ASTM E572-02a(2006)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
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.
1. Scope E 305 Practice for Establishing and Controlling Spectro-
2 chemical Analytical Curves
1.1 This test method covers the analysis of stainless and
E 691 Practice for Conducting an Interlaboratory Study to
alloy steels by wavelength dispersive X-ray Fluorescence
Determine the Precision of a Test Method
Spectrometry for the determination of the following elements:
E 1361 Guide for Correction of Interelement Effects in
Element Range %
X-Ray Spectrometric Analysis
Chromium 2.0 to 25.0
Cobalt 0.03 to 0.40
E 1601 Practice for Conducting an Interlaboratory Study to
Copper 0.05 to 3.50
Evaluate the Performance of an Analytical Method
Manganese 0.3 to 5.0
E 1622 Practice for Correction of Spectral Line Overlap in
Molybdenum 0.15 to 3.5
Nickel 0.20 to 35.0
Wavelength-Dispersive X-Ray Spectrometry
Niobium 0.05 to 1.3
E 1806 Practice for Sampling Steel and Iron for Determi-
Phosphorus 0.01 to 0.03
nation of Chemical Composition
Silicon 0.05 to 0.20
Sulfur 0.02 to 0.30
Titanium 0.002 to 0.04
3. Terminology
Vanadium 0.03 to 0.25
3.1 For definitions of terms used in this test method, refer to
NOTE 1—Unless exceptions are noted, concentration ranges can be
Terminology E 135.
extended by the use of suitable reference materials.
4. Summary of Test Method
1.2 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4.1 The test specimen is finished to a clean, uniform surface
responsibility of the user of this standard to establish appro-
and then irradiated with an X-ray beam of high energy. The
priate safety and health practices and determine the applica-
secondary X-rays produced are dispersed by means of crystals
bility of regulatory limitations prior to use. Specific precau-
and the intensities are measured by suitable detectors at
tionary statements are given in Section 10.
selected wavelengths. The outputs of the detectors in voltage
pulsesarecounted.Radiationmeasurementsaremadebasedon
2. Referenced Documents
the time required to reach a fixed number of counts, or on the
2.1 ASTM Standards:
total counts obtained for a fixed time (generally expressed in
E 135 Terminology Relating to Analytical Chemistry for
counts per unit time). Concentrations of the elements are
Metals, Ores, and Related Materials
determined by relating the measured radiation of unknown
specimenstoanalyticalcurvespreparedwithsuitablereference
materials.Afixed-channel, polychromator system or a sequen-
This test method is under the jurisdiction of ASTM Committee E01 on
tial, monochromator can be used for measurement of the
Analytical Chemistry for Metals, Ores and Related Materials and is the direct
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys. elements.
Current edition approved Nov. 1, 2006. Published November 2006. Originally
approved in 1976. Last previous edition approved in 2002 as E 572 – 02a.
5. Significance and Use
Supporting data for this test method as determined by cooperative testing have
5.1 Thisprocedureissuitableformanufacturingcontroland
been filed at ASTM International Headquarters as RR: E-1-1032.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or for verifying that the product meets specifications. It provides
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.
E572–02a (2006)
rapid, multi-element determinations with sufficient accuracy to conjunctionwiththedetectorsmayberequiredtoprovidemore
assure product quality. The analytical performance data in- accurate measurements. The system shall be equipped with an
cluded may be used as a benchmark to determine if similar appropriate device.
X-ray spectrometers provide equivalent precision and accu-
8. Reagents and Materials
racy, or if the performance of a particular spectrometer has
changed.
8.1 Detector Gas (P-10), consisting of a mixture of 90 %
argon and 10 % methane, for use with gas-flow proportional
6. Interferences
counters only.
6.1 Interelement effects or matrix effects exist for some of
the elements listed. Mathematical correction may be used to 9. Reference Materials
solve for these elements. Various mathematical correction
9.1 Certified Reference Materials are available from na-
procedures are commonly utilized. See Guides E 1361 and
tional and international sources.
E 1622. Any of these procedures that achieves analytical
9.2 Reference Materials with matrices similar to that of the
accuracy equivalent to that provided by this test method is
test specimen and containing varying amounts of the elements
acceptable.
to be determined may be used provided they have been
analyzed in accordance with ASTM standard methods or
7. Apparatus
similar procedures established by the certifying body. These
7.1 Specimen Preparation Equipment:
referencematerialsshallbehomogeneousandfreeofvoidsand
7.1.1 Surface Grinder or Sander With Abrasive Belts or
porosity.
Disks, or Lathe, capable of providing a flat, uniform surface on
9.3 The reference materials shall cover the concentration
the reference materials and test specimens. Aluminum oxide
ranges of the elements being sought. A minimum of three
and zirconium oxide belts and discs with a grit size of between
reference materials shall be used for each element. A greater
60 and 180 have been found suitable.
number of calibrants may be required if the analyst chooses to
7.2 Excitation Source:
perform mathematical corrections for interelement effects. See
7.2.1 X-ray Tube Power Supply, providing a constant po-
Guide E 1361.
tential or rectified power of sufficient energy to produce
secondary radiation of the specimen for the elements specified.
10. Hazards
The generator may be equipped with a line voltage regulator
10.1 OSHA Standards for ionizing radiation shall be ob-
and current stabilizer.
served at all X-ray emission spectrometer installations. It is
7.2.2 X-ray Tubes, with targets of various high-purity ele-
also recommended that operating and maintenance personnel
ments that are capable of continuous operation at required
follow the guidelines of safe operating procedures given in
potentials and currents and that will excite the elements to be
current handbooks and publications from National Institute of
determined.
Standards and Technology and the U.S. Government Printing
7.3 Spectrometer, designed for X-ray emission analysis and
Office , or similar handbooks on radiation safety.
equipped with specimen holders and a specimen chamber. The
10.2 X-rayequipmentshallbeusedonlyundertheguidance
chamber shall contain a specimen spinner, and must be
and supervision of a responsible, qualified person.
equipped for vacuum or helium-flushed operation for the
10.3 Monitoring Devices, either film badges or dosimeters
determination of elements of atomic number 20 (calcium) or
may be worn by all operating and maintenance personnel.
lower.
Safety regulations shall conform to applicable local, state, and
7.3.1 Analyzing Crystals, flat or curved crystals with opti-
federal regulations.
mized capability for the diffraction of the wavelengths of
interest.Theuseofsyntheticmultilayerstructurescanbefound
11. Preparation of Reference Materials and Test
in state–of–the–art equipment.
Specimens
7.3.2 Collimators or Slits, for controlling the divergence of
11.1 The analyst must choose a measurement area or
the characteristic X rays. Use per the equipment manufactur-
diameter from the options built into the spectrometer. All test
er’s recommendations.
7.3.3 Detectors, sealed or gas-flow proportional type, scin-
tillation counters or equivalent.
Federal Register,Vol36,No.105,May1971,Section1910.96oroflatestissue
7.3.4 Vacuum System, providing for the determination of
of Subpart G, available from Superintendent of Documents, U.S. Government
elements whose radiation is absorbed by air (for example,
PrintingOffice,Washington,DC20025;or National Bureau of Standards Handbook
silicon, phosphorus, and sulfur). The system shall consist of a
111, ANSI N43.2-1971.
Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,
vacuum pump, gage, and electrical controls to provide auto-
Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098, http://
maticpumpdownoftheopticalpath,andmaintainacontrolled
www.dodssp.daps.mil.
pressure,usually13Pa(100:mHg)orless,controlledto;3Pa 7
Available from U.S. Department of Health, Education, and Welfare, Rockville,
(;20 :m Hg). A helium-flushed system is an alternative to a
MD 20850.
The sole source of supply of the apparatus known to the committee at this time
vacuum system.
is available from Seimens Gammasonics, Inc., 2000 Nuclear Drive, Des Plaines, IL
7.4 Measuring System, consisting of electronic circuits ca-
60018. If you are aware of alternative suppliers, please provide this information to
pable of amplifying and integrating pulses received from the
ASTM International Headquarters. Your comments will receive careful consider-
detectors. For some measurements, a pulse height selector in ation at a meeting of the responsible technical committee, which you may attend.
E572–02a (2006)
specimens and reference materials must have a flat surface of 10 000 counts is required for one percent precision of the
greater diameter than the chosen viewed area. counting statistics, 40 000 for one-half percent.
11.2 Prepare the reference materials and test specimens to
13. Calibration and Standardization
provideaclean,flatuniformsurfacetobeexposedtotheX-ray
beam. One surface of a reference material may be designated
13.1 Calibration (Preparation of Analytical Curves)—
by the producer as the certified surface. The same surface
Using the conditions given in Section 12, measure a series of
preparation medium shall be used for all reference materials
reference materials that cover the required concentration
and test specimens.
ranges. Use at least three reference materials for each element.
11.3 Refinish the surface of the reference materials and test
Prepare an analytical curve for each element being determined
specimens as needed to eliminate oxidation.
(refer to Practice E 305). For information on correction of
interelement effects in X-ray Spectrometric Analysis refer to
12. Preparation of Apparatus
Guide E 1361. Information on correction of spectral line
overlap in wavelength dispersive X-ray spectrometry can be
12.1 Prepare and operate the spectrometer in accordance
found in Practice E 1622.
with the manufacturer’s instructions.
13.2 Standardization (Analytical Curve Adjustment)—
NOTE 2—It is not within the scope of this test method to prescribe
Using a control reference material, check the calibration of the
minute details relative to the preparation of the apparatus. For a descrip-
X-rayspectrometeratafrequencyconsistentwithSPCpractice
tion and specific details concerning the operation of a particular spectrom-
or when the detector gas or major components have been
eter, refer to the manufacturer’s manual.
changed. If the calibration check indicates that the spectrom-
12.1.1 Start-up—Turn on the power supply and electronic
eter has drifted, make appropriate adjustments according to the
circuits and allow sufficient time for instrument warm-up prior
instructions in the manufacturer’s manual. Refer to Practice
to taking measurements.
E 305 for frequency of verification of standardization.
12.2 Tube Power Supply—The power supply conditions
should be set according to the manufacturers recommenda-
14. Procedure
tions.
14.1 Specimen Loading—Place the reference materials and
12.2.1 The voltage and current established as optimum for
test specimens in the appropriate specimen holding container.
the X-ray tube power supply in an individual laboratory shall
If the spectrometer is equipped with an automated loading
be reproduced for subsequent measurements.
device, repeatability may be improved by loading and unload-
12.3 Proportional Counter Gas Flow—When a gas-flow
ing all specimens from the same holder. The container shall
proportional counter is used, adjust the flow of the P-10 gas in
have a suitable opening to achieve the required precision in an
accordance with the equipment manufacturer’s instructions.
acceptable amount of time. The holder must be equipped to
When changing P-10 tanks, the detectors should be adequately
keep the specimen from moving inside the holder.
flushed with detector gas before the instrument is used. After
14.2 Excitation—Expose the specimen to primary X radia-
changing P-10 tanks, check pulse height selector according to
tion in accordance with Section 12.
the manufacturer’s instructions.
14.3 Radiation Measurements—Obtain and record the
12.4 Measurement Conditions—The K–L (Ka) lines for countingratemeasurementforeachelement.Eitherfixedcount
2,3
each element are used. When using a scanning (sequential)
or fixed time modes may be used. Obtain at least the prede-
spectrometer, locations shall be calibrated according to the termined minimum counts for all specimens.
manufacturer’s guidelines.
14.4 Spectral Interferences—Some X-ray spectrometers
will not completely resolve radiation from several metal
12.4.1 Crystals and Detectors—The following crystals and
detectors are used for the elements indicated: combinations (for example, molybdenum and sulfur; molyb-
denum and phosphorus; and iron and cobalt). Therefore, care
Element Crystal Detector
Chromium L1, L2 SP, Sc, FP
must be exercised in the interpretation of intensities when both
Cobalt L1, L2 SP, Sc, FP
elements are present. Mathematical calculations must be used
Copper L1, L2 SP, Sc, FP
to correct for the interferences.
Manganese L1, L2 SP, Sc, FP
Molybdenum L1, L2 Sc
14.5 Replicate Measurements—Make a single measurement
Nickel L1, L2 SP, Sc, FP
on each test specimen.The performance of an X-ray spectrom-
Niobium L1, L2 Sc
eter is not improved significantly by making multiple measure-
Phosphorus Ge FP, SP
Silicon PET, InSb Fb, SP
ments on the same surface of the specimen. Confidence in the
Sulfur Ge FP, SP
accuracy of analysis will improve by making multiple mea-
...