ASTM E572-02a(2006)e1
(Test Method)Standard Test Method for Analysis of Stainless and Alloy Steels by X-ray Fluorescence Spectrometry
Standard Test Method for Analysis of Stainless and Alloy Steels by X-ray Fluorescence Spectrometry
SCOPE
1.1 This test method covers the analysis of stainless and alloy steels by wavelength dispersive X-ray Fluorescence Spectrometry for the determination of the following elements:Note 1
Unless exceptions are noted, concentration ranges can be extended by the use of suitable reference materials.
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. Specific precautionary statements are given in Section 10.
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Designation:E572–02a(Reapproved 2006)
Standard Test Method for
Analysis of Stainless and Alloy Steels by X-ray
Fluorescence Spectrometry
This standard is issued under the fixed designation E 572; 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.
e NOTE—Updated Section 2 Reference Documents in December 2006.
1. Scope chemical Analytical Curves
2 E 691 Practice for Conducting an Interlaboratory Study to
1.1 This test method covers the analysis of stainless and
Determine the Precision of a Test Method
alloy steels by wavelength dispersive X-ray Fluorescence
E 1361 Guide for Correction of Interelement Effects in
Spectrometry for the determination of the following elements:
X-Ray Spectrometric Analysis
Element Range %
E 1601 Practice for Conducting an Interlaboratory Study to
Chromium 2.0 to 25.0
Cobalt 0.03 to 0.40
Evaluate the Performance of an Analytical Method
Copper 0.05 to 3.50
E 1621 Guide for X-Ray Emission Spectrometric Analysis
Manganese 0.3 to 5.0
E 1806 Practice for Sampling Steel and Iron for Determi-
Molybdenum 0.15 to 3.5
Nickel 0.20 to 35.0
nation of Chemical Composition
Niobium 0.05 to 1.3
Phosphorus 0.01 to 0.03
3. Terminology
Silicon 0.05 to 0.20
Sulfur 0.02 to 0.30
3.1 For definitions of terms used in this test method, refer to
Titanium 0.002 to 0.04
Terminology E 135.
Vanadium 0.03 to 0.25
NOTE 1—Unless exceptions are noted, concentration ranges can be
4. Summary of Test Method
extended by the use of suitable reference materials.
4.1 The test specimen is finished to a clean, uniform surface
1.2 This standard does not purport to address all of the
and then irradiated with an X-ray beam of high energy. The
safety concerns, if any, associated with its use. It is the
secondary X-rays produced are dispersed by means of crystals
responsibility of the user of this standard to establish appro-
and the intensities are measured by suitable detectors at
priate safety and health practices and determine the applica-
selected wavelengths. The outputs of the detectors in voltage
bility of regulatory limitations prior to use. Specific precau-
pulsesarecounted.Radiationmeasurementsaremadebasedon
tionary statements are given in Section 10.
the time required to reach a fixed number of counts, or on the
total counts obtained for a fixed time (generally expressed in
2. Referenced Documents
counts per unit time). Concentrations of the elements are
2.1 ASTM Standards:
determined by relating the measured radiation of unknown
E 135 Terminology Relating to Analytical Chemistry for
specimenstoanalyticalcurvespreparedwithsuitablereference
Metals, Ores, and Related Materials
materials.Afixed-channel, polychromator system or a sequen-
E 305 Practice for Establishing and Controlling Spectro-
tial, monochromator can be used for measurement of the
elements.
This test method is under the jurisdiction of ASTM Committee E01 on 5. Significance and Use
Analytical Chemistry for Metals, Ores and Related Materials and is the direct
5.1 Thisprocedureissuitableformanufacturingcontroland
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
for verifying that the product meets specifications. It provides
Current edition approved Nov. 1, 2006. Published November 2006. Originally
approved in 1976. Last previous edition approved in 2002 as E 572 – 02a.
rapid, multi-element determinations with sufficient accuracy to
Supporting data for this test method as determined by cooperative testing have
assure product quality. The analytical performance data in-
been filed at ASTM International Headquarters as RR: E-1-1032.
cluded may be used as a benchmark to determine if similar
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
Withdrawn.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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E572–02a (2006)
X-ray spectrometers provide equivalent precision and accu- 8. Reagents and Materials
racy, or if the performance of a particular spectrometer has
8.1 Detector Gas (P-10), consisting of a mixture of 90 %
changed.
argon and 10 % methane, for use with gas-flow proportional
counters only.
6. Interferences
6.1 Interelement effects or matrix effects exist for some of
9. Reference Materials
the elements listed. Mathematical correction may be used to
9.1 Certified Reference Materials are available from na-
solve for these elements. Various mathematical correction
tional and international sources.
procedures are commonly utilized. See Guides E 1361 and
9.2 Reference Materials with matrices similar to that of the
E 1621. Any of these procedures that achieves analytical
test specimen and containing varying amounts of the elements
accuracy equivalent to that provided by this test method is
to be determined may be used provided they have been
acceptable.
analyzed in accordance with ASTM standard methods or
similar procedures established by the certifying body. These
7. Apparatus
referencematerialsshallbehomogeneousandfreeofvoidsand
7.1 Specimen Preparation Equipment:
porosity.
7.1.1 Surface Grinder or Sander With Abrasive Belts or
9.3 The reference materials shall cover the concentration
Disks, or Lathe, capable of providing a flat, uniform surface on
ranges of the elements being sought. A minimum of three
the reference materials and test specimens. Aluminum oxide
reference materials shall be used for each element. A greater
and zirconium oxide belts and discs with a grit size of between
number of calibrants may be required if the analyst chooses to
60 and 180 have been found suitable.
perform mathematical corrections for interelement effects. See
7.2 Excitation Source:
Guide E 1361.
7.2.1 X-ray Tube Power Supply, providing a constant po-
tential or rectified power of sufficient energy to produce
10. Hazards
secondary radiation of the specimen for the elements specified.
10.1 OSHA Standards for ionizing radiation shall be ob-
The generator may be equipped with a line voltage regulator
served at all X-ray emission spectrometer installations. It is
and current stabilizer.
also recommended that operating and maintenance personnel
7.2.2 X-ray Tubes, with targets of various high-purity ele-
follow the guidelines of safe operating procedures given in
ments that are capable of continuous operation at required
current handbooks and publications from National Institute of
potentials and currents and that will excite the elements to be
Standards and Technology and the U.S. Government Printing
determined.
Office , or similar handbooks on radiation safety.
7.3 Spectrometer, designed for X-ray emission analysis and
10.2 X-rayequipmentshallbeusedonlyundertheguidance
equipped with specimen holders and a specimen chamber. The
and supervision of a responsible, qualified person.
chamber shall contain a specimen spinner, and must be
10.3 Monitoring Devices, either film badges or dosimeters
equipped for vacuum or helium-flushed operation for the
may be worn by all operating and maintenance personnel.
determination of elements of atomic number 20 (calcium) or
Safety regulations shall conform to applicable local, state, and
lower.
federal regulations.
7.3.1 Analyzing Crystals, flat or curved crystals with opti-
mized capability for the diffraction of the wavelengths of
11. Preparation of Reference Materials and Test
interest.Theuseofsyntheticmultilayerstructurescanbefound
Specimens
in state–of–the–art equipment.
11.1 The analyst must choose a measurement area or
7.3.2 Collimators or Slits, for controlling the divergence of
diameter from the options built into the spectrometer. All test
the characteristic X rays. Use per the equipment manufactur-
specimens and reference materials must have a flat surface of
er’s recommendations.
greater diameter than the chosen viewed area.
7.3.3 Detectors, sealed or gas-flow proportional type, scin-
11.2 Prepare the reference materials and test specimens to
tillation counters or equivalent.
provideaclean,flatuniformsurfacetobeexposedtotheX-ray
7.3.4 Vacuum System, providing for the determination of
elements whose radiation is absorbed by air (for example,
silicon, phosphorus, and sulfur). The system shall consist of a
Federal Register,Vol36,No.105,May1971,Section1910.96oroflatestissue
vacuum pump, gage, and electrical controls to provide auto-
of Subpart G, available from Superintendent of Documents, U.S. Government
maticpumpdownoftheopticalpath,andmaintainacontrolled
PrintingOffice,Washington,DC20025;or National Bureau of Standards Handbook
pressure, usually 13 Pa (100 :m Hg) or less, controlled to 63
111, ANSI N43.2-1971.
Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,
Pa (620 :m Hg). A helium-flushed system is an alternative to
Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098, http://
a vacuum system.
www.dodssp.daps.mil.
7.4 Measuring System, consisting of electronic circuits ca- 7
Available from U.S. Department of Health, Education, and Welfare, Rockville,
pable of amplifying and integrating pulses received from the
MD 20850.
The sole source of supply of the apparatus known to the committee at this time
detectors. For some measurements, a pulse height selector in
is available from Seimens Gammasonics, Inc., 2000 Nuclear Drive, Des Plaines, IL
conjunctionwiththedetectorsmayberequiredtoprovidemore
60018. If you are aware of alternative suppliers, please provide this information to
accurate measurements. The system shall be equipped with an
ASTM International Headquarters. Your comments will receive careful consider-
appropriate device. ation at a meeting of the responsible technical committee, which you may attend.
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E572–02a (2006)
beam. One surface of a reference material may be designated reference materials that cover the required concentration
by the producer as the certified surface. The same surface ranges. Use at least three reference materials for each element.
preparation medium shall be used for all reference materials Prepare an analytical curve for each element being determined
and test specimens. (refer to Practice E 305). For information on correction of
11.3 Refinish the surface of the reference materials and test interelement effects in X-ray Spectrometric Analysis refer to
specimens as needed to eliminate oxidation. Guide E 1361. Information on correction of spectral line
overlap in wavelength dispersive X-ray spectrometry can be
12. Preparation of Apparatus
found in Practice E 1621.
12.1 Prepare and operate the spectrometer in accordance
13.2 Standardization (Analytical Curve Adjustment)—
with the manufacturer’s instructions.
Using a control reference material, check the calibration of the
X-rayspectrometeratafrequencyconsistentwithSPCpractice
NOTE 2—It is not within the scope of this test method to prescribe
minute details relative to the preparation of the apparatus. For a descrip- or when the detector gas or major components have been
tion and specific details concerning the operation of a particular spectrom-
changed. If the calibration check indicates that the spectrom-
eter, refer to the manufacturer’s manual.
eter has drifted, make appropriate adjustments according to the
12.1.1 Start-up—Turn on the power supply and electronic instructions in the manufacturer’s manual. Refer to Practice
circuits and allow sufficient time for instrument warm-up prior E 305 for frequency of verification of standardization.
to taking measurements.
14. Procedure
12.2 Tube Power Supply—The power supply conditions
14.1 Specimen Loading—Place the reference materials and
should be set according to the manufacturers recommenda-
tions. test specimens in the appropriate specimen holding container.
If the spectrometer is equipped with an automated loading
12.2.1 The voltage and current established as optimum for
the X-ray tube power supply in an individual laboratory shall device, repeatability may be improved by loading and unload-
ing all specimens from the same holder. The container shall
be reproduced for subsequent measurements.
12.3 Proportional Counter Gas Flow—When a gas-flow have a suitable opening to achieve the required precision in an
acceptable amount of time. The holder must be equipped to
proportional counter is used, adjust the flow of the P-10 gas in
accordance with the equipment manufacturer’s instructions. keep the specimen from moving inside the holder.
14.2 Excitation—Expose the specimen to primary X radia-
When changing P-10 tanks, the detectors should be adequately
flushed with detector gas before the instrument is used. After tion in accordance with Section 12.
14.3 Radiation Measurements—Obtain and record the
changing P-10 tanks, check pulse height selector according to
the manufacturer’s instructions. countingratemeasurementforeachelement.Eitherfixedcount
12.4 Measurement Conditions—The K–L (Ka) lines for or fixed time modes may be used. Obtain at least the prede-
2,3
each element are used. When using a scanning (sequential) termined minimum counts for all specimens.
spectrometer, locations shall be calibrated according to the 14.4 Spectral Interferences—Some X-ray spectrometers
manufacturer’s guidelines. will not completely resolve radiation from several metal
12.4.1 Crystals and Detectors—The following crystals and combinations (for example, molybdenum and sulfur; molyb-
denum and phosphorus; and iron and cobalt). Therefore, care
detectors are used for the elements indicated:
must be exercised in the interpretation of intensities when both
Element Crystal Detector
Chromium L1, L2 SP, Sc, FP
elements are present. Mathematical calculations must be used
Cobalt L1, L2 SP, Sc, FP
to correct for the interferences.
Copper L1, L2 SP, Sc, FP
14.5 Replicate Measurements—Make a single measurement
Manganese L1, L2 SP, Sc, FP
Molybdenum L1, L2 Sc
on each test specimen.The performance of an X-ray spectrom-
Nickel L1, L2 SP, Sc, FP
eter is not improved significantly by making multiple measure-
Niobium L1, L2 Sc
ments on the same surface of the specimen. Confidence in the
Phosphorus Ge FP, SP
Silicon PET, InSb Fb, SP
accuracy of analysis will improve by making multiple mea-
Sulfur Ge FP, SP
surements on freshly prepared surfaces of the same specimen.
Titanium L1, L2 SP, Sc, FP
Vanadium L1, L2 SP, Sc, FP
15. Calculation of Results
L1 = LiF(200),
L2 = LiF(220),
15.1 Usingtheradiationmeasurementsforthetestspeci
...
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