This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: E1086 − 22

Standard Test Method for

Analysis of Austenitic Stainless Steel by Spark Atomic
Emission Spectrometry1
This standard is issued under the fixed designation E1086; 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 1.5 This international standard was developed in accor-

2
1.1 This test method covers the analysis of austenitic dance with internationally recognized principles on standard-
stainless steel by spark atomic emission spectrometry for the ization established in the Decision on Principles for the
following elements in the ranges shown Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
Element Composition Range, %
Chromium 17.0 to 23.0
Barriers to Trade (TBT) Committee.
Nickel 7.5 to 13.0
Molybdenum 0.01 to 3.0 2. Referenced Documents
Manganese 0.01 to 2.0
Silicon 0.01 to 0.90 2.1 ASTM Standards:3
Copper 0.01 to 0.30 E29 Practice for Using Significant Digits in Test Data to
Carbon 0.005 to 0.25
Phosphorus 0.003 to 0.15 Determine Conformance with Specifications
Sulfur 0.003 to 0.065 E135 Terminology Relating to Analytical Chemistry for
1.2 This test method is designed for the analysis of chill-cast Metals, Ores, and Related Materials
disks or inspection testing of stainless steel samples that have E305 Practice for Establishing and Controlling Spark
a flat surface of at least 13 mm (0.5 in.) in diameter. The Atomic Emission Spectrochemical Analytical Curves
samples must be sufficiently massive to prevent overheating E406 Practice for Using Controlled Atmospheres in Atomic
during the discharge and of a similar metallurgical condition Emission Spectrometry
and composition as the reference materials. E1060 Practice for Interlaboratory Testing of Spectrochemi-
cal Methods of Analysis (Withdrawn 1997)4
1.3 One or more of the reference materials must closely E1329 Practice for Verification and Use of Control Charts in
approximate the composition of the specimen. The technique Spectrochemical Analysis (Withdrawn 2019)4
of analyzing reference materials with unknowns and perform- E1806 Practice for Sampling Steel and Iron for Determina-
ing the indicated mathematical corrections (typically referred tion of Chemical Composition
to as type standardization) may also be used to correct for
interference effects and to compensate for errors resulting from 2.2 Other ASTM Documents:
instrument drift. A variety of such systems are commonly used. MNL 7 Manual on Presentation of Data and Control Chart
Any of these that will achieve analytical accuracy equivalent to Analysis5
that reported for this test method are acceptable.
3. Terminology
1.4 This standard does not purport to address all of the
3.1 Definitions—For definitions of terms used in this test
safety concerns, if any, associated with its use. It is the
method, refer to Terminology E135.
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
4. Summary of Test Method
mine the applicability of regulatory limitations prior to use.
4.1 A controlled discharge is produced between the flat
surface of the specimen and the counter electrode. The radiant
1
This test method is under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
3
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 Aug. 15, 2022. Published September 2022. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1985. Last previous edition approved in 2014 as E1086 – 14. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/E1086-22. the ASTM website.
2 4
Supporting data have been filed at ASTM International Headquarters and may The last approved version of this historical standard is referenced on
be obtained by requesting Research Report RR:E02-1023. Contact ASTM Customer www.astm.org.
5
Service at service@astm.org. ASTM Manual Series, ASTM International, 9th edition, 2018.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

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 E1086 − 22
energies of selected analytical lines are converted into electri- TABLE 1 Analytical and Internal Standard Lines
cal energies by photomultiplier tubes and stored on capacitors. Mass Fraction %
The discharge is terminated at a predetermined level of Element Wavelength, nm Switch Over
Points
accumulated radiant energy from the internal standard iron line
Chromium 298.919
or after a fixed integration time. At the end of the integration Nickel 243.789
period, the charge on each capacitor is measured, and displayed 227.021
or recorded as a relative energy or mass fraction %. 218.549
216.910
Molybdenum 202.030 <1%
5. Significance and Use 281.615
308.561 >1%
5.1 The chemical composition of stainless steels must be 369.265
determined accurately to ensure the desired metallurgical Manganese 293.306
properties. This test method is suitable for manufacturing Silicon 251.612A
288.158
control and inspection testing. Copper 327.396 < 0.10 %
224.699 > 0.10 %
6. Apparatus Carbon 193.092
Phosphorus 178.287A
6.1 Sampling and Sample Preparation Equipment: Sulfur 180.731
6.1.1 Refer to Practice E1806 for devices and practices to IronB 271.441
sample liquid and solid steel. 322.775
A
6.1.2 Abrasive Grinder, a suitable belt grinder, horizontal Silicon 251.612 can have a small but significant interference from molybdenum
251.611. Phosphorus 178.287 may show small but significant interferences from
disk grinder, or similar grinding apparatus. The resulting unlisted lines or background due to molybdenum, chromium, and manganese.
surface should be uniformly plane and free of defects. These Interference corrections will not be necessary if: separate silicon and phosphorus
may be either wet or dry grinding devices. Grinding materials curves are used for 316 and 317 alloys; the manganese content varies only
between 0.7 % and 1.5 %; and the chromium content is held between 17 % and
with grit sizes ranging from 60 to 180 have been found 20 %.
satisfactory. 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 an internal standard line
6.2 Excitation Source, with parameters capable of produc- with any of the listed analytical lines. Iron 271.441 is not appropriate for tungsten
ing a usable spectrum in accordance with 11.1. tool steels or super alloys with high cobalt because of interference from cobalt
271.442.
6.3 Excitation Stand, suitable for mounting in optical
alignment, a flat surface of the specimen in opposition to a
counter electrode. The stand shall provide an atmosphere of
argon and may be water cooled. Counter electrodes and argon 7. Reagents and Materials
are described in 7.1 and 7.2. 7.1 Argon, must be of sufficient purity (gas or liquid supply)
6.4 Spectrometer, having sufficient resolving power and to permit proper excitation of the analytical lines of interest.
linear dispersion to separate clearly the analytical lines from Argon of 99.998 % purity has been found satisfactory. Refer to
other lines in the spectrum of a specimen in the spectral region Practice E406.
170.0 nm to 500.0 nm. Spectrometer characteristics for two of 7.2 Counter Electrodes, can vary in diameter from 1.5 mm
the instruments used in this test method are described as having to 6.5 mm (depending on the instrument manufacturer) and
dispersion of 0.697 nm/mm (first order), and a focal length of typically are machined to a 90° or 120° angled tip. Silver or
1 m. Spectral lines are listed in Table 1. tungsten rods are typically used. Other material may be used
6.5 Measuring System, consisting of photomultiplier tubes provided it can be shown experimentally that equivalent
having individual voltage adjustment, capacitors on which the precision and accuracy are obtained.
output of each photomultiplier tube is stored and an electronic
system to measure voltages on the capacitors either directly or 8. Reference Materials
indirectly, and the necessary switching arrangements to pro- 8.1 Certified Reference Materials (CRMs) are available
vide the desired sequence of operation. from NIST6 and other international metrology organizations.
6.6 Readout, capable of indicating the ratio of the analytical 8.2 Reference Materials (RMs) with matrices similar to that
lines to the internal standard line with sufficient precision to of the test specimen and containing varying amounts of the
produce the accuracy of analysis desired. elements to be determined may be used provided they have
6.7 Vacuum Pump, capable of maintaining a vacuum of 25 been chemically analyzed in accordance with ASTM E01
µm Hg or less. standard test methods. These reference materials shall be
homogeneous, and free of voids or porosity.
6.8 Gas System, consisting of an argon supply with pressure
and flow regulation. Automatic sequencing shall be provided to 8.3 The reference materials shall cover the ranges of the
actuate the flow at a given rate for a specific time interval. The elements being sought. A minimum of three reference materials
flow rate may be manually or automatically controlled. The shall be used for each element.
argon system shall be in accordance with Practice E406.
NOTE 1—It is not within the scope of this test method to prescribe all 6
Available from National Institute of Standards and Technology (NIST), 100
details of equipment to be used. Equipment varies among manufacturers. Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http://www.nist.gov.

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 E1086 − 22
9. Preparation of Samples permits, perform random excitations of each calibration RM
9.1 The specimens and reference materials must be prepared and drift correction sample and repeat with different random
in the same manner. A specimen cut from a large sample sequences at least four times. Follow the spectrometer manu-
section must be of sufficient size and thickness for preparation facturer’s software procedures to convert sample intensities
and to properly fit the spectrometer stand. into mass fraction %. Using the averages of the data for each
point, determine calibration curves in accordance with Practice
9.2 Ensure the specimens are homogenous and free from E305.
voids and pits in the region to be excited. Grind the surface
with an abrasive belt or disc. Refer to 6.1.2. Perform the final 12.2 Drift Correction (Standardization)—Following the
grind with a dry abrasive belt or disc. manufacturer’s recommendations, drift correct on an initial
setup or anytime that it is known or suspected that readings
10. Preparation of Apparatus have shifted. Make the necessary corrections. Drift correction
will be done anytime verification indicates that readings have
10.1 Follow the manufacturer’s instructions for verifying
gone out of statistical control.
the optical alignment of the entrance slit and programming the
appropriate wavelengths (Table 1). 12.3 Verification—Analyze verifiers in replicate to confirm
that they read within the expected confidence interval, as
11. Excitation and Integration directed in 12.4.
11.1 Electrical Parameters—Two different types of sources 12.3.1 Each laboratory should determine the frequency of
were employed in the interlaboratory study (ILS) of this test verification necessary based on statistical analysis. Typically,
method. every 4 h to 8 h is practical and adequate (or if the instrument
11.1.1 Directional Self-Initiating Capacitor Discharge has been idle for more than 1 h). If the results are not within the
Source: control limits established in 12.4, perform a drift correction and
Capacitance, µF 0.015
then repeat verification. Repeat drift correction as necessary so
Inductance, L1, µH 310 verifications are within control limits or investigate further for
Inductance, L2, µH 20 instrument problems.
Resistance, Ω residual
Potential, V 13 500 12.4 The confidence interval will be established from ob-
Peak Current, A 90 servations of the repeatability of the verifiers by utilizing the
First Valley Current, A 60
Current pulse duration, µs 120 upper and lower limit of a control chart in accordance with
Number of discharges/s 240 Practice E1329 or ASTM Manual MNL 7.
11.1.1.1 Excitation Conditions:
13. Procedure for Excitation and Radiation Measurement
Flush, s 7 Argon Flow 0.42 m3/h
Preburn, s 20 Argon Flow 0.42 m3/h 13.1 Produce and record the intensities using the conditions
Integration, s 20 Argon Flow 0.42 m3/h in 11.1.
11.1.2 Triggered Capacitor Discharge Source: 13.2 Replicate Excitation—Make duplicate excitations of
Preburn Integration each specimen and report the average. Place the freshly
Pulse Output:
Capacitance, µF (d-c charged) 7.5 2.5
surfaced specimen on the excitation stand to effect a gas-tight
Inductance, µH 50 50 seal and adequate argon flushing. Position the specimen so
Resistance, Ω residual residual there will be a uniform pattern of excitations around its face.
Potential, V 950 950
Peak Current, A 275 100
For example, a disk-shaped specimen should have a ring of
Current pulse duration, µs 250 130 excitation marks around its outer edge and approximately 6
Number of discharges/s 120 120 mm (0.25 in.) from the edge. Avoid the center of cast
Trigger:
Capacitance (d-c charged), µF 1.2 ...
specimens because of possible quench cracks and segregation.
Inductance, µH residual ... Make a good electrical ground. If required, cool the specimen
Resistance, Ω residual ... after two excitations to prevent overheating. Examine the
Potential, V 425 ...
specimen after each excitation to evaluate the quality of
11.1.2.1 Excitation Conditions: excitation. Cracks, voids, pits, moisture, or inclusions will limit
Flush, s 2 Argon Flow 0.56 m3/h the sampling and the accuracy of a determination. Successive
Preburn, s 10 Argon Flow 0.56 m3/h
Integration, s 10 or 15 Argon Flow 0.56 m3/h
excitations shall be sufficiently separated so that the discharge
patterns do not overlap.
12. Calibration, Drift Correction (Standardization), and
Verification 14. Calculation of Results
12.1 Calibration—Using the conditions given in 11.1, excite 14.1 Average the readings obtained for each specimen. Use
each calibration RM and drift correction sample two to four the spectrometer software and the calibration curves to convert
times and bracket these with similar excitations of any verifi- the intensities obtained to mass fraction %.
ers. A verifier may be used as a calibration RM even though it 14.2 Rounding of test results obtained using this test method
is sparked only as a verifier. There shall be at least three shall be performed in accordance with Practice E29, Rounding
calibration RMs for each element, spanning the required mass Method, unless an alternative rounding method is specified by
fraction range. If the spectrometer system and software the customer or applicable material specification.

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 E1086 − 22
TABLE 2 Precision Data
Range of Duplicates,
Average Standard Deviation, Single Value
95 % Confidence
Element SampleA Mass
Fraction % Within Between
E1060, (R1)B , % E1060, (R2)C , %
Laboratory, % Laboratories, %
Carbon CT-304 0.062 0.0011 0.0033 0.0035 0.0100
CT-305 0.067 0.0015 0.0052 0.0046 0.0159
CT-316 0.061 0.0013 0.0015 0.0040 0.0047
Manganese CT-304 0.765 0.0038 0.0212 0.0120 0.0643
CT-305 1.84 0.016 0.037 0.049 0.111
CT-316 1.66 0.012 0.022 0.036 0.067
Phosphorus CT-304 0.025 0.0004 0.0025 0.0014 0.0077
CT-305 0.025 0.0004 0.0010 0.0011 0.0029
CT-316 0.031 0.0004 0.0012 0.0014 0.0036
Sulfur CT-304 0.022 0.0007 0.0017 0.0021 0.0052
CT-305 0.022 0.0007 0.0018 0.0023 0.0054
CT-316 0.024 0.0006 0.0011 0.0018 0.0034
Silicon CT-304 0.55 0.005 0.006 0.015 0.019
CT-305 0.56 0.004 0.008 0.013 0.026
CT-316 0.72 0.008 0.016 0.025 0.047
Copper CT-304 0.33 0.005 0.022 0.016 0.067
CT-305 0.29 0.005 0.022 0.016 0.019
CT-316 0.24 0.003 0.012 0.011 0.038
Nickel CT-304 9.63 0.055 0.237 0.17 0.72
CT-305 11.97 0.105 0.191 0.33 0.58
CT-316 12.54 0.073 0.242 0.23 0.73
Chromium CT-304 18.65 0.075 0.148 0.24 0.45
CT-305 18.55 0.107 0.108 0.34 0.33
CT-316 17.48 0.053 0.150 0.17 0.46
Molybdenum CT-304 0.316 0.0035 0.0082 0.0109 0.0250
CT-305 0.470 0.0020 0.0116 0.006 0.0366
CT-316 2.44 0.016 0.019 0.052 0.057
A
This is a composite of each of the five one-week daily results. This represents a total of 15 determinations. The results reported by each laboratory are on file at ASTM
International Headquarters.
B
Within-laboratory, repeatability, degrees of freedom = 10.
C
Between-laboratories, reproducibility, degrees of freedom = 14.

15. Precision and Bias2 the ILS of this test method. The agreement between the results
15.1 Precision—The precision of this test method was obtained by chemical methods and those obtained by this test
determined by submitting three stainless alloy samples to five method is displayed in Table 3. These data were obtained by
different laboratories. The ILS was conducted in accordance procedures outlined in Practice E1060.
with Practice E1060. Spectrometer calibrations were per- 15.2 Bias—There is no known bias in this test method.
formed utilizing (1) RMs supplied with the unknowns, (2)
in-house RMs, and (3) NIST and British CRMs. The unknowns 16. Keywords
and in-house RMs were tested on three separate days. The
precision data for the three unknowns are shown in Table 2. 16.1 austenitic stainless steel; spark atomic emission; spec-
15.1.1 Accuracy—The three unknowns were analyzed by trometric analysis; spectrometry
alternate chemical methods by two laboratories independent of

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 E1086 − 22
TABLE 3 Accuracy Data
Mass Fraction % Accuracy, % (95 % Confidence)
Element Sample A Assumed B
Determined E1060, Sa E1060, S(w)C E1060, S(SR)D
True Value
Carbon CT-304 0.062 0.063 0.0025 0.0011 0.0033
CT-305 0.067 0.067 0.0052 0.0015 0.0052
CT-316 0.061 0.061 0.0026 0.0013 0.0015
Manganese CT-304 0.765 0.78 0.025 0.0038 0.0212
CT-305 1.84 1.85 0.027 0.016 0.037
CT-316 1.66 1.67 0.022 0.012 0.022
Phosphorus CT-304 0.025 0.026 0.0015 0.0004 0.0025
CT-305 0.025 0.025 0.0009 0.0004 0.0010
CT-316 0.031 0.029 0.0021 0.0004 0.0012
Sulfur CT-304 0.022 0.023 0.0021 0.0007 0.0017
CT-305 0.022 0.022 0.0017 0.0007 0.0018
CT-316 0.024 0.023 0.0018 0.0006 0.0011
Silicon CT-304 0.55 0.56 0.013 0.005 0.006
CT-305 0.56 0.55 0.014 0.004 0.008
CT-316 0.72 0.69 0.013 0.008 0.016
Copper CT-304 0.33 0.34 0.023 0.005 0.022
CT-305 0.29 0.29 0.007 0.005 0.006
CT-316 0.24 0.25 0.017 0.003 0.012
Nickel CT-304 9.63 9.60 0.223 0.055 0.237
CT-305 11.97 11.95 0.181 0.105 0.191
CT-316 12.54 12.61 0.78 0.073 0.242
Chromium CT-304 18.65 18.57 0.165 0.075 0.148
CT-305 18.55 18.58 0.114 0.107 0.108
CT-316 17.48 17.60 0.184 0.053 0.150
Molybdenum CT-304 0.316 0.33 0.017 0.0035 0.0082
CT-305 0.470 0.45 0.019 0.0020 0.0116
CT-316 2.44 2.45 0.020 0.016 0.019
A
All mass fractions consist of a 15-determination average, the “apparent” outliers were left in because a statistical evaluation of the data is not a satisfactory reason for
eliminating the data values. The results for each individual laboratory are on file at ASTM International Headquarters.
B
Estimate of the overall accuracy for a single analysis from any laboratory.
C
Estimate of the standard deviation of any single random analysis within laboratories.
D
Variable use to calculate R2 in Table 2 and comprised of the = of the sum of (1) estimate of variance between laboratories and (2)Sw2 divided by the number of analyses
that are averaged to obtain the reported value.

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