ASTM E1086-94(2005)
(Test Method)Standard Test Method for Optical Emission Vacuum Spectrometric Analysis of Stainless Steel by the Point-to-Plane Excitation Technique
Standard Test Method for Optical Emission Vacuum Spectrometric Analysis of Stainless Steel by the Point-to-Plane Excitation Technique
SIGNIFICANCE AND USE
The chemical composition of stainless steels must be determined accurately in order 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 optical emission vacuum spectrometric analysis of stainless steel in solid form by the point-to-plane excitation technique for the following elements in the concentration ranges shown:ElementConcentration Range, %Chromium17.0 to 23.0Nickel 7.5 to 13.0Molybdenum0.01 to 3.0 Manganese0.01 to 2.0 Silicon 0.01 to 0.90Copper 0.01 to 0.30Carbon 0.005 to 0.25Phosphorus0.003 to 0.15Sulfur 0.003 to 0.065
1.2 This test method is designed for the routine analysis of chill-cast disks or inspection testing of stainless steel samples that have a flat surface of at least 13 mm (0.5 in.) in diameter. The samples must be sufficiently massive to prevent overheating during the discharge and of a similar metallurgical condition and composition as the reference materials.
1.3 Analytical curves are plotted using the concentration ratio method as shown in Practice E158. One or more of the reference materials must closely approximate the composition of the specimen. The technique of analyzing reference materials along with unknowns and performing the indicated mathematical corrections may also be used to correct for interference effects and to compensate for errors resulting from instrument drift. A variety of such systems are commonly used. Any of these that will achieve analytical accuracy equivalent to that reported for this test method are acceptable.
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:E1086–94 (Reapproved 2005)
Standard Test Method for
Optical Emission Vacuum Spectrometric Analysis of
Stainless Steel by Point-to-Plane Excitation Technique
This standard is issued under the fixed designation E 1086; 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 priate safety and health practices and determine the applica-
2 bility of regulatory limitations prior to use.
1.1 This test method covers for the optical emission
vacuum spectrometric analysis of stainless steel in solid form
2. Referenced Documents
by the point-to-plane excitation technique for the following
2.1 ASTM Standards:
elements in the concentration ranges shown:
E 135 Terminology Relating to Analytical Chemistry for
Element Concentration Range, %
Metals, Ores, and Related Materials
Chromium 17.0 to 23.0
Nickel 7.5 to 13.0
E 158 Practice for Fundamental Calculations to Convert
Molybdenum 0.01 to 3.0
Intensities into Concentrations in Optical Emission Spec-
Manganese 0.01 to 2.0
trochemical Analysis
Silicon 0.01 to 0.90
Copper 0.01 to 0.30
E 172 Practice for Describing and Specifying the Excitation
Carbon 0.005 to 0.25
Source in Emission Spectrochemical Analysis
Phosphorus 0.003 to 0.15
E 305 Practice for Establishing and Controlling Spectro-
Sulfur 0.003 to 0.065
chemical Analytical Curves
1.2 This test method is designed for the routine analysis of
E 406 Practice for Using Controlled Atmospheres in Spec-
chill-cast disks or inspection testing of stainless steel samples
trochemical Analysis
that have a flat surface of at least 13 mm (0.5 in.) in diameter.
E 876 Practice for Use of Statistics in the Evaluation of
The samples must be sufficiently massive to prevent overheat-
Spectrometric Data
ing during the discharge and of a similar metallurgical condi-
E 1060 Practice for Interlaboratory Testing of Spectro-
tion and composition as the reference materials.
chemical Methods of Analysis
1.3 Analytical curves are plotted using the concentration
ratio method as shown in Practice E 158. One or more of the
3. Terminology
reference materials must closely approximate the composition
3.1 Definitions—For definitions of terms used in this test
of the specimen. The technique of analyzing reference mate-
method, refer to Terminology E 135.
rials along with unknowns and performing the indicated
mathematical corrections may also be used to correct for
4. Summary of Test Method
interference effects and to compensate for errors resulting from
4.1 A controlled discharge is produced between the flat
instrument drift.Avariety of such systems are commonly used.
surface of the specimen and the counter electrode. The radiant
Anyofthesethatwillachieveanalyticalaccuracyequivalentto
energy of selected analytical lines are converted into electrical
that reported for this test method are acceptable.
energiesbyphotomultipliertubesandstoredoncapacitors.The
1.4 This standard does not purport to address all of the
discharge is terminated at a predetermined level of accumu-
safety concerns, if any, associated with its use. It is the
lated radiant energy from the internal standard iron line or after
responsibility of the user of this standard to establish appro-
a fixed exposure time. At the end of the exposure period, the
charge on each capacitor is measured, and displayed or
recorded as a relative energy or concentration.
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 1985. Last previous edition approved in 2000 as E 1086 – 94 (2000). 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: E02-1023. Withdrawn.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E1086–94 (2005)
TABLE 1 Analytical and Internal Standard Lines
5. Significance and Use
Concentration Switch Over
5.1 The chemical composition of stainless steels must be
Element Wavelength, nm
Points
determined accurately in order to ensure the desired metallur-
Chromium 298.919
gical properties. This procedure is suitable for manufacturing
Nickel 243.789
control and inspection testing.
227.021
218.549
216.910
6. Apparatus
Molybdenum 202.030 <1 %
6.1 Sample Preparation Equipment: 281.615
308.561 >1 %
6.1.1 Sample Mold, capable of producing castings that are
369.265
homogeneous and free of voids and porosity. The following
Manganese 293.306
A
Silicon 251.612
mold types have been found to produce acceptable samples.
288.158
6.1.1.1 Refractory Mold Ring, having a minimum inside
Copper 327.396 <0.10 %
diameter of 32 mm (1.25 in.) and a minimum height of 25 mm
224.699 >0.10 %
Carbon 193.092
(1.0 in.). The ring is placed on a flat surface of a copper plate
A
Phosphorus 178.287
approximately 50 mm (2.0 in.) thick.
Sulfur 180.731
B
6.1.1.2 Book-Type Steel Mold, to produce a chill-cast disk
Iron 271.441
322.706
64mm(2.5in.)indiameterand13mm(0.5in.)thick.Thewall
A
thickness of the mold should be 32 mm (1.25 in.) to aid chill Silicon 251.612 can have a small but significant interference from molybde-
num 251.611. Phosphorus 178.287 may show small but significant interferences
casting.
from unlisted lines or background due to molybdenum, chromium, and manga-
6.1.2 Abrasive Grinder, a suitable belt grinder, horizontal
nese. Interference corrections will not be necessary if: separate silicon and
phosphoruscurvesareusedfor316and317alloys;themanganesecontentvaries
disk grinder, or similar grinding apparatus. The resulting
only between 0.7 and 1.5 %; and the chromium concentration is held between 17
surface should be uniformly plane and free of defects. These
and 20 %.
may be either wet or dry grinding devices. Grinding materials B
Either iron line 271.441 or 322.775 with narrow entrance and exit slits to avoid
interference from manganese 322.809 can be used as internal standard with any
with grit sizes ranging from 60 to 180 have been found
of the listed analytical lines. Iron 271.441 is not appropriate for tungsten tool steels
satisfactory.
or super alloys with high cobalt because of interference from cobalt 271.442.
6.2 Excitation Source, with parameters capable of produc-
ing a usable spectrum in accordance with 10.2 and Practice
E 172.
details of equipment to be used. Equipment varies among laboratories.
6.3 Excitation Stand, suitable for mounting in optical align-
7. Reagents and Materials
ment, a flat surface of the specimen in opposition to a counter
electrode. The stand shall provide an atmosphere of argon and
7.1 Argon, either gaseous or liquid, must be of sufficient
may be water cooled. Electrode and argon are described in 7.1
purity to permit proper excitation of the analytical lines of
and 7.2.
interest.Argon of 99.998 % purity has been found satisfactory.
6.4 Spectrometer, having sufficient resolving power and
Refer to Practice E 406.
linear dispersion to separate clearly the analytical lines from
7.2 Electrodes, may be 3 to 6 mm (0.125 to 0.25 in.) in
other lines in the spectrum of a specimen in the spectral region
diameter ground to a 90° tip or whatever the instrument
170.0 to 500.0 nm. Spectrometer characteristics for two of the
manufacturer recommends for the particular source. Hard-
instruments used in this test method are described as having drawn, fine, silver rods, thoriated-tungsten rods, or other
dispersion of 0.697 nm/mm (first order), the focal length of 1
material may be used provided it can be shown experimentally
m. Spectral lines are listed in Table 1. that equivalent precision and accuracy are obtained.
6.5 Measuring System, consisting of photomultiplier tubes
having individual voltage adjustment, capacitors on which the 8. Reference Materials
output of each photomultiplier tube is stored and an electronic
8.1 Certified Reference Materials are available from the
system to measure voltages on the capacitors either directly or 5
National Institute of Standards and Technology and other
indirectly, and the necessary switching arrangements to pro-
international certification agencies.
vide the desired sequence of operation.
8.2 Reference Materials with matrices similar to that of the
6.6 Readout Console, capable of indicating the ratio of the
test specimen and containing varying amounts of the elements
analytical lines to the internal standard with sufficient precision
to be determined may be used provided they have been
to produce the accuracy of analysis desired.
chemically analyzed in accordance with ASTM standard test
6.7 Vacuum Pump, capable of maintaining a vacuum of 25
methods.These reference materials shall be homogeneous, and
µm Hg.
free of voids or porosity.
6.8 Flushing System, consisting of argon tanks, a pressure
8.3 The reference materials shall cover the concentration
regulator, and a gas flowmeter. Automatic sequencing shall be
ranges of the elements being sought. A minimum of three
provided to actuate the flow of argon at a given flow rate for a
reference materials shall be used for each element.
given time interval and to start the excitation at the end of the
required flush period. The flushing system shall be in accor-
dance with Practice E 406.
National Institute of Standards and Technology, U.S. Department of Com-
NOTE 1—It is not within the scope of this test method to prescribe all merce, Gaithersburg, MD 20899.
E1086–94 (2005)
9. Preparation of Samples Using the averages of the data for each point, determine
analytical curves in accordance with Practice E 305.
9.1 Cast samples from molten metal into a suitable mold
11.2 Standardization—Following the manufacturer’s rec-
and cool. Prepare the sur
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