ASTM E327-94
(Test Method)Test Method for Optical Emission Spectrometric Analysis of Stainless Type 18-8 Steels by the Point-To-Plane Technique (Withdrawn 1999)
Test Method for Optical Emission Spectrometric Analysis of Stainless Type 18-8 Steels by the Point-To-Plane Technique (Withdrawn 1999)
SCOPE
1.1 This test method covers the optical emission spectrometric analysis of stainless Type 18-8 steels for the following elements: Element Concentration Range, % Chromium 17.0 to 20.0 Nickel 8.0 to 15.0 Manganese 0.8 to 2.0 Silicon 0.4 to 0.8 Copper 0.1 to 0.2
1.2 This test method is designed for routine analysis of chill-cast disks or inspection testing of stainless Type 18-8 steel flats upon which a surface of at least 13-mm (1/2-in.) diameter may be prepared. The samples must be sufficiently massive to prevent overheating during the discharge and of similar metallurgical condition and composition as the standards used.
1.3 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.
General Information
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Please contact ASTM International (www.astm.org) for the latest information.
Designation:E327–94
Standard Test Method for
Optical Emission Spectrometric Analysis of Stainless Type
18-8 Steels by the Point-To-Plane Technique
This standard is issued under the fixed designation E 327; 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.
1. Scope E 305 Practice for Establishing and Controlling Spectro-
chemical Analytical Curves
1.1 This test method covers the optical emission spectro-
E 876 Practice for Use of Statistics in the Evaluation of
metric analysis of stainless Type 18-8 steels for the following
Spectrometric Data
elements:
Element Concentration Range, %
3. Terminology
Chromium 17.0 to 20.0
3.1 Definitions—For definitions of terms used in this test
Nickel 8.0 to 15.0
method, refer to Terminology E 135E 135.
Manganese 0.8 to 2.0
Silicon 0.4 to 0.8
4. Summary of Test Method
Copper 0.1 to 0.2
4.1 A controlled discharge is produced between the flat
1.2 This test method is designed for routine analysis of
ground surface of the sample and a specially shaped graphite
chill-castdisksorinspectiontestingofstainlessType18-8steel
1 electrode. The radiant energy of selected analytical lines is
flats upon which a surface of at least 13-mm ( ⁄2-in.) diameter
converted into electrical energy by multiplier photo tubes and
may be prepared. The samples must be sufficiently massive to
is stored on capacitors. The discharge is terminated at a
prevent overheating during the discharge and of similar met-
predetermined level of accumulated radiant energy from the
allurgical condition and composition as the standards used.
internal standard iron line or after a fixed exposure time.At the
1.3 This standard does not purport to address all of the
end of the exposure period, the charge on each condenser is
safety concerns, if any, associated with its use. It is the
evaluated electronically and displayed or recorded as relative
responsibility of the user of this standard to establish appro-
energies or concentrations.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
5. Apparatus
2. Referenced Documents 5.1 Sample Preparation Equipment:
5.1.1 Sample Mold, capable of producing castings that are
2.1 ASTM Standards:
homogeneous and free from voids and porosity. The following
E 130 Practice for Designation of Shapes and Sizes of
2 mold types have been found to produce acceptable samples:
Graphite Electrodes
5.1.1.1 Cast Iron Mold—A mold 70 mm (2 ⁄4 in.) deep, 64
E 135 Terminology Relating to Analytical Chemistry for
2 mm (2 ⁄2 in.) in diameter at the top of the mold, and 57 mm
Metals, Ores, and Related Materials
(2 ⁄2 in.) in diameter at the bottom of the mold. The wall
E 158 Practice for Fundamental Calculations to Convert
thickness of the mold is approximately 32 mm (1 ⁄4 in.).
Intensities into Concentrations in Optical Emission Spec-
5.1.1.2 Refractory Mold Ring—Amold that has a minimum
trochemical Analysis
inside diameter of 32 mm (1 ⁄2 in.) and a minimum of 25 mm
E 172 Practice for Describing and Specifying the Excitation
(1 in.) in height.The ring is placed on a flat surface of a copper
Source in Emission Spectrochemical Analysis
plate approximately 50 mm (2 in.) thick.
5.1.1.3 Book-Type Steel Mold, to produce a chill-cast disk
1 1
64 mm (2 ⁄2 in.) in diameter and 13 mm ( ⁄2 in.) thick.
This test method is under the jurisdiction of ASTM Committee E-1 on
5.1.2 Abrasive Grinder—A suitable belt grinder, horizontal
Analytical Chemistry for Metals, Ores and Related Materials and is the direct
disk grinder, or similar grinding apparatus may be used. The
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
Current edition approved Jan. 15, 1994. Published March 1994. Originally
published as E 327 – 67 T. Last previous edition E 327 – 88.
2 3
Annual Book of ASTM Standards, Vol 03.05. Annual Book of ASTM Standards, Vol 03.06.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Please contact ASTM International (www.astm.org) for the latest information.
E327–94
resulting surface should be perfectly plane and free of defects. The metallurgical history of secondary standards should be
These may be either wet or dry grinding devices. Grit size of compatible with that of the samples being analyzed.
grinding material in the range from 60 to 180 has been found
8. Preparation of Samples and Secondary Standards
satisfactory.
5.2 Electrode Cutter, for shaping electrodes to the configu- 8.1 Cast Samples—Cast the sample from molten metal in
the sample mold, remove from the mold, and let air cool.
ration selected in 6.1.
Obtain a smooth flat surface by grinding. Make certain that the
5.3 Excitation Source, with parameters capable of produc-
cast samples are homogeneous and free of voids or pits in the
ing a usable spectrum as described in 9.2. (See Practice
region to be sparked. To speed up the surface preparation,
E 172E 172.)
preliminary surfacing with a relatively coarse grinder (30 to 50
5.4 Excitation Stand, suitable for mounting in optical align-
grit) will be found helpful. For the final polishing, a grit
ment a flat disk sample in opposition to a graphite counter
between 60 and 180 shall be selected and used for all samples.
electrode.
Standards and test pieces must have the same surface treat-
5.5 Spectrometer, having sufficient resolving power and
ment. Standards and samples shall be refinished before being
linear dispersion to separate clearly the analytical lines from
resparked on the same area. The grinding material or finish, or
other lines in the spectrum of the sample in the spectral region
2200 to 4600 Å . Suitable instruments can be purchased both,mustbesuchthataminimumofcontaminationwilloccur
from this source.
commercially. Spectrometer characteristics for two of the
instruments used in the evaluation of this test method are given 8.2 Rolled or Forged Samples—If necessary, saw or ma-
chine to the appropriate size and prepare the surface as
in Table 1.
5.6 Measuring System, consisting of photomultipliers hav- described in 7.1.
ing individual voltage adjustment, capacitors on which the
9. Preparation of Apparatus
output of each photomultiplier is stored and an electronic
system to evaluate voltages on the capacitors either directly or NOTE 1—The instructions given herein apply to most spectrometers;
however, some settings and adjustments may need to be varied, and
indirectly, and the necessary switching arrangements to pro-
depending on the particular equipment, additional preparation of the
vide the desired sequence of operation.
equipment may be required. It is not within the scope of an ASTM test
method to prescribe minute details of the apparatus preparation which
6. Reagents and Materials
differ not only for each manufacturer, but also often for different
6.1 Electrodes—The counter electrode shall be Type C-2 or
equipment from the same manufacturer. For a description and further
C-5 as given in Practice E 130E 130.
details of operation of a particular spectrometer, refer to the manufactur-
er’s handbook.
7. Standards
9.1 Program the spectrometer to accommodate the internal
7.1 Primary standards are available from the National Insti-
standard lines and analytical lines listed in Table 2 (Note 2).
tute of Standards and Technology. These cover all or part of
Connect the photomultipliers, capacitors, and related measur-
the concentration ranges listed in 1.1. They are valuable in
ingsystem.Positionortestthepositionofthespectrometerexit
establishing preliminary working curves and determining the
slits to ensure that peak radiation passes through each slit and
precision of the instrument. However, due to metallurgical
isincidentuponthephotomultiplier.Thisshallbedoneinitially
differences between these standards and the production
and as often as necessary thereafter to maintain proper align-
samples prepared by the sampling procedures recommended
ment.
forthistestmethod,curvesbasedonprimarystandardsmustbe
corrected with values from secondary standards.
TABLE 2 Analytical Lines
7.2 Secondary Standards—These shall be chemically ana-
Analytical Line, Internal Standard Line, Concentration Range,
lyzed test samples taken from production heats. They shall
Å Å %
cover the concentration ranges of the elements determined and
Cr 2989.19 Fe 2714.41 5.0 to 20.0
shall include all of the specific types of alloys being analyzed. Cr 2860.93 Fe 2714.41
Cr 2862.57 Fe 2714.41
These standards shall be homogeneous and free of voids or
porosity.Theyshallbepreparedinthemannerdescribedin8.1.
Mn 2593.73 Fe 2714.41 0.1 to 5.0
Mn 2949.21 Fe 2714.41
Mn 4034.49 Fe 3719.94
Mn 2933.06 Fe 2714.41
National Institute of Standards and Technology, U.S. Department of Com-
merce, Gaithersburg, MD 20899.
Ni 2316.04 Fe 2714.41 2.0 to 15.0
Ni 3414.76 Fe 3719.94
TABLE 1 Spectrometer Characteristics
Ni 3012.00 Fe 3719.94
Instrument A Instrument B
Si 2516.12 Fe 2714.41 0.1 to 2.0
Focal length, m 1.5 3 Si 2516.12 Fe 3719.94
Concave grafting, grooves/mm 1200 1200 Si 2881.58 Fe 2714.41
Reciprocal linear dispersion, Å/mm 7 2.75 Si 2881.58 Fe 3719.94
(first order)
Primary slit width, µm 20 75 Cu 3273.96 Fe 2714.41 0.05 to 0.50
Secondary slit width, µm 20 to 100 50 to 200 Cu 3273.96 Fe 4404.75
Wavelength coverage, Å 2200 to 4600 2200 to 4600 Cu 3273.96 Fe 3719.94
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Please contact ASTM International (www.astm.org) for the latest information.
E327–94
NOTE 2—The lines listed have been proven satisfactory for the ele-
10. Calibration, Standardization, and Ver
...
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