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T his 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.

a Designation: E415- 21

�u 117
INTERNATIONAL

Standard Test Method for


Analysis of Carbon and Low-Alloy Steel by Spark Atomic
Emission Spectrometry 1

This standard is issued under the fixed designation E415; the number irrunediately 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 stand opening. The specimen thickness can vary significantly


according to the design of the spectrometer stand, but a
1.1 This test method covers the simultaneous determination
thickness between 10 mm and 38 mm has been found to be
of 21 alloying and residual elements in carbon and low-alloy
most practical.
steels by spark atomic emission vacuum spectrometry in the
mass fraction ranges shown Note 1. 1.3 This test method covers the routine control analysis in

Composition Range, % iron and steelmaking operations and the analysis of processed
Applicable material. It is designed for chill-cast, rolled, and forged
Element Range, Quantitative Range, specimens. Better performance is expected when reference
Mass Fraction Mass Fraction %8
OfoA materials and specimens are of similar metallurgical condition
Aluminum 0 to 0.093 0.006 to 0.093 and composition. However, it is not required for all applica­
Antimony 0 to 0.027 0.006 to 0.027 tions of this standard.
Arsenic 0 to 0. 1 0.003 to 0. 1
Boron 0 to 0.007 0.0004 to 0.007 1.4 This standard does not purport to address all of the
Calcium 0 to 0.003 0.002 to 0.003
safety concerns, if any, associated with its use. It is the
Carbon 0 to 1. 1 0. 02 to 1. 1
Chromium 0 to 8. 2 0.007 to 8. 14 responsibility of the user of this standard to establish appro­
Cobalt 0 to 0.20 0.006 to 0. 20 priate safety, health, and environmental practices and deter­
Copper 0 to 0. 5 0.006 to 0. 5
mine the applicability of regulatory limitations prior to use.
Lead e 0 to 0. 2 0.002 to 0. 2
Manganese 0 to 2. 0 0. 03 to 2. 0 1.5 This international standard was developed in accor­
Molybdenum 0 to 1.3 0.007 to 1. 3 dance with internationally recognized principles on standard­
Nickel 0 to 5.0 0.006 to 5. 0
ization established in the Decision on Principles for the
Niobium 0 to 0.12 0.003 to 0. 12
Nitrogen 0 to 0.015 0. 01 to 0.055 Development of International Standards, Guides and Recom­
Phosphorous 0 to 0.085 0.006 to 0.085 mendations issued by the World Trade Organization Technical
Silicon 0 to 1.54 0. 02 to 1.54
Barriers to Trade (TBT) Committee.
Sulfur 0 to 0.055 0.001 to 0.055
Tin 0 to 0.061 0.005 to 0.061
Titanium 0 to 0. 2 0.001 to 0. 2 2. Referenced Documents
Vanadium 0 to 0. 3 0.003 to 0. 3 3
Zirconium 0 to 0.05 0. 01 to 0.05 2.1 ASTM Standards:

A Applicable range in accordance with Guide E1763 for results reported in


E29 Practice for Using Significant Digits in Test Data to
accordance with Practice E1950. Determine Conformance with Specifications
8 Quantitative range in accordance with Practice E1601.
E135 Terminology Relating to Analytical Chemistry for
c Newly added element, refer to 15. 4 and Table 3.
Metals, Ores, and Related Materials
NoTE 1-The mass fraction ranges of the elements listed have been E305 Practice for Establishing and Controlling Spark
2
established through cooperative testing of reference materials.
Atomic Emission Spectrochemical Analytical Curves
1.2 This test method covers analysis of specimens having a E350 Test Methods for Chemical Analysis of Carbon Steel,
diameter adequate to overlap and seal the bore of the spark Low-Alloy Steel, Silicon Electrical Steel, Ingot Iron, and
Wrought Iron
E406 Practice for Using Controlled Atmospheres in Atomic
' This test method is under the jw·isdiction of ASTM Committee EO! on Emission Spectrometry
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
E691 Practice for Conducting an Interlaboratory Study to
responsibility of Subcommittee EOI.OI on Iron, Steel, and Ferroalloys.
Current edition approved Oct. I, 2021. Published November 2021. Originally
approved in 1971. Last previous edition approved in 2017 as E415 -17. DOl:
I 0.1520/E0415-21. 3 For referenced ASTM standards, visit the ASTM website, www.astm.org, or
2 Supporting data have been filed at ASTM International Headquarters and may contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
be obtained by requesting Research Report RR:EOl-1122. Contact ASTM Customer Standards volume information, refer to the standard's Document Summary page on
Service at service@astm.org. the ASTM website.

Copyright© ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
cO E415- 21
Determine the Precision of a Test Method 6.2 Excitation Source, capable of providing electrical pa­
E1019 Test Methods for Determination of Carbon, Sulfur, rameters to spark a sample. See 11.1 for details.
Nitrogen, and Oxygen in Steel, Iron, Nickel, and Cobalt
6.3 Spark Chamber, automatically flushed with argon. The
Alloys by Various Combustion and Inert Gas Fusion
spark chamber shall be mounted directly on the spectrometer
Techniques
and shall be provided with a spark stand to hold a flat specimen
E1329 Practice for Verification and Use of Control Charts in
4 and a lower counter electrode of rod form.
Spectrochemical Analysis (Withdrawn 2019)
6. 3.1 Follow the manufacturer's recommendations for
E1601 Practice for Conducting an Interlaboratory Study to
cleaning the spark chamber. During continuous operation, this
Evaluate the Performance of an Analytical Method
typically should be done every 24 h. Follow the manufacturer's
El763 Guide for Interpretation and Use of Results from
recommendations for cleaning the entrance lens or window
Interlaboratory Testing of Chemical Analysis Methods
4 (verifier data or other reference sample intensity data can
(Withdrawn 2015)
typically indicate when this is necessary).
El806 Practice for Sampling Steel and Iron for Determina­
tion of Chemical Composition 6.4 Spectral L ines Table 1 lists spectral lines and internal
-

E1950 Practice for Reporting Results from Methods of standards usable for carbon and low alloy steel. The spectrom­
Chemical Analysis eter must be able to measure at least one of the listed spectral
E2972 Guide for Production, Testing, and Value Assignment lines for each of the listed elements. Spectral lines other than
of In-House Reference Materials for Metals, Ores, and those listed in Table I may be used provided it can be shown
Other Related Materials experimentally that equivalent precision and accuracy are
5 obtained.
2.2 Other ASTM Document:
ASTM MNL 7 Manual on Presentation of Data and Control 6.5 Measuring System, spectrometer capable of converting
Chart Analysis light intensities to measurable electrical signals. The measuring
system may consist of one of the following configurations:
3. Terminology 6.5.1 A photomultiplier (PMT) array having individual
3.1 For definitions of terms used in this test method, refer to voltage adjustments, capacitors in which the output of each
Terminology E135. photomultiplier is stored, a voltage measuring system to
register the voltages on the capacitors either directly or
4. Summary of Test Method indirectly, and the necessary switching arrangements to pro­
vide the desired sequence of operation.
4.1 A capacitor discharge is produced between the flat,
6.5.2 A semiconductor detector array (CCD or CMO S),
ground surface of the disk specimen and a conically shaped
pixel selection electronics to reset the pixels and to transport
electrode. The discharge is terminated at a predetermined
the voltage of an individual pixel to one or more output ports
intensity time integral of a selected iron line, or at a predeter­
of the detector arrays, and a voltage measuring system to
mined time, and the relative radiant energies of the analytical
register the voltage of said output ports.
lines are recorded. The most sensitive lines of arsenic, boron,
6.5.3 A hybrid design using both photomultipliers and
carbon, nitrogen, phosphorus, sulfur, and tin lie in the vacuum
semiconductor arrays.
ultraviolet region. The absorption of the radiation by air in this
region is overcome by evacuating the spectrometer or by use of 6.6 Optical Path-If the instrument is operated using a
a vacuum ultraviolet (V UV ) transparent gas and flushing the V UV transparent gas, check the manufacturer's suggested gas
spark chamber with argon. purity. It may be necessary to have a gas purification system
consisting of a circulation pump and a cleaning cartridge to
5. Significance and Use keep the 02 (g) residual <500 ng/g and H20 (g) residual
5.1 This test method for the spectrometric analysis of metals < I f..lg/g and remove impurities of nitrogen and hydrocarbons.
and alloys is primarily intended to test such materials for If the instrument is using a vacuum pump, it should be capable
compliance with compositional specifications. It is assumed of maintaining a vacuum of 3.33 Pa (25 fJffi Hg) or less.
that all who use this test method will be analysts capable of NoTE 2-A pump with a displacement of at least 0.23 m3/min (8
performing common laboratory procedures skillfully and 3
ft /min) is usually adequate.
safely. It is expected that work will be performed in a properly
6.7 Gas System, consisting of an argon supply with pressure
equipped laboratory.
and flow regulation. Automatic sequencing shall be provided to
actuate the flow at a given rate for a specific time interval. The
6. Apparatus
flow rate may be manually or automatically set. The argon
6.1 Sampling Devices: system shall be in accordance with Practice E406.
6.1.1 Refer to Practice E1806 for devices and practices to
sample liquid and solid iron and steel. 7. Reagents and Materials

7.1 Counter Electrodes-The counter electrodes can be


silver or tungsten rods, or other material, provided it can be
4 The last approved version of this historical standard is referenced on
www.astm.org. shown experimentally that equivalent precision and bias are
5 ASTM Manual Series, ASTM International, 8th edition, 2010. obtained. The rods can vary in diameter from 1.5 mm to 6.5

2
cO E415- 21
TABLE 1 Internal Standard and Analytical Lines

Wavelength, Line Possible


Element
A., nm ClassificationA lnterference8
Aluminum 396.15 Mo
394.40 V, Mn, Mo, Ni
308.22 V, Mn

Antimony 217.6 Ni, Nb, Mn, W

Arsenic 189.04 V, Cr
197.20 Mo, W
193.76 Mn

Boron 345.13
182.64 S, Mn, Mo
182.59 W, Mn, Cu

Calcium 393.37
396.85 Nb

Carbon 165.81 Cr
193.09 AI

Chromium 312.26 v
313.21
425.44
298.92 Mn, V, Ni, Nb, Mo
267.72 Mn, Mo, W

Cobalt 345.35 Cr, Mo


228.62 Ni, Cr
258.03 Fe, Mn, W

Copper 212.3 Si
324.75 Mn, Nb
327.40 Nb
224.26 W, Ni
213.60 Mo, Cr
510.55 w
136.14
157.40
172.24
174.28
179.34
182.88
205.13
216.20
217.81
218.65
226.76
235.12
239.15
277.21
281.33
285.18
296.69
297.05
299.95
300.81
303.74
304.76

Iron (IS) 305.91


316.79
517.16
321.33
487.21
458.38
413.70
410.75
383.63
363.83
339.93
328.68
308.37
282.33
249.59

3
cO E415- 21
TABLE 1 Continued

Wavelength, Line Possible


Element
A., nm ClassifcationA lnterference8
226.76
218.65
216.20
193.53
190.48
187.75
149.65
271.44
273.07
Co
492.39

Lead 405.75 Mn

Manganese 293.31 Cr, Mo, Ni


255.86 Zr
263.82 AI, W

Molybdenum 379.83
Mn
202.03
277.54 Cu, V, Co, Mn
281.61 Mn
386.41 V, Cr

Nickel 471.44
227.73
341.48
352.45
231.60 Co, Ti
227.02 Nb, W
243.79 Co, Fe, Ni

Niobium 313.08 Ti, V


319.50 Mo,AI, V

Nitrogen 149.26 Fe, Ti, Si, Mn, Cu, Ni and nitride


forming elements such as Ti

Phosphorus 178.29 Mo

Silicon 288.16 Mo, Cr, W


251.61 Fe, V
212.41 Mo, Ni, V, Cu, Nb
390.55 Cr, Cu, W, Ti

Sulfur 180.73 Mn

Tin 147.52
189.99 Mn, Mo, AI

Titanium 308.80 Cu, Co


337.28 Nb

Tungsten 324.20 Nb
400.88
202.99 Ti, V, Mn
220.50 Co

Vanadium 437.92
310.23 Fe, Mo, Nb, Ni

Zirconium 468.78
349.62
343.82 w
206.19 w
A The numerals I or II in the line classification column indicate that the line has been classified in a term array and definitely assigned to the normal atom (I) or to the singly
ionized atom (II).
8 Interferences are dependent upon instrument design, spectrum line choices, and excitation conditions, and those listed require confirmation based upon specimens
selected especially to demonstrate suspected interferences.

mm (depending on the instrument design) and typically are 7.1.1 A black deposit will collect on the tip of the electrode.
machined to a 90° or 120° angled tip. This deposit should be removed between specimens (typically

4
cO E415- 21
with a wire brush). If not removed, it can reduce the overall dry abrasive belt or disc. A finer abrasive grinding media (for
intensity of the spectral radiation or transfer slight amounts of example, 120-grit) may be used for the final grind, but is not
contamination between specimens, or both. The number of essential.

NoTE 5-Specimen porosity is undesirable because it leads to the


acceptable burns on an electrode varies from one instrument to
another, and should be established in each laboratory. improper "diffuse-type" rather than the desired "concentrated-type" dis­

NoTE 3-It has been reported that thousands of burns can be performed
charge. The specimen surface should be kept clean because the specimen
is the electron emitter, and electron emission is inhibited by oily, dirty
on a tungsten electrode before replacement is necessary.
surfaces.
7.2 Inert Gas, Argon, in accordance with Practice E406.
9.2.1 Reference materials and specimens shall be refinished
dry on an abrasive belt or disc before being remeasured on the
8. Reference Materials
same area.
8.1 Certified Reference Materials ( CRMs)-These are avail­
able from the National Institute of Standards and Technology 10. Preparation of Apparatus
(NIST) and other sources and span all or part of the mass NOTE 6-The instructions given in this test method apply to most
fraction ranges listed in 1.1. They are used to calibrate the spectrometers. However, some settings and adjustments may require
modification, and additional preparation of the equipment may be re­
spectrometer for the elements of interest or to validate the
quired. It is not within the scope of an ASTM test method to prescribe the
performance of the test method. It is not recommended to use
minute details of the apparatus preparation, which may differ not only for
CRMs as verifiers or to establish the repeatability of the each manufacturer, but also for different equipment from the same
chemical measurement process. manufacturer. For a description of and further details of operation for a
particular spectrometer, refer to the manufacturer's manual(s).
NoTE 4-Certified Reference Materials manufactured by NIST are
trademarked with the name, "Standard Reference Material." 10.1 Program the spectrometer to use the internal standard
lines and one of the analytical lines for each element listed in
8.2 Reference Materials (RMs)-These are available from
Table I. Multiple lines may be used for a given element (for
multiple suppliers or can be developed in house. Reference
example, nickel) depending on the mass fraction range and the
Materials are typically used in control procedures (verifiers)
individual spectrometer software.
and in drift correction (standardization) of the spectrometer,
and they may be useful in calibrations. These reference 10.2 Test the positioning of the spectrometer entrance slit to
materials shall be homogenous and contain appropriate mass ensure that peak radiation is entering the spectrometer cham­
fractions of each element for the intended purpose. Refer to ber. This shall be done initially and as often as necessary to
Guide E2972 for production of your own reference materials. maintain proper entrance slit alignment. Follow the manufac­
turer's recommended procedures. The laboratory will deter­
8.3 Several issues can impact the selection and use of
mine the frequency of positioning the alignment based on
CRMs and RMs:
instrument performance.
8.3.1 Samples and reference materials may exhibit differ­
ences in metallurgical structure, in particular having different 10.3 Exit slit positioning and alignment is normally per­
sizes, compositions, and distributions of inclusions. Inhomo­ formed by the manufacturer at spectrometer assembly. Under
geneous distribution of inclusions can worsen repeatability of normal circumstances, further exit slit alignment is not neces­
individual measurements of elements found in the inclusions. sary (Note 7).
Some inclusions may be removed during preburn steps prior to NoTE 7-The manner and frequency of positioning or checking the
integration of intensities, causing low results. Typical samples position of the exit slits will depend on factors such as the type of
can be used to determine repeatability of individual measure­ spectrometer, the variety of analytical problems encountered, and the

ments to yield estimates consistent with performance for actual frequency of use. Each laboratory should establish a suitable check
procedure utilizing qualified service engineers.
samples.
8.3.2 For certain elements, there may be no available
11. Burn and Exposure
reference materials with metallurgical structure similar to
typical samples. Therefore, calibrations may be biased. It is 11.1 Electrical Parameters:
recommended to validate results using typical samples ana­ 11.1.1 Burn parameters are normally established by the
lyzed using Test Methods E350 and E1019. spectrometer manufacturer. The following ranges are historical
guidelines and newer instruments may vary from these:
9. Preparation of Specimens and Reference Materials Triggered Capacitor Discharge
Capacitance, >�F 10 to 15
9.1 The specimens and reference materials shall be prepared Inductance. >�H 50 to 70
in the same manner. A specimen cut from a large sample Resistance, l1 3 to 5
Potential, V 940 to 1000
section shall be of sufficient size and thickness for preparation
Current, A, r-1 0. 3 to 0. 8
and to properly fit the spectrometer stand. A 10-mm to 38-mm Number of discharges 60
thick specimen is normally most practical.
11.1.2 When parameter values are established, maintain
9.2 Ensure that the specimens are free from voids and pits in them carefully. The variation of the power supply voltage shall
the region to be measured (Note 5). Initially, grind the surface not exceed ::!::5% and preferably should be held within ::!::2%.
with a 50-grit to 80-grit abrasive belt or disc (wet or dry) or 11.1.3 Initiation Circuit-The initiator circuit parameters
mill the surface. If wet grinding, perform the final grind with a shall be adequate to uniformly trigger the capacitor discharge.

5
cO E415- 21
The following settings are historical guidelines and newer that it is known or suspected that readings have shifted. Make
instruments may vary from these: the necessary corrections either by adjusting the controls on the
Capacitance, 11F 0.0025 readout or by applying arithmetic corrections. Standardization
Inductance, 11H residual shall be done anytime verification indicates that readings have
Resistance, Q 2. 5
gone out of statistical control. In the case of automatic
Peak voltage, V 18 000
corrections conducted by the spectrometer software, observe
11.1.4 Other Electrical Parameters-Excitation units, on
the standardization factors or offsets, or both. The factors or
which the precise parameters given in 11.1.1 and 11.1.3 are not
offsets, or both, are often presented in the spectrometer
available, may be used provided that it can be shown experi­
software after standardization or stored in log files, or both.
mentally that equivalent precision and accuracy are obtained.
Refer to your instrument manual or instrument manufacturer
11.2 Burn and Measurement Conditions-The following for access to this information.
ranges are normally adequate:
12.3 Verification-Verify that the instrument's standardiza­
Argon flush period, s 5 to 15
tion is valid immediately after each standardization and as
Preburn period, s 5 to 20
Exposure period, s 3 to 30 required in accordance with 12.3.2.
12.3.1 Analyze verifiers in accordance with Section 13. If
Argon flow ft3/h Limin
results do not fall within the control limits established in 12.4,
Flush 5 to 45 2. 5 to 25
Preburn 5 to 45 2. 5 to 25 run another standardization or investigate why the instrument
Exposure 5 to 30 2. 5 to 15 may be malfunctioning.
11.2.1 Select preburn and exposure periods after a study of 12.3.2 Each laboratory shall determine the necessary fre­
volatization rates during specimen burns. Once established, quency of verification based on statistical analysis. Typically
maintain the parameters consistently. every 4 h to 8 h is practical and adequate. If the results are not
11.2.2 A high-purity argon atmosphere is required at the within the control limits established in 12.4, perform a stan­
analytical gap. Molecular gas impurities, such as nitrogen, dardization and repeat verification. Repeat standardization as
oxygen, hydrocarbons, or water vapor, either in the gas system necessary so verification results are within control limits or
or from improperly prepared specimens, should be minimized. investigate further for instrument problems.

11. 3 Electrode System- The specimen, electrically 12.4 Quality Control-Establish control limits in accor­
negative, serves as one electrode. The opposite electrode is a dance with ASTM MNL 7, Practice E1329, or other equivalent
tungsten or silver rod, the tip of which has been machined to a quality control procedure.
90° or 120° angled cone. Use either a 3 mm, 4 mm, or 5 mm
(:::':::0.1 mm) analytical gap. Condition a fresh counter electrode 13. Measurements
with two burns to six burns using the operating conditions
13.1 Place the prepared surface of the specimen on the
described in 11.1 and 11.2.
sample stand so that the measurement will impinge on a
11.4 Photomultiplier Potentials-The sensitivities of the location known to be representative of the entire specimen.
photomultipliers are normally established and set by the
spectrometer manufacturer based on the particular wavelengths NoTE 8-With certain spectrometers, a properly burned specimen
usually exhibits a dark ring around the pitted sparked area. With that
selected.
equipment, a smooth texture, white burn without the characteristic dark
11.5 Semiconductor Detector Array-In newer instruments ring indicates an improperly burned specimen. If boron nitride disks are
used to mechanically restrict the burned area of the sample, a properly
semiconductor detector arrays are replacing PMTs. The width
burned specimen may not exhibit a dark ring.
of the individual pixels shall be similar to the width of the exit
slits used in conventional instruments equipped with PMTs. 13.2 Measure specimens in duplicate and report the average
of the duplicate results.
12. Calibration, Standardization, and Verification

12.1 Calibration-Using the conditions given in 11.1 - 14. Calculation


11.3, measure calibrants and potential drift correction samples
14.1 Using the average results obtained in 13.2, calculate
in a random sequence, bracketing these with measurements of
the mass fractions of the elements from the analytical curves
any materials intended for use as verifiers. (A calibrant may be
developed in 12.1.
used later as a verifier. See 8.1.) There shall be at least three
calibrants for each element, spanning the required mass frac­ 14.2 Rounding of test results obtained using this test method
tion range. Measure each calibrant, drift correction sample, and shall be performed in accordance with the Rounding Method of
verifier two times to four times and use the average value. If Practice E29, unless an alternative rounding method is speci­
the spectrometer system and software permit, repeat with fied by the customer or applicable material specification.
different random sequences at least two times. Using the
averages of the data for each point, determine analytical curves 15. Precision and Bias
as directed in the spectrometer manufacturer's software or
15.1 Supporting data have been filed at ASTM International
Practice E305.
Headquarters and may be obtained by requesting RR:EO1-
2
12.2 Standardization-Following the manufacturer's 1122. The interlaboratory test data summarized in Table 2
recommendations, standardize on an initial setup or anytime have been evaluated in accordance with Practice E1601.

6
cO E415- 21
TABLE 2 Statistical Information

Number of Certified
Material Xbar R Bias
Laboratories Value,%
Aluminum
Sample 1 7 0.016 0.0175 0.0034 0.0047 0.0015
Sample 2 7 0.041 0.0413 0.0037 0.0067 0.0003
Sample 3 8 0.015 0.0174 0.0013 0.0028 0.0024
Sample 4 8 0.018 0.0200 0.0006 0.0024 0.0020
Sample 5 8 0.062 0.0668 0.0042 0. 0111 0.0048
Sample 6 8 0.0009 0.0023 0.0002 0.0022 0.0014
Sample 7 8 0.093 0.0890 0.0031 0.0152 -0.0040
Sample 8 7 0.021 0.0234 0.0015 0.0031 0.0024
Sample 9 7 0. 03 0.0333 0.0017 0.0037 0.0033
Sample 10 8 0.024 0.0256 0.0009 0.0028 0.0016
Sample 11 8 0.027 0.0286 0.0010 0.0032 0.0016
Sample 12 8 0.017 0.0201 0.0012 0.0043 0.0031
Sam le 13 7 0.0031 0.0010 0.0027
Antimon
Sample 1 7 0.027 0.0272 0.0026 0.0098 0.0002
Sample 2 5 0.0008 0.0007 0.0012
Sample 3 7 0.0014 0.0009 0.0022
Sample 4 6 0.0009 0.0007 0.0022
Sample 5 6 0.0004 0. 0011 0.0007 0.0024 0.0007
Sample 6 8 0.0025 0.0026 0.0011 0.0033 0.0001
Sample 7 8 0.006 0.0062 0.0011 0.0029 0.0002
Sample 8 7 0.002 0.0017 0.0007 0.0022 -0.0003
Sample 9 5 0.0006 0.0005 0.0011
Sample 10 8 0.003 0.0019 0.0012 0.0037 -0.0011
Sample 11 6 0.0010 0.0008 0.0024
Sample 12 8 0.0015 0.0008 0.0028
Sam le 13 7 0.0024 0.0010 0.0047
Arsenic
Sample 1 6 0. 05 0.0459 0.0024 0.0116 -0.0041
Sample 2 6 0.003 0.0033 0.0008 0.0014 0.0003
Sample 3 7 0.0052 0.0008 0.0047
Sample 4 7 (<0.005) 0.0004 0.0006 0.0009
Sample 5 7 0.0035 0.0037 0.0008 0.0014 0.0002
Sample 6 7 0.0056 0.0071 0.0010 0.0021 0.0015
Sample 7 7 (0.005) 0.0065 0.0008 0.0048
Sample 8 6 0.007 0.0074 0.0008 0.0037 0.0004
Sample 9 6 0.0041 0.0009 0.0034
Sample 10 7 0.004 0.0053 0.0008 0.0035 0.0013
Sample 11 7 0.0044 0.0050 0.0009 0.0014 0.0006
Sample 12 7 0.007 0.0079 0.0012 0.0076 0.0009
Sample 13 6 0. 07 0.0654 0.0077 0.0196 -0.0046
Boron
Sample 1 4 (0.00002) 0.0002 0.0001 0.0002
Sample 2 7 (0.0002) 0.0003 0.0001 0.0002
Sample 3 8 0.0004 0.0001 0.0004
Sample 4 8 (<0.0005) 0.0005 0.0001 0.0002
Sample 5 7 0.0002 0.0001 0.0002
Sample 6 8 0.0002 0.0003 0.0000 0.0002 0.0001
Sample 7 8 0.0047 0.0045 0.0004 0.0020 -0.0002
Sample 8 5 0.0002 0.0001 0.0005
Sample 9 4 0.0003 0.0000 0.0004
Sample 10 7 0.0002 0.0001 0.0002
Sample 11 8 0.0003 0.0001 0.0004
Sample 12 8 (0.0004) 0.0004 0.0001 0.0006
Sam le 13 7 0.0005 0.0001 0.0002
Calcium
Sample 1 3 (<0.0001) 0.0001 0.0001 0.0003
Sample 2 4 (0.0005) 0.0001 0.0001 0.0001
Sample 3 8 0.0003 0.0001 0.0003
Sample 4 6 (0.001) 0.0002 0.0001 0.0002
Sample 5 4 (<0.0005) 0.0001 0.0001 0.0002
Sample 6 8 0.0012 0.0012 0.0003 0.0008 0.0000
Sample 7 8 0.0006 0.0001 0.0004
Sample 8 7 0.0003 0.0002 0.0004
Sample 9 7 0.002 0.0018 0.0004 0.0008 -0.0002
Sample 10 7 0.0003 0.0002 0.0001 0.0002 -0.0001
Sample 11 6 0.0001 0.0001 0.0002
Sample 12 3 (0.0001) 0.0001 0.0000 0.0002
Sample 13 7 0.0003 0.0003 0.0004
Carbon
Sample 1 7 0.211 0.2169 0.0073 0.0252 0.0059
Sample 2 7 0.142 0.1525 0.0084 0.0230 0.0105
Sample 3 8 0. 13 0.1384 0.0072 0.0167 0.0084

7
cO E415- 21
TABLE 2 Continued

Number of Certified
Material Xbar R Bias
Laboratories Value,%
Sample 4 8 0.658 0.6605 0.0075 0.0163 0.0025
Sample 5 8 0.483 0.4892 0.0092 0.0124 0.0062
Sample 6 8 0.457 0.4687 0.0110 0.0156 0.0117
Sample 7 8 0.332 0.3251 0.0202 0.0279 -0.0069
Sample 8 7 0.128 0.1305 0.0045 0.0076 0.0025
Sample 9 7 0. 12 0.1196 0.0039 0.0142 -0.0004
Sample 10 8 1. 03 1.024 0.0170 0.0227 -0.006
Sample 11 8 0.255 0.2530 0.0072 0.0137 -0.0020
Sample 12 8 0.107 0.1114 0.0040 0.0115 0.0044
Sample 13 7 0.376 0.3593 0.0280 0.0280 -0.0167
Chromium
Sample 1 7 0.081 0.0797 0.0020 0.0066 -0.0013
Sample 2 7 0.044 0.0444 0.0009 0.0051 0.0004
Sample 3 8 4. 22 4. 209 0.0327 0.3209 -0.011
Sample 4 8 0. 16 0.1564 0.0030 0.0133 -0.0036
Sample 5 8 0.021 0.0190 0.0012 0.0035 -0.0020
Sample 6 8 0.098 0.0973 0.0013 0.0079 -0.0007
Sample 7 8 5.11 5.086 0.0432 0.3534 -0.024
Sample 8 7 2. 09 2.095 0.0169 0.0832 0.005
Sample 9 7 2. 56 2.557 0.0167 0.1249 -0.003
Sample 10 8 1. 36 1.356 0.0221 0.0911 -0.004
Sample 11 8 0. 34 0.3334 0.0023 0.0255 -0.0066
Sample 12 8 8. 22 8. 143 0.0789 0.8918 -0.077
Sample 13 7 0.062 0.0650 0.0083 0.0083 0.0030
Cobalt
Sample 1 7 0. 19 0.1885 0.0011 0.0217 -0.0015
Sample 2 7 0.005 0.0033 0.0002 0.0028 -0.0017
Sample 3 8 0.011 0. 0116 0.0006 0.0026 0.0006
Sample 4 8 0.0019 0.0020 0.0009 0.0024 0.0001
Sample 5 8 0.005 0.0038 0.0006 0.0025 -0.0012
Sample 6 8 0.0078 0.0072 0.0007 0.0032 -0.0006
Sample 7 8 0.006 0.0071 0.0009 0.0026 0.0011
Sample 8 7 0. 01 0.0096 0.0006 0.0033 -0.0004
Sample 9 7 0.0088 0.0009 0.0029
Sample 10 8 0.007 0.0068 0.0009 0.0028 -0.0002
Sample 11 8 0. 01 0.0093 0.0009 0.0022 -0.0007
Sample 12 8 0.016 0.0160 0.0008 0.0041 0.0000
Sample 13 7 0.0061 0.0009 0.0032
Co er
Sample 1 7 0.023 0.0231 0.0011 0.0030 0.0001
Sample 2 7 0. 03 0.0339 0.0014 0.0034 0.0039
Sample 3 8 0.11 0.1151 0.0045 0.0101 0.0051
Sample 4 8 0.151 0.1518 0.0070 0.0146 0.0008
Sample 5 8 0.015 0.0145 0.0007 0.0032 -0.0005
Sample 6 8 0.299 0.2993 0.0039 0.0254 0.0003
Sample 7 8 0.057 0.0569 0.0025 0.0058 -0.0001
Sample 8 7 0.177 0.1784 0.0034 0.0104 0.0014
Sample 9 7 0. 08 0.0797 0.0034 0.0061 -0.0003
Sample 10 8 0.106 0.1068 0.0081 0.0130 0.0008
Sample 11 8 0.11 0.1094 0.0049 0.0103 -0.0006
Sample 12 8 0.115 0.1190 0.0050 0.0097 0.0040
Sample 13 7 0.051 0. 0511 0.0031 0.0047 0.0001
Man anese
Sample 1 7 0.316 0.3153 0.0033 0.0130 -0.0007
Sample 2 7 1. 12 1.148 0.0200 0.0373 0.028
Sample 3 8 0. 44 0.4549 0.0058 0.0161 0.0149
Sample 4 8 0.82 0.8319 0.0176 0.0336 0.0119
Sample 5 8 0. 72 0.7330 0.0081 0.0265 0.0130
Sample 6 8 0.772 0.7825 0.0116 0.0298 0.0105
Sample 7 8 0.169 0.1713 0.0033 0.0091 0.0023
Sample 8 7 0. 441 0.4437 0.0066 0.0168 0.0027
Sample 9 7 0. 55 0.5584 0.0075 0.0226 0.0084
Sample 10 8 0. 33 0.3340 0.0075 0.0182 0.0040
Sample 11 8 1.42 1.445 0.0132 0.0551 0.025
Sample 12 8 0.333 0.3374 0.0028 0.0131 0.0044
Sample 13 7 0. 8 0.8070 0.0251 0.0402 0.0070
Mol benum
Sample 1 7 0. 05 0.0517 0.0016 0.0024 0.0017
Sample 2 7 0.008 0.0083 0.0002 0.0034 0.0003
Sample 3 8 0. 47 0.4743 0.0095 0.0270 0.0043
Sample 4 8 0.019 0.0204 0.0009 0.0033 0.0014
Sample 5 8 0.005 0.0051 0.0004 0.0037 0.0001
Sample 6 8 0.0419 0.0417 0.0019 0.0026 -0.0002
Sample 7 8 1.28 1.307 0.0415 0.1200 0.027

8
cO E415- 21
TABLE 2 Continued

Number of Certified
Material Xbar R Bias
Laboratories Value,%
Sample 8 7 0.89 0.9044 0.0163 0.0798 0.0144
Sample 9 7 1. 02 1.035 0.0128 0.1032 0.015
Sample 10 8 0.044 0.0448 0.0013 0.0024 0.0008
Sample 11 8 0. 42 0.4210 0.0103 0.0168 0.0010
Sample 12 8 0. 9 0.8976 0.0215 0.0490 -0.0024
Sample 13 7 0.2 0.1978 0.0228 0.0228 -0.0022
Nickel
Sample 1 7 0. 43 0.4286 0.0044 0.0347 -0.0014
Sample 2 7 0.029 0.0316 0.0006 0.0027 0.0026
Sample 3 8 0. 12 0.1290 0.0020 0.0091 0.0090
Sample 4 8 0.163 0.1682 0.0031 0.0116 0.0052
Sample 5 8 0.015 0.0146 0.0007 0.0031 -0.0004
Sample 6 8 0.154 0.1573 0.0018 0.0119 0.0033
Sample 7 8 0. 445 0.4486 0.0074 0.0363 0.0036
Sample 8 7 0.197 0.1999 0.0021 0.0159 0.0029
Sample 9 7 0. 25 0.2498 0.0033 0.0178 -0.0002
Sample 10 8 0.135 0.1356 0.0035 0.0115 0.0006
Sample 11 8 1.74 1.728 0.0237 0.0867 -0.012
Sample 12 8 0.123 0.1213 0.0023 0.0105 -0.0017
Sample 13 7 0.069 0.0694 0.0019 0.0071 0.0004
Niobium
Sample 1 7 0.003 0.0031 0.0003 0.0013 0.0001
Sample 2 7 0.041 0.0415 0.0015 0.0074 0.0005
Sample 3 8 0.002 0.0064 0.0004 0.0028 0.0044
Sample 4 8 0.024 0.0245 0.0021 0.0048 0.0005
Sample 5 5 (<0.002) 0.0003 0.0002 0.0006
Sample 6 7 0.0009 0.0005 0.0002 0.0007 -0.0004
Sample 7 8 0.122 0.1178 0. 011 0.0215 -0.0042
Sample 8 7 (<0.003) 0.0036 0.0003 0.0018
Sample 9 7 0.0044 0.0003 0.0018
Sample 10 8 0.0021 0.0003 0.0015
Sample 11 8 0.0013 0.0003 0.0022
Sample 12 8 0.076 0.0839 0.0019 0.0139 0.0079
Sample 13 6 0.0005 0.0003 0.0006 0.0005
Nitro en
Sample 1 7 0.0099 0.0083 0.0008 0.0048 -0.0016
Sample 2 7 0.0078 0.0010 0.0050
Sample 3 8 0.018 0.0228 0.0684 0.0684 0.0048
Sample 4 6 0. 0011 0.0004 0.0029
Sample 5 8 0.0056 0.0040 0.0009 0.0050 -0.0016
Sample 6 8 0.0106 0.0099 0.0010 0.0055 -0.0007
Sample 7 8 0.0076 0.0094 0.0013 0.0054 0.0018
Sample 8 7 0.0097 0.0102 0.0012 0.0056 0.0005
Sample 9 7 0.0101 0.0009 0.0064
Sample 10 8 0.0084 0.0075 0.0007 0.0048 -0.0009
Sample 11 8 0.0066 0.0071 0.0008 0.0051 0.0005
Sample 12 6 0.055 0.0564 0.0026 0.0233 0.0014
Sam le 13 7 0.0106 0.0010 0.0051
Phos horous
Sample 1 7 0.018 0.0170 0.0007 0.0043 -0.0010
Sample 2 7 0.016 0.0183 0.0012 0.0053 0.0023
Sample 3 8 0.017 0.0159 0.0008 0.0047 -0.0011
Sample 4 8 0.011 0. 0112 0.0010 0.0043 0.0002
Sample 5 8 0. 01 0.0090 0.0007 0.0029 -0.0010
Sample 6 8 0.0096 0.0101 0.0018 0.0034 0.0005
Sample 7 8 0.006 0.0064 0.0008 0.0029 0.0004
Sample 8 7 0.012 0.0129 0.0008 0.0034 0.0009
Sample 9 7 0. 01 0.0088 0.0006 0.0017 -0.0012
Sample 10 8 0.013 0.0164 0.0564 0.0567 0.0034
Sample 11 8 0. 01 0.0087 0.0008 0.0019 -0.0013
Sample 12 8 0.008 0.0078 0.0008 0.0020 -0.0002
Sample 13 7 0.061 0.0584 0.0068 0.0105 -0.0026
Silicon
Sample 1 7 0.015 0.0127 0.0010 0.0071 -0.0023
Sample 2 7 0.058 0.0668 0.0012 0.0088 0.0088
Sample 3 8 0.27 0.2787 0.0043 0.0117 0.0087
Sample 4 8 0. 5 0.4959 0.0074 0.0153 -0.0041
Sample 5 8 0. 24 0.2251 0.0036 0.0094 -0.0149
Sample 6 8 0. 21 0. 2111 0.0030 0. 0111 0.0011
Sample 7 8 0.775 0.7541 0.0157 0.0330 -0.0209
Sample 8 7 0.255 0.2520 0.0022 0.0100 -0.0030
Sample 9 7 0. 32 0. 3211 0.0039 0.0117 0. 0011
Sample 10 8 0. 32 0.3217 0.0057 0.0116 0.0017
Sample 11 8 1.54 1.519 0.0217 0.0612 -0.021

9
cO E415- 21
TABLE 2 Continued

Number of Certified
Material Xbar R Bias
Laboratories Value,%
Sample 12 8 0.327 0.3322 0.0043 0.0197 0.0052
Sample 13 7 0. 31 0.3044 0.0082 0.0135 -0.0056
Sulfur
Sample 1 7 0.005 0.0460 0.0024 0.3116 0.0410
Sample 2 7 0.008 0.0076 0.0008 0.0031 -0.0004
Sample 3 8 0.015 0.0146 0.0010 0.0021 -0.0004
Sample 4 8 0.012 0.0135 0.0018 0.0044 0.0015
Sample 5 8 0.025 0.0232 0.0039 0.0064 -0.0018
Sample 6 8 0.0234 0.0221 0.0035 0.0054 -0.0013
Sample 7 8 0.033 0.0321 0.0038 0.0063 -0.0009
Sample 8 7 0.026 0.0241 0.0026 0.0056 -0.0019
Sample 9 7 0.003 0.0013 0.0005 0.0014 -0.0017
Sample 10 8 0.014 0.0144 0.0032 0.0046 0.0004
Sample 11 8 0.004 0.0046 0.0007 0.0007 0.0006
Sample 12 8 0.008 0.0076 0.0005 0.0023 -0.0004
Sample 13 7 0.047 0.0454 0.0082 0.0112 -0.0016
Tin
Sample 1 7 0.061 0.0588 0.0011 0.0079 -0.0022
Sample 2 7 0.002 0.0028 0.0008 0.0022 0.0008
Sample 3 8 0.008 0.0073 0.0003 0.0014 -0.0007
Sample 4 8 0.026 0.0263 0.0010 0.0028 0.0003
Sample 5 7 (0.0006) 0.0015 0.0002 0.0014
Sample 6 8 0.0124 0.0127 0.0006 0.0016 0.0003
Sample 7 8 0.005 0.0049 0.0003 0.0023 -0.0001
Sample 8 7 0.013 0.0135 0.0003 0.0015 0.0005
Sample 9 7 0.0047 0.0002 0.0019
Sample 10 8 0.006 0.0064 0.0010 0.0013 0.0004
Sample 11 8 0.006 0.0075 0.0003 0.0013 0.0015
Sample 12 8 0.009 0.0094 0.0021 0.0022 0.0004
Sample 13 7 0.054 0.0481 0.0043 0.0062 -0.0059
Titanium
Sample 1 7 0.004 0.0036 0.0002 0.0008 -0.0004
Sample 2 7 0.008 0.0076 0.0003 0.0009 -0.0004
Sample 3 8 0.003 0.0036 0.0002 0.0005 0.0006
Sample 4 8 0.015 0.0156 0.0011 0.0016 0.0006
Sample 5 7 (0.001) 0. 0011 0.0001 0.0006
Sample 6 8 0.0009 0.0009 0.0001 0.0006 0.0000
Sample 7 8 0.034 0.0358 0.0028 0.0040 0.0018
Sample 8 7 (0.001) 0.0012 0.0001 0.0006
Sample 9 7 0.0017 0.0001 0.0006
Sample 10 8 0.003 0.0020 0.0010 0.0012 -0.0010
Sample 11 8 0.003 0.0037 0.0004 0.0007 0.0007
Sample 12 8 (0.002) 0.0027 0.0001 0.0006
Sample 13 7 0. 01 0. 0112 0.0022 0.0028 0.0012
Vanadium
Sample 1 7 0. 01 0.0106 0.0008 0.0019 0.0006
Sample 2 7 0.012 0.0122 0.0007 0.0024 0.0002
Sample 3 8 0.016 0.0194 0.0008 0.0021 0.0034
Sample 4 8 0.012 0.0124 0.0010 0.0030 0.0004
Sample 5 7 (<0.002) 0.0012 0.0002 0.0014
Sample 6 8 0.0295 0.0298 0.0009 0.0029 0.0003
Sample 7 8 0.802 0.8233 0.0205 0.0403 0.0213
Sample 8 7 0.003 0.0036 0.0005 0.0013 0.0006
Sample 9 7 0.015 0.0134 0.0009 0.0020 -0.0016
Sample 10 8 0.005 0.0046 0.0004 0.0015 -0.0004
Sample 11 8 0.003 0.0020 0.0003 0.0020 -0.0010
Sample 12 8 0.236 0.2366 0.0062 0.0163 0.0006
Sample 13 7 0.0036 0.0025 0.0031
Zirconium
Sample 1 6 (0.01) 0.0278 0.0096 0.0108
Sample 2 6 0.022 0.0173 0.0055 0.0061 -0.0047
Sample 3 7 0.0005 0.0002 0.0019
Sample 4 7 0.0003 0.0001 0.0006
Sample 5 7 0.0002 0.0001 0.0004
Sample 6 7 0.0007 0.0003 0.0001 0.0005 -0.0004
Sample 7 7 0.052 0.0513 0.0126 0.0190 -0.0007
Sample 8 5 0.0004 0.0001 0.0015
Sample 9 6 0.0005 0.0006 0.0023
Sample 10 7 0.0003 0.0002 0.0008
Sample 11 7 0.0003 0.0001 0.0011
Sample 12 7 (0.001) 0.0007 0.0001 0.0034
Sample 13 6 0.0003 0.0001 0.0006

10
cO E415- 21
15.2 Precision-Up to eight laboratories cooperated in per­ Practice E691 was followed for the design and analysis of the
6
forming this test method with thirteen unknown samples and data; the details are given in RR:EOI-2000. The interlabora­
obtained the statistical information summarized in Table 2. tory test data summarized in Table 3 have been evaluated in

15.3 Bias-Differences between average composition deter­ accordance with Practice El601.

mined by this method and the certified compositions provides


16. Keywords
the bias found in the interlaboratory study. Bias information is
found in Table 2. 16.1 carbon steel; low-alloy steel; spark atomic emission;
spectrometric analysis; spectrometry
15.4 A new study was performed in 2019 in order to
demonstrate method precision and bias for lead. Eight labora­
tories participated in this interlaboratory study, testing eight
6 Supporting data have been filed at ASTM International Headquarters and may
materials. One of the laboratories submitted datasets from two be obtained by requesting Research Report RR:EOl-2000. Contact ASTM Customer
instruments, making nine datasets available in most cases. Service at service@astm.org.

11
cO E415- 21
TABLE 3 Statistical Information for Lead
Material Certified Number of AverageA Bias Repeatability Reproducibility Repeatability Reproducibility
Value,% Labs Standard Standard Limit Limit
Deviation Deviation
n x % s s r R
SS457/2 0.0098 9 0.00966 -1. 47 0.00045 0.00096 0.00127 0.00268
SS458/2 0.0140 9 0.01429 2. 08 0.00055 0.00150 0.00153 0.00421
SS456/2 0.0189 9 0.01861 -1.53 0.00032 0.00221 0.00089 0.00618
SS459/2 0.0044 9 0.00419 -4. 73 0.00016 0.00035 0.00044 0.00099
SS460/2 0.0005 9 0.00045 -9.64 0.00010 0.00018 0.00027 0.00050
BS 728 0.1740 9 0.18157 4. 35 0.01045 0.02512 0.02926 0.07035
BS 75G 0.2470 sa 0.26130 5. 79 0.01713 0.02837 0.04797 0.07943
1264A 0.0240 9 0.02442 1.74 0.00107 0.00306 0.00299 0.00857
A The average of the laboratories' calculated averages.
8 BS75G does not meet the minimum number of laboratories required for Practice E691 compliant precision.

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12

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