Designation: E1085 − 16

Standard Test Method for

Analysis of Low-Alloy Steels by Wavelength Dispersive
X-Ray Fluorescence Spectrometry 1
This standard is issued under the fixed designation E1085; 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 2. Referenced Documents

1.1 This test method covers the wavelength dispersive 2.1 ASTM Standards:2
X-ray fluorescence analysis of low-alloy steels for the follow- E29 Practice for Using Significant Digits in Test Data to
ing elements: Determine Conformance with Specifications
E135 Terminology Relating to Analytical Chemistry for
Element Mass Fraction
Range, % Metals, Ores, and Related Materials
Calcium 0.001 to 0.007 E691 Practice for Conducting an Interlaboratory Study to
Chromium 0.04 to 2.5
Cobalt 0.03 to 0.2
Determine the Precision of a Test Method
Copper 0.03 to 0.6 E1361 Guide for Correction of Interelement Effects in
Manganese 0.04 to 2.5 X-Ray Spectrometric Analysis
Molybdenum 0.005 to 1.5
Nickel 0.04 to 3.0
E1621 Guide for Elemental Analysis by Wavelength Disper-
Niobium 0.002 to 0.1 sive X-Ray Fluorescence Spectrometry
Phosphorus 0.010 to 0.08 E2857 Guide for Validating Analytical Methods
Silicon 0.06 to 1.5
Sulfur 0.009 to 0.1
Vanadium 0.012 to 0.6 3. Terminology
NOTE 1—Unless exceptions are noted, mass fraction ranges can be 3.1 For definitions of terms used in this test method, refer to
extended and additional elements can be included by the use of suitable Terminology E135.
reference materials and measurement conditions. Deviations from the
published scope must be validated by experimental means. See Guide 4. Summary of Test Method
E2857 for information on validation options.
4.1 The test specimen is finished to a clean uniform surface
1.2 The values stated in the International System of Units and then irradiated with a primary X-ray beam of high energy.
(SI) are to be regarded as standard. The values given in The secondary X-rays produced are dispersed by means of
parentheses are mathematical conversions to other units that crystals, and the intensities (also called count rates) are
are provided for information only, because they may used in measured by suitable detectors at selected wavelengths. Radia-
older software and laboratory procedures. tion measurements are made based on the time required to
1.3 This standard does not purport to address all of the reach a fixed number of counts, or on the total counts obtained
safety concerns, if any, associated with its use. It is the for a fixed time. Mass fractions of the elements are determined
responsibility of the user of this standard to establish appro- by relating the measured intensities from unknown specimens
priate safety and health practices and determine the applica- to analytical curves prepared with suitable reference materials.
bility of regulatory limitations prior to use. Specific precau- Either a fixed-channel, polychromator system or a sequential,
tionary statements are given in Section 10. wavelength dispersive monochromator system may be used to
provide simultaneous or sequential determinations of elements,
respectively.
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
2
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 May 1, 2016. Published June 2016. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1987. Last previous edition approved in 2009 as E1085 – 09. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/E1085-16. the ASTM website.

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

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 E1085 − 16
5. Significance and Use 7.2.1.1 For the determination of calcium, only chromium
5.1 This test method is suitable for manufacturing control target tubes were tested. Other targets may be used provided
and for verifying that a product meets specifications. This test they produce data that meets the precision and bias in Section
method provides rapid, multi-element determinations with .
sufficient accuracy to ensure product quality and to minimize 7.2.2 Analyzing Crystals, flat or curved crystals with opti-
production delays. The analytical performance data may be mized capability for the diffraction of the wavelengths of
used as a benchmark to determine if similar X-ray spectrom- interest.
eters provide equivalent precision and accuracy, or if the 7.2.3 Collimator, for limiting the characteristic X-rays to a
performance of a particular X-ray spectrometer has changed. parallel bundle when flat crystals are used. Curved crystals do
not require a collimator.
5.2 Calcium is sometimes added to steel to affect inclusion 7.2.4 Detectors, sealed or gas-flow proportional-type, scin-
shape to enhance certain mechanical properties of steel. This tillation counters, or equivalent.
test method is useful for determining the residual calcium in 7.2.5 Vacuum System, providing for the determination of
the steel after such treatment. elements whose radiation is absorbed by air, atomic number 20
5.2.1 Because calcium occurs primarily in inclusions, the (calcium) or lower. The system shall consist of a vacuum
precision of this test method is a function of the distribution of pump, gage, and electrical controls to provide automatic
the calcium-bearing inclusions in the steel. The variation of pumpdown of the optical path and maintain a controlled
determinations on freshly prepared surfaces will give some pressure, usually 13 Pa (100 µm Hg) or less, controlled to
indication of the distribution of these inclusions. 6 3 Pa (6 20 µm Hg).
6. Interferences 8. Reagents and Materials
6.1 Interelement or matrix effects may exist for some 8.1 Detector Gas (P-10), consisting of a mixture of 90 %
elements in 1.1. Mathematical corrections may be used to argon and 10 % methane, for use with gas-flow proportional
compensate for these effects. Various mathematical correction counters only.
procedures are commonly utilized. See Guide E1361 and
Guide E1621. Any of these procedures is acceptable that will 9. Reference Materials
achieve analytical accuracy equivalent to that provided by this
9.1 Certified Reference Materials are available from na-
test method.
tional metrology institutes, other government organizations,
6.2 Spectroscopic interferences or line overlaps may be and commercial suppliers.
observed, if the energy resolution of the measurement condi-
9.2 Reference Materials with matrices similar to that of the
tions is insufficient. Mathematical corrections may be used to
test specimen and containing varying amounts of the elements
calibrate the overlaps and perform corrections. See Guide
to be determined may be used provided they have been
E1621.
chemically analyzed in using valid, independent test methods.
6.3 Because trace amounts of calcium are being determined These reference materials shall be homogeneous, and free of
with this test method, exercise care not to contaminate the voids or porosity.
specimen. Calcium in the grinding medium will contaminate
9.3 The reference materials shall cover the mass fraction
the specimen to the extent that erratic and incorrect results will
ranges of the elements being sought. A minimum of three
be obtained. Therefore, the grinding medium shall be analyzed
reference materials shall be used for each element. When
for calcium, and only materials that are free of calcium shall be
correction factors for matrix effects and spectroscopic interfer-
used.
ences are to be calculated from the empirical data as calibration
7. Apparatus parameters, at least one additional reference material is needed
for each correction parameter. Refer to Guide E1361 and Guide
7.1 Specimen Preparation Equipment:
E1621.
7.1.1 Surface Grinder or Sander with Abrasive Belts, Disks, NOTE 2—Calculation of correction factors for matrix effects and
or Lathe, capable of providing a flat, uniform surface on the spectroscopic interferences from X-ray theory can be used to reduce the
reference materials and test specimens. number of reference materials required for calibration.
7.1.1.1 When calcium is to be determined, 240-grit,
calcium-free silicon carbide belts or disks shall be used. 10. Hazards
7.2 Wavelength Dispersive Spectrometer, designed for X-ray 10.1 U.S Nuclear Regulatory Commission Standards for
fluorescence analysis, and equipped with specimen holders and ionizing radiation as found in the Code of Federal Regulations
a specimen chamber. The chamber may contain a specimen 10 CFR Part 19, “Notices, Instructions and Reports to Workers:
spinner, and must be equipped for vacuum or helium-flushed Inspection and Investigations” and 10 CFR Part 20, ”Standards
operation for the determination of elements of atomic number for Protection Against Radiation”3 shall be observed at all
20 (calcium) or lower. X-ray emission spectrometer installations in the U.S. It is also
7.2.1 X-Ray Tubes, with targets of various high-purity
elements, that are capable of continuous operation at required 3
Available from U.S. Government Printing Office, Superintendent of
potentials and currents, and will excite the elements to be Documents, 732 N. Capitol St., NW, Washington, DC 20401-0001, http://
determined. www.access.gpo.gov

2
 E1085 − 16
recommended that operating and maintenance personnel fol- Element Crystal DetectorA
low the guidelines of safe operating procedures given in similar Nickel LiF(200), LiF(220) SP, FP, Sc
Chromium LiF(200), LiF(220) FP, SP, Sc
handbooks on radiation safety. Manganese LiF(200), LiF(220) FP, SP, Sc
10.2 Exposure to excessive quantities of high energy radia- Silicon PET, InSb FP
Molybdenum LiF(200), LiF(220) Sc, SP
tion such as those produced by X-ray spectrometers is injurious Copper LiF(200), LiF(220) SP, FP, Sc
to health. The operator should take appropriate actions to avoid Vanadium LiF(200), LiF(220) FP, SP, Sc
exposing any part of their body, not only to primary X-rays, but Cobalt LiF(200), LiF(220) FP, SP, Sc
Sulfur Ge FP
also to secondary or scattered radiation that might be present. Niobium LiF(200), LiF(220) Sc, SP
The X-ray spectrometer should be operated in accordance with Phosphorus Ge FP
Calcium LiF(200) FP
regulations governing the use of ionizing radiation. During
manufacturing, manufacturers of X-ray fluorescence spectrom- A
SP = Sealed Proportional, Sc = Scintillation, and FP = Flow Proportional.
eters generally build into X-ray equipment appropriate shield-
ing and safety interlocks that minimize the risk of excessive 12.4.2 Counting Time—Collect a sufficient number of
radiation exposure to operators. Operators should not attempt counts so that the repeatability of the analysis will not be
to bypass or defeat these safety devices. Only authorized affected by variance in X-ray counting. A minimum of 10 000
personnel should service X-ray spectrometers. counts is required for 1 % relative standard uncertainty and 40
000 counts for 0.5 %.
11. Preparation of Reference Materials and Test
Specimens 13. Calibration and Standardization
11.1 Prepare the reference materials and test specimens to 13.1 Calibration (Preparation of Analytical Curves)—
provide a clean, flat uniform surface to be exposed to the X-ray Using the conditions given in Section 12, measure a series of
beam. For abrasive sanding, select a grit size, and use that grit reference materials that cover the mass fraction ranges of
and size exclusively for all reference materials and test interest. Prepare an analytical curve for each element being
specimens. Aluminum oxide and zirconium oxide belts and determined. Refer to Guide E1361 and Guide E1621.
discs with a grit size of between 60 and 180 have been found 13.2 Standardization (Drift Correction)—Using a control
suitable. reference material, check the calibration of the X-ray spec-
11.2 Refinish the surfaces of the reference materials and test trometer at a frequency consistent with statistical process
specimens as needed to eliminate surface contamination. control practice, or when the detector gas or major components
have been changed. If the calibration check indicates that drift
12. Preparation of Apparatus has occurred, make appropriate adjustments in accordance with
12.1 Prepare and operate the spectrometer in accordance the instructions in the manufacturer’s manual.
with the manufacturer’s instructions.
14. Procedure
NOTE 3—It is not within the scope of this test method to prescribe
minute details relative to the preparation of the apparatus. For a descrip- 14.1 Specimen Loading—Orient the reference materials and
tion and specific details concerning the operation of a particular test specimens in the specimen chamber so that the relationship
spectrometer, refer to the manufacturer’s manual. between the X-ray beam and the grinding striations is the same
12.1.1 Start-up—Turn on the spectrometer and allow suffi- for all measurements. This is an essential requirement if the
cient time for instrument stabilization prior to taking measure- spectrometer is not equipped with a specimen spinner, but is
ments. not necessary when a spinner is used.
12.2 Tube Power Supply—Adjust the voltage of the power 14.2 Excitation—Expose the specimen to primary X-rays in
supply to produce optimum conditions. accordance with Section 12.
12.2.1 The voltage and current established as optimum for 14.3 Radiation Measurements—Obtain the count rate mea-
the power supply in an individual laboratory shall be repro- surement for each element. Either fixed count or fixed time
duced for subsequent measurements. modes may be used. Obtain at least the predetermined mini-
12.3 Proportional Counter Gas Flow—When a gas-flow mum counts for all specimens.
proportional counter is used, adjust the flow of the P-10 gas in 14.4 Replicate Measurements—Make a single measurement
accordance with the equipment manufacturer’s instructions. on each test specimen. The performance of an X-ray spectrom-
When changing P-10 tanks, the detectors should be adequately eter is not improved significantly by making multiple measure-
flushed with detector gas and adjusted before the instrument is ments on the same surface of the specimen. Confidence in the
used. accuracy of analysis will improve by making multiple mea-
12.4 Measurement Conditions—The K-L2,3 (Kα) line is surements on freshly prepared surfaces of the same specimen
measured for each element. The peak location, when using a or by analyzing more than one specimen.
scanning spectrometer, should be optimized for each instru-
ment. 15. Calculation of Results
12.4.1 Crystals and Detectors—The following crystals and 15.1 Using the count rates measured for the test specimen
detectors used for the elements are listed below. In some and the appropriate analytical curves, determine the mass
spectrometers, multiple detectors may be used simultaneously. fractions of the elements.

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 E1085 − 16
TABLE 1 Repeatability and Reproducibility
(For all elements, except Ca, all values have units of %)
Sample Certificate Value, % X sr sR r R
Nickel
1 0.031 ± 0.001 0.031 0.0013 0.0061 0.0037 0.0171
2 0.250 ± 0.004 0.250 0.0024 0.0104 0.0067 0.0292
3 1.30 ± 0.01 1.317 0.0051 0.0421 0.0141 0.1180
4 0.20 ± 0.01 0.203 0.0031 0.0093 0.0087 0.0260
5 0.182 ± 0.005 0.183 0.0026 0.0085 0.0072 0.0239
6 0.202 ± 0.004 0.203 0.0025 0.0089 0.0071 0.0251
7 2.97 ± 0.02 3.006 0.0189 0.1133 0.0530 0.3174
8 0.025 0.032 0.0011 0.0045 0.0032 0.0126
9 0.16 0.157 0.0031 0.0064 0.0087 0.0180
Chromium
1 1.26 ± 0.01 1.27 0.0044 0.0096 0.0123 0.0270
2 0.25 ± 0.01 0.258 0.0023 0.0108 0.0064 0.0304
3 0.062 ± 0.002 0.067 0.0017 0.0092 0.0048 0.0257
4 2.37 ± 0.03 2.36 0.0159 0.0288 0.0445 0.0806
5 0.157 ± 0.006 0.156 0.0064 0.0113 0.0179 0.0316
6 0.201 ± 0.006 0.201 0.0024 0.0099 0.0066 0.0276
7 0.56 ± 0.008 0.575 0.0038 0.0128 0.0106 0.0360
8 0.015 0.014 0.0010 0.0029 0.0029 0.0081
9 1.96 1.95 0.0319 0.0483 0.0893 0.1353
Manganese
1 2.11 ±< 0.01 2.113 0.0065 0.0116 0.0183 0.0326
2 0.91 ± 0.03 0.913 0.0053 0.0123 0.0148 0.0346
3 0.322 ± 0.007 0.314 0.0016 0.0025 0.0044 0.0071
4 0.55 ± 0.01 0.564 0.0036 0.0064 0.0102 0.0179
5 0.97 ± 0.006 0.997 0.0041 0.0126 0.0114 0.0353
6 0.75 ± 0.006 0.756 0.0029 0.0102 0.0081 0.0686
7 0.97 ± 0.02 0.908 0.0054 0.0245 0.0151 0.0686
8 0.025 0.023 0.0006 0.0079 0.0016 0.0221
9 0.325 0.319 0.0034 0.0080 0.0095 0.0223
Silicon
1 0.019 ± 0.003 0.026 0.0036 0.0173 0.0102 0.0484
2 0.235 ± 0.009 0.258 0.0071 0.0544 0.0199 0.1524
3 1.06 ± 0.01 1.14 0.0247 0.1919 0.0690 0.5373
4 0.18 ± 0.01 0.195 0.0059 0.0452 0.0166 0.1265
5 0.175 ± 0.005 0.195 0.0060 0.0439 0.0168 0.1231
6 0.456 ± 0.005 0.503 0.0100 0.0924 0.0281 0.2588
7 0.22 ± 0.01 0.234 0.0063 0.0476 0.0176 0.1334
8 0.14 0.166 0.0076 0.0390 0.0214 0.1091
9 0.75 0.821 0.0203 0.1394 0.0567 0.3902
Molybdenum
1 0.79 ± 0.01 0.792 0.0021 0.0081 0.0058 0.0225
2 0.090 ± 0.003 0.089 0.0005 0.0006 0.0013 0.0016
3 0.028 ± 0.002 0.026 0.0003 0.0009 0.0009 0.0025
4 0.93 ± 0.01 0.942 0.0025 0.0084 0.0071 0.0235
5 0.087 ± 0.005 0.089 0.0004 0.0008 0.0011 0.0024
6 0.153 ± 0.003 0.149 0.0007 0.0013 0.0019 0.0035
7 0.98 ± 0.01 1.003 0.0023 0.0159 0.0064 0.0444
8 0.005 0.002 0.0002 0.0011 0.0007 0.0032
9 1.35 1.38 0.0091 0.0159 0.0254 0.0444
Copper
1 0.032 ± 0.002 0.033 0.0008 0.0022 0.0021 0.0062
2 0.109 ± 0.002 0.110 0.0010 0.0021 0.0029 0.0059
3 0.425 ± 0.004 0.428 0.0017 0.0133 0.0048 0.0371
4 0.134 ± 0.005 0.138 0.0013 0.0028 0.0035 0.0078
5 0.060 ± 0.003 0.058 0.0009 0.0023 0.0027 0.0064
6 0.153 ± 0.005 0.152 0.0012 0.0026 0.0033 0.0074
7 0.50 ± 0.01 0.513 0.0025 0.0209 0.0069 0.0585
8 0.035 0.039 0.0010 0.0027 0.0027 0.0074
9 0.10 0.093 0.0019 0.0028 0.0052 0.0078
Vanadium
1 0.003 ± 0.0006 0.003 0.0005 0.0023 0.0015 0.0065
2 0.072 ± 0.002 0.074 0.0005 0.0043 0.0015 0.0121
3 0.441 ± 0.001 0.442 0.0128 0.0358 0.0358 0.0608
4 0.013 ± 0.000 0.013 0.0006 0.0017 0.0018 0.0048
5 0.002 ± 0.000 0.003 0.0006 0.0024 0.0017 0.0067
6 0.102 ± 0.004 0.102 0.0007 0.0044 0.0021 0.0123
7 0.50 ± 0.01 0.531 0.0040 0.0143 0.0112 0.0401
8 0.002 0.0004 0.0015 0.0012 0.0043
9 0.045 0.038 0.0008 0.0022 0.0023 0.0063
Cobalt
1 0.179 ± 0.004 0.172 0.0015 0.0277 0.0041 0.0776
2 0.025 ± 0.001 0.027 0.0010 0.0026 0.0028 0.0074
3 0.012 ± 0.002 0.014 0.0009 0.0026 0.0028 0.0074

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 E1085 − 16
TABLE 1 Continued
Sample Certificate Value, % X sr sR r R
4 0.011 ± 0.001 0.010 0.0014 0.0072 0.0039 0.0203
5 0.012 ± 0.003 0.011 0.0007 0.0038 0.0020 0.0107
6 0.042 ± 0.003 0.044 0.0009 0.0037 0.0026 0.0102
7 0.030 ± 0.003 0.027 0.0013 0.0047 0.0035 0.0132
8 0.008 0.0010 0.0057 0.0027 0.0160
9 0.01 0.005 0.0008 0.0060 0.0022 0.0167
Sulfur
1 0.044 ± 0.002 0.050 0.0012 0.0093 0.0034 0.0259
2 0.022 ± 0.000 0.024 0.0016 0.0068 0.0044 0.0190
3 0.0067 ± 0.0006 0.006 0.0007 0.0016 0.0020 0.0045
4 0.030 ± 0.0015 0.025 0.0009 0.0042 0.0025 0.0118
5 0.088 ± 0.0015 0.085 0.0026 0.0191 0.0073 0.0535
6 0.046 ± 0.0015 0.046 0.0015 0.0117 0.0041 0.0328
7 0.0083 ± 0.0005 0.006 0.0007 0.0016 0.0020 0.0045
8 0.002 0.002 0.0008 0.0016 0.0022 0.0045
9 0.039 0.040 0.0014 0.0073 0.0040 0.0205
Niobium
1 0.003 ± 0.001 0.002 0.0002 0.0008 0.0005 0.0022
2 0.049 ± 0.002 0.049 0.0004 0.0026 0.0010 0.0072
3 0.102 ± 0.002 0.106 0.0007 0.0072 0.0019 0.0203
4 0.002 ± 0.001 0.001 0.0003 0.0007 0.0008 0.0020
5 0.000 0.0002 0.0002 0.0004 0.0007
6 0.030 ± 0.001 0.028 0.0003 0.0018 0.0008 0.0049
7 0.030 ± 0.001 0.028 0.0003 0.0017 0.0009 0.0048
8 0.000 0.00 0.0001 0.0001 0.0002 0.0003
9 0.021 0.0005 0.0017 0.0015 0.0048
Phosphorus
1 0.005 ± 0.001 0.008 0.0007 0.0019 0.0019 0.0052
2 0.034 ± 0.001 0.035 0.0007 0.0018 0.0019 0.0049
3 0.074 ± 0.002 0.076 0.0008 0.0033 0.0019 0.0092
4 0.018 ± 0.002 0.019 0.0007 0.0017 0.0021 0.0049
5 0.068 ± 0.004 0.067 0.0008 0.0028 0.0023 0.0082
6 0.023 ± 0.001 0.021 0.0005 0.0015 0.0014 0.0041
7 0.056 ± 0.002 0.060 0.0010 0.0021 0.0028 0.0059
8 0.005 0.004 0.0023 0.0023 0.0065 0.0065
9 0.035 0.033 0.0009 0.0027 0.0025 0.0075
Calcium, µg/g
1 73 69.5 1.98 2.52 5.54 7.06
2 10 9.6 0.47 1.63 1.31 4.57
3 61 61.8 1.53 1.75 4.29 4.69
4 40 37.9 1.68 1.68 4.69 4.69

15.1.1 If mathematical calculations are required to correct NOTE 4—Because calcium exists in inclusions that may not be
for interelement effects, any one of a number of correction uniformly distributed within a sample, the r and R values can be expected
procedures may be employed. Refer to Guide E1361 and the to be high. To demonstrate the precision of this test method without
reflecting the variation in inclusion distribution, three samples were
equipment manufacturer’s manual for the recommended pro- analyzed without resurfacing between analyses. At mass fraction levels of
cedure for the instrument being used. 7 µg/g, 27 µg/g, and 53 µg/g, the r values were 0.4 µg/g, 0.5 µg/g, and 0.8
15.2 Rounding of test results obtained using this test method µg/g, respectively. The R values were 3.3 µg/g, 3.6 µg/g, and 2.4 µg/g,
shall be performed in accordance with Practice E29, Rounding respectively. While better precision is obtained using this technique, it is
not recommended as a general practice, as it may not reflect the general
Method, unless an alternative rounding method is specified by distribution of the calcium in the steel.
the customer or applicable material specification.
16.2 Bias (Accuracy)—There is no bias indicated in this test
16. Precision and Bias method.
16.1 Precision—An acceptable number of laboratories
tested this test method in accordance with Practice E691. 17. Keywords
Precision data, including repeatability (precision within 17.1 low-alloy steel; wavelength dispersive; X-ray fluores-
laboratories), r, and reproducibility (precision between cence
laboratories), R, are provided in Table 1.

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 E1085 − 16
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