clean the excitation chamber when the counter electrode is
with Test MethodsE30, E 350, and E 1019.
replaced. Clean the lens or protective window after approximately 200 to
8.2 Reference Materials—Periodically check the instrument
300 excitations to minimize transmission losses.
for drift. For this purpose, verifiers and standardants are
6.4 Spectrometer, having a reciprocal linear dispersion of employed. These reference materials shall be homogeneous
0.60 nm/mm, or better, in the first order and a focal length of and contain appropriate amounts of each element, covering the
0.75 to 3 m. Its approximate range shall be from 120.0 to 400.0 concentration range of elements contained in the specimens.
E415–99a (2005)
TABLE 1 Internal Standard and Analytical Lines
9. Preparation of Specimens and Reference Materials
Line
B
9.1 Use cast or rolled and forged samples. Cut a 13 to
Element Wavelength, nm Possible Interference
A
Classification
25-mm ( ⁄2 to 1-in.) thick slice from the sample or obtain an
Aluminum 394.40 I V, Mn, Mo, Ni
initial smooth flat surface by machining at least 1.3 mm (0.05
308.22 I V, Mn
in.) off the original surface using a lathe or grinder. Make
Arsenic 197.20 I Mo, W
193.76 I Mn
certain that the specimens are homogeneous and free from
Boron 182.64 I S, Mn, Mo
voids and pits in the region to be excited (Note 5). Rough grind
182.59 I W, Mn, Cu
the cut surface by grinding on a belt surfacer, either wet or dry,
Calcium 396.85 II Nb
Carbon 193.09 I Al
with 50 to 80-grit abrasive belt. Obtain the final surface by dry
Chromium 298.92 II Mn, V, Ni, Nb, Mo
grinding. A finer abrasive belt, such as 120-grit, may be used
267.72 II Mn, Mo, W
for final dry grinding, but is not essential (Note 6).
Cobalt 345.35 I Cr, Mo
228.62 II Ni, Cr
NOTE 5—Specimen porosity is undesirable because it leads to the
Copper 327.40 I Nb
improper “diffuse-type” rather than the desired “concentrated-type” dis- 213.60 II Mo, Cr
Iron (IS) 271.44 II
charge. The specimen surface should be kept clean because the specimen
273.07 II Co
is the electron emitter, and electron emission is inhibited by oily, dirty
Manganese 293.31 II Cr, Mo, Ni
surfaces.
255.86 II Zr
NOTE 6—Reference materials and specimens shall be refinished dry on
Molybdenum 379.83 II Mn
a belt sander before being re-excited on the same area. 277.54 I Cu, V, Co, Mn
386.41 I V, Cr
Nickel 231.60 II Co, Ti
10. Preparation of Apparatus
227.02 II Nb, W
Niobium 319.50 II Mo, Al, V
NOTE 7—The instructions given in this test method apply to most
Nitrogen 149.26 I Fe, Ti, Si, Mn, Cu, Ni
spectrometers; however, some settings and adjustments may need to be
and nitride forming
varied, and additional preparation of the equipment may be required. It is
elements such as Ti
not within the scope of an ASTM test method to prescribe the minute
Phosphorus 178.29 I Mo
details of the apparatus preparation, which may differ not only for each Silicon 288.16 I Mo, Cr, W
251.61 I Fe, V
manufacturer, but also for different equipment from the same manufac-
Sulfur 180.73 I Mn
turer. For a description of and further details of operation of a particular
Tin 189.99 II Mn, Mo, Al
spectrometer, refer to the manufacturer’s handbook.
Titanium 337.28 II Nb
324.20 II Nb
10.1 Program the spectrometer to accommodate the internal
Vanadium 310.23 II Fe, Mo, Nb, Ni
standard lines and one of the analytical lines for each element
311.07 II Mn, Ti, Fe
Zirconium 343.82 II W
listed in Table 1.
A
The numerals I or II in the line classification column indicate that the line has
NOTE 8—The lines listed in Table 1 have proven satisfactory for the
been classified in a term array and definitely assigned to the normal atom (I) or to
elements and concentration ranges described in the scope. Other internal
the singly ionized atom (II).
B
standard and analytical lines, such as those listed in Table 2, may be used
Interferences are dependent upon instrument design, spectrum line choices,
providedthatitcanbeshownexperimentallythatequivalentprecisionand and excitation conditions, and those listed require confirmation based upon
specimens selected especially to demonstrate suspected interferences.
accuracy are obtained.
10.2 Position or test the position of the spectrometer exit
TABLE 2 Other Analytical Lines
slits to ensure that peak radiation passes through each slit and
Line
B
Element Wavelength, nm Possible Interference
is incident on the photomultiplier. This shall be done initially A
Classification
and as often as necessary thereafter to maintain proper align-
Arsenic 189.04 I V, Cr
ment.
Carbon 165.81 I
NOTE 9—The manner and frequency of positioning or checking the
position of the exit slits will depend on factors such as: the type of
Copper 224.26
...
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