ASTM E572-02a(2006)e2
(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
SIGNIFICANCE AND USE
This procedure is suitable for manufacturing control and for verifying that the product meets specifications. It provides rapid, multi-element determinations with sufficient accuracy to assure product quality. The analytical performance data included may be used as a benchmark to determine if similar X-ray spectrometers provide equivalent precision and accuracy, or if the performance of a particular spectrometer has changed.
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.
General Information
Relations
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
´2
Designation: E572 − 02a (Reapproved2006)
Standard Test Method for
Analysis of Stainless and Alloy Steels by X-ray
Fluorescence Spectrometry
This standard is issued under the fixed designation E572; 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.
´ NOTE—Updated Section 2 Reference Documents in December 2006.
´ NOTE—Made Editorial corrections to 7.3.4 in March 2007.
1. Scope Emission Spectrochemical Analytical Curves
2 E691 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
E1361 Guide for Correction of Interelement Effects in
Spectrometry for the determination of the following elements:
X-Ray Spectrometric Analysis
Element Range %
E1601 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
E1621 Guide for X-Ray Emission Spectrometric Analysis
Manganese 0.3 to 5.0
E1806 Practice for Sampling Steel and Iron for Determina-
Molybdenum 0.15 to 3.5
Nickel 0.20 to 35.0 tion 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 E135.
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
E135 Terminology Relating to Analytical Chemistry for
specimenstoanalyticalcurvespreparedwithsuitablereference
Metals, Ores, and Related Materials
materials. A fixed-channel, polychromator system or a
E305 Practice for Establishing and Controlling Atomic
sequential,monochromatorcanbeusedformeasurementofthe
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
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
5.1 Thisprocedureissuitableformanufacturingcontroland
Current edition approved Nov. 1, 2006. Published November 2006. Originally
for verifying that the product meets specifications. It provides
approved in 1976. Last previous edition approved in 2002 as E572 – 02a. DOI:
rapid, multi-element determinations with sufficient accuracy to
10.1520/E0572-02AR06E02.
assure product quality. The analytical performance data in-
Supporting data for this test method as determined by cooperative testing have
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
X-ray spectrometers provide equivalent precision and
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
accuracy,oriftheperformanceofaparticularspectrometerhas
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. changed.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´2
E572 − 02a (2006)
6. Interferences 8. Reagents and Materials
8.1 Detector Gas (P-10), consisting of a mixture of 90 %
6.1 Interelement effects or matrix effects exist for some of
argon and 10 % methane, for use with gas-flow proportional
the elements listed. Mathematical correction may be used to
counters only.
solve for these elements. Various mathematical correction
procedures are commonly utilized. See Guides E1361 and
9. Reference Materials
E1621. Any of these procedures that achieves analytical
accuracy equivalent to that provided by this test method is
9.1 Certified Reference Materials are available from na-
acceptable.
tional and international sources.
9.2 Reference Materials with matrices similar to that of the
7. Apparatus
test specimen and containing varying amounts of the elements
to be determined may be used provided they have been
7.1 Specimen Preparation Equipment:
analyzed in accordance with ASTM standard methods or
7.1.1 Surface Grinder or Sander With Abrasive Belts or
similar procedures established by the certifying body. These
Disks, or Lathe, capable of providing a flat, uniform surface on
referencematerialsshallbehomogeneousandfreeofvoidsand
the reference materials and test specimens. Aluminum oxide
porosity.
and zirconium oxide belts and discs with a grit size of between
60 and 180 have been found suitable.
9.3 The reference materials shall cover the concentration
ranges of the elements being sought. A minimum of three
7.2 Excitation Source:
reference materials shall be used for each element. A greater
7.2.1 X-ray Tube Power Supply, providing a constant poten-
number of calibrants may be required if the analyst chooses to
tialorrectifiedpowerofsufficientenergytoproducesecondary
perform mathematical corrections for interelement effects. See
radiation of the specimen for the elements specified. The
Guide E1361, E691.
generator may be equipped with a line voltage regulator and
current stabilizer.
10. Hazards
7.2.2 X-ray Tubes, with targets of various high-purity ele-
10.1 OSHA Standards for ionizing radiation shall be ob-
ments that are capable of continuous operation at required
served at all X-ray emission spectrometer installations. It is
potentials and currents and that will excite the elements to be
also recommended that operating and maintenance personnel
determined.
follow the guidelines of safe operating procedures given in
7.3 Spectrometer, designed for X-ray emission analysis and current handbooks and publications from National Institute of
equipped with specimen holders and a specimen chamber. The Standards and Technology and the U.S. Government Printing
chamber shall contain a specimen spinner, and must be Office , or similar handbooks on radiation safety.
equipped for vacuum or helium-flushed operation for the
10.2 X-rayequipmentshallbeusedonlyundertheguidance
determination of elements of atomic number 20 (calcium) or
and supervision of a responsible, qualified person.
lower.
10.3 Monitoring Devices, either film badges or dosimeters
7.3.1 Analyzing Crystals, flat or curved crystals with opti-
may be worn by all operating and maintenance personnel.
mized capability for the diffraction of the wavelengths of
Safety regulations shall conform to applicable local, state, and
interest.Theuseofsyntheticmultilayerstructurescanbefound
federal regulations.
in state–of–the–art equipment.
7.3.2 Collimators or Slits, for controlling the divergence of
11. Preparation of Reference Materials and Test
the characteristic X rays. Use per the equipment manufactur-
Specimens
er’s recommendations.
11.1 The analyst must choose a measurement area or
7.3.3 Detectors, sealed or gas-flow proportional type, scin-
diameter from the options built into the spectrometer. All test
tillation counters or equivalent.
specimens and reference materials must have a flat surface of
7.3.4 Vacuum System, providing for the determination of
greater diameter than the chosen viewed area.
elements whose radiation is absorbed by air (for example,
silicon, phosphorus, and sulfur). The system shall consist of a
vacuum pump, gage, and electrical controls to provide auto-
Federal Register,Vol36,No.105,May1971,Section1910.96oroflatestissue
maticpumpdownoftheopticalpath,andmaintainacontrolled
of Subpart G, available from Superintendent of Documents, U.S. Government
PrintingOffice,Washington,DC20025;or National Bureau of Standards Handbook
pressure, usually 13 Pa (100 µm Hg) or less, controlled to 63
111,ANSI N43.2-1971.
Pa (620 µm Hg).Ahelium-flushed system is an alternative to
Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,
a vacuum system.
Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098, http://
www.dodssp.daps.mil.
7.4 Measuring System, consisting of electronic circuits ca- 6
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.
´2
E572 − 02a (2006)
11.2 Prepare the reference materials and test specimens to 13. Calibration and Standardization
provideaclean,flatuniformsurfacetobeexposedtotheX-ray
13.1 Calibration (Preparation of Analytical Curves)—
beam. One surface of a reference material may be designated
Using the conditions given in Section 12, measure a series of
by the producer as the certified surface. The same surface
reference materials that cover the required concentration
preparation medium shall be used for all reference materials
ranges. Use at least three reference materials for each element.
and test specimens.
Prepare an analytical curve for each element being determined
11.3 Refinish the surface of the reference materials and test (refer to Practice E305). For information on correction of
specimens as needed to eliminate oxidation. interelement effects in X-ray Spectrometric Analysis refer to
Guide E1361. Information on correction of spectral line
12. Preparation of Apparatus
overlap in wavelength dispersive X-ray spectrometry can be
found in Practice E1621.
12.1 Prepare and operate the spectrometer in accordance
with the manufacturer’s instructions.
13.2 Standardization(AnalyticalCurveAdjustment)—Using
a control reference material, check the calibration of the X-ray
NOTE 2—It is not within the scope of this test method to prescribe
spectrometer at a frequency consistent with SPC practice or
minute details relative to the preparation of the apparatus. For a descrip-
tion and specific details concerning the operation of a particular when the detector gas or major components have been
spectrometer, refer to the manufacturer’s manual.
changed. If the calibration check indicates that the spectrom-
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
to taking measurements. E305 for frequency of verification of standardization.
12.2 Tube Power Supply—The power supply conditions
14. Procedure
should be set according to the manufacturers recommenda-
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-
ing all specimens from the same holder. The container shall
12.3 Proportional Counter Gas Flow—When a gas-flow
have a suitable opening to achieve the required precision in an
proportional counter is used, adjust the flow of the P-10 gas in
acceptable amount of time. The holder must be equipped to
accordance with the equipment manufacturer’s instructions.
keep the specimen from moving inside the holder.
When changing P-10 tanks, the detectors should be adequately
14.2 Excitation—Expose the specimen to primary X radia-
flushed with detector gas before the instrument is used. After
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 (Kα) lines for countingratemeasurementforeachelement.Eitherfixedcount
2,3
or fixed time modes may be used. Obtain at least the prede-
each element are used. When using a scanning (sequential)
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
12.4.1 Crystals and Detectors—The following crystals and
will not completely resolve radiation from several metal
detectors are used for the elements indicated:
combinations (for example, molybdenum and sulfur; molyb-
Element Crystal Detector
denum and phosphorus; and iron and cobalt). Therefore, care
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
Manganese L1, L2 SP, Sc, FP
to correct for the interferences.
Molybdenum L1, L2 Sc
Nickel L1, L2 SP, Sc, FP 14.5 Replicate Measurements—Make a single measurement
Niobium L1, L2 Sc
on each test specimen.The performance of an X-ray spectrom-
Phosphorus Ge FP, SP
eter is not improved significantly by making multiple measure-
Silicon PET, InSb Fb, SP
Sulfur Ge FP, SP ments on the same surface of the specimen. Confidence in the
Titanium L1, L2 SP, Sc, FP
accuracy of analysis will improve by making m
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.