ASTM E1085-95(2000)
(Test Method)Standard Test Method for X-Ray Emission Spectrometric Analysis of Low-Alloy Steels
Standard Test Method for X-Ray Emission Spectrometric Analysis of Low-Alloy Steels
SCOPE
1.1 This test method covers the wavelength dispersive X-ray spectrometric analysis of low-alloy steels for the following elements:ElementConcentration Range, %Nickel 0.04 to 3.0Chromium0.04 to 2.5Manganese0.04 to 2.5Silicon 0.06 to 1.5Molybdenum0.005 to 1.5Copper 0.03 to 0.6Vanadium0.012 to 0.6Cobalt 0.03 to 0.2Sulfur 0.009 to 0.1Niobium 0.002 to 0.1Phosphorus0.010 to 0.08Calcium 0.001 to 0.007
1.2 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:E1085–95 (Reapproved 2000)
Standard Test Method for
X-Ray Emission Spectrometric Analysis of Low-Alloy
Steels
This standard is issued under the fixed designation E 1085; 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 3. Terminology
1.1 This test method covers the wavelength dispersive 3.1 For definitions of terms used in this test method, refer to
X-ray spectrometric analysis of low-alloy steels for the follow- Terminology E 135.
ing elements:
4. Summary of Test Method
Element Concentration Range, %
Nickel 0.04 to 3.0
4.1 The test specimen is finished to a clean uniform surface
Chromium 0.04 to 2.5
and then irradiated with an X-ray beam of high energy. The
Manganese 0.04 to 2.5
secondary X rays produced are dispersed by means of crystals,
Silicon 0.06 to 1.5
Molybdenum 0.005 to 1.5
and the intensities are measured by suitable detectors at
Copper 0.03 to 0.6
selected wavelengths. Radiation measurements are made based
Vanadium 0.012 to 0.6
on the time required to reach a fixed number of counts, or on
Cobalt 0.03 to 0.2
Sulfur 0.009 to 0.1
the total counts obtained for a fixed time. Concentrations of the
Niobium 0.002 to 0.1
elements are determined by relating the measured radiation of
Phosphorus 0.010 to 0.08
unknownspecimenstoanalyticalcurvespreparedwithsuitable
Calcium 0.001 to 0.007
reference materials. Either a fixed-channel, polychromator
1.2 This standard does not purport to address all of the
system or a sequential, monochromator system may be used to
safety concerns, if any, associated with its use. It is the
providesimultaneousorsequentialdeterminationsofelements.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5. Significance and Use
bility of regulatory limitations prior to use. Specific precau-
5.1 This procedure is suitable for manufacturing control and
tionary statements are given in Section 10.
for verifying that the product meets specifications. This test
method provides rapid, multielement determinations with suf-
2. Referenced Documents
ficient accuracy to ensure product quality and minimize pro-
2.1 ASTM Standards:
duction delays. The analytical performance data may be used
E 135 Terminology Relating to Analytical Chemistry for
as a benchmark to determine if similar X-ray spectrometers
Metals, Ores, and Related Materials
provide equivalent precision and accuracy, or if the perfor-
E 305 Practice for Establishing and Controlling Spectro-
mance of a particular X-ray spectrometer has changed.
chemical Analytical Curves
5.2 Calcium is sometimes added to steel to effect inclusion
E 691 Practice for Conducting an Interlaboratory Study to
shapecontrolinordertoenhancecertainmechanicalproperties
Determine the Precision of a Test Method
of steel. This test method is useful for determining the residual
E 1361 Guide for Correction of Interelement Effects in
calcium in the steel after such treatment.
X-Ray Spectrometric Analysis
5.2.1 Because calcium occurs primarily in inclusions, the
E 1622 Practice for the Correction of Spectral Line Overlap
precision of this test method is a function of the distribution of
in Wavelength X-Ray Spectrometry
the calcium-bearing inclusions in the steel. The variation of
determinations on freshly prepared surfaces will give some
1 indication of the distribution of these inclusions.
This test method is under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry of Metals, Ores, and Related Materials and is the direct
6. Interferences
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
Current edition approved Sept. 10, 1995. Published November 1995. Originally
6.1 Interelement or matrix effects may exist for some of the
published as E 1085 – 87. Last previous edition E 1085 – 87.
elementsin1.1.Mathematicalcorrectionsmaybeusedtosolve
Annual Book of ASTM Standards, Vol 03.05.
Annual Book of ASTM Standards, Vol 14.02. for these effects. Various mathematical correction procedures
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E1085
are commonly utilized. See Guide E 1361 and Practice E 1622. 8. Reagents and Materials
Any of these procedures is acceptable that will achieve
8.1 Detector Gas (P-10), consisting of a mixture of 90 %
analytical accuracy equivalent to that provided by this test
argon and 10 % methane, for use with gas-flow proportional
method.
counters only.
6.2 Because trace amounts of calcium are being determined
9. Reference Materials
with this test method, exercise care not to contaminate the
specimen. The presence of calcium in the grinding medium
9.1 Certified Reference Materials are available from the
will contaminate the specimen to the extent that erratic and
National Institute of Standards and Technology and other
incorrect results will be obtained. Therefore, the grinding
international certification agencies.
medium shall be analyzed for calcium and only those materials
9.2 Reference Materials with matrices similar to that of the
that are free of calcium shall be used.
test specimen and containing varying amounts of the elements
to be determined may be used provided they have been
7. Apparatus
chemically analyzed in accordance with ASTM standard test
methods.These reference materials shall be homogeneous, and
7.1 Specimen Preparation Equipment:
free of voids or porosity.
7.1.1 Surface Grinder or Sander WithAbrasive Belts, Disks,
9.3 The reference materials shall cover the concentration
or Lathe, capable of providing a flat, uniform surface on the
ranges of the elements being sought. A minimum of three
reference materials and test specimens.
reference materials shall be used for each element.
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 Excitation Source:
10.1 Occupational Health and Safety standards for ionizing
7.2.1 X-Ray Tube Power Supply, providing a constant po-
radiation shall be observed at all X-ray emission spectrometer
tential or rectified power of sufficient energy to produce
installations. It is also recommended that operating and main-
secondary radiation of the specimen for the elements specified.
tenance personnel follow the guidelines of safe operating
The generator may be equipped with a line voltage regulator
procedures given in current handbooks and publications from
and current stabilizer.
6,7
the National Institute of Standards and Technology and the
7.2.2 X-Ray Tubes, with targets of various high-purity
U.S. Government Printing Office, or similar handbooks on
elements, that are capable of continuous operation at required
radiation safety.
potentials and currents, and will excite the elements to be
10.2 X-rayequipmentshallbeusedonlyundertheguidance
determined.
and supervision of a responsible, qualified person.
7.2.2.1 For the determination of calcium only chromium
10.3 Monitoring Devices, either film badges or dosimeters
target tubes were tested. Other targets shall be tested prior to
may be worn by all operating and maintenance personnel.
use.
Safety regulations shall conform to applicable local, state, and
7.3 Spectrometer, designed for X-ray emission analysis, and
federal regulations. To meet local, state, and federal radiation
equipped with specimen holders and a specimen chamber. The
standards,periodicradiationsurveysoftheequipmentforleaks
chamber may contain a specimen spinner, and must be
and excessive scattered radiation shall be made by a qualified
equipped for vacuum or helium-flushed operation for the
person using an ionization-chamber detector.The personal film
determination of elements of Atomic Number 20 (calcium) or
badge survey record, the radiation survey record, and an
lower.
equipment maintenance record shall be available upon request.
7.3.1 Analyzing Crystals, flat or curved crystals with opti-
10.4 Special precautions for operators and maintenance
mized capability for the diffraction of the wavelengths of
personnel shall be posted at the equipment site.
interest.
10.5 Radiation caution signs shall be posted near the X-ray
7.3.2 Collimator, for limiting the characteristic X rays to a
equipment and at all entrances to the radiation area, consistent
parallel bundle when flat crystals are used in the instrument.
with state and federal regulations.
For curved crystal optics, a collimator is not necessary.
10.6 Fail-safe “X-Ray On” warning lights shall be used on
7.3.3 Detectors, sealed or gas-flow proportional-type, scin-
the equipment.
tillation counters, or equivalent.
7.3.4 Vacuum System, providing for the determination of
Office of Standard Reference Materials, National Institute of Standards and
elements whose radiation is absorbed by air (for example,
Technology, U.S. Department of Commerce, Gaithersburg, MD 20899.
calcium, silicon, phosphorus, and sulfur). The system shall
ANSI/NBS Handbook 114, General Safety Standard for Installations Using
consist of a vacuum pump, gage, and electrical controls to
Non-Medical X-Ray and Sealed Gamma-Ram Sources, available from American
provide automatic pumpdown of the optical path and maintain National Standards Institute, 11 W. 42nd St., 13th Floor, New York, NY 10036.
NBS Handbook 76, Medical X-Ray Protection Up to Three Million Volts,
a controlled pressure, usually 13 Pa (100 µm Hg) or less,
available as NCRP 33 from NCRP Publications, 7910 WoodmontAve., Suite 1016,
controlled to 63Pa(620 µm Hg).
Bethesda, MD 20814.
7.4 Measuring System, consisting of electronic circuits ca-
ANSI N43.2-1977/NBS Handbook 111, Radiation Safety for X-Ray Diffraction
and Fluorescence Analysis, available from American National Standards Institute,
pable of amplifying and integrating pulses received from the
11 W. 42nd St., 13th Floor, New York, NY 10036.
detectors. For some measurements, pulse height analyzers may
Moore, T. M., and McDonald, D. J., Radiation Safety Recommendations for
be required to provide more accurate measurements. The
X-Ray Diffraction and Spectrographic Equipment, MORP 68-14, 1968, available
system shall be equipped with an appropriate recording device. from National Technical Information Service, Springfield, VA 22161.
E1085
11. Preparation of Reference Materials and Test reference materials that cover the required concentration
Specimens ranges. Use at least three reference materials for each element.
Measure the reference materials at least two different times on
11.1 Prepare the reference materials and test specimens to
each of two separate days. Prepare an analytical curve for each
provide a clean, flat uniform surface to be exposed to the X-ray
element being determined (refer to Practice E 305).
beam. For abrasive sanding, select a grit size, and use that grit
13.2 Standardization (Analytical Curve Adjustment)—
and size exclusively for all reference materials and test
Using a control reference material, check the calibration of the
specimens.
X-ray spectrometer at a frequency consistent with statistical
11.2 Refinish the surface of the reference materials and test
process control practice, or when the detector gas or major
specimens as needed to eliminate surface contamination.
components have been changed. If the calibration check
indicates that the spectrometer has drifted, make appropriate
12. Preparation of Apparatus
adjustments in accordance with the instructions in the manu-
12.1 Prepare and operate the spectrometer in accordance
facturer’s manual. Refer to Practice E 305 for frequency of
with the manufacturer’s instructions.
verification of standardization.
NOTE 1—It is not within the scope of this test method to prescribe
14. Procedure
minute details relative to the preparation of the apparatus. For a descrip-
tion and specific details concerning the operation of a particular spectrom-
14.1 Specimen Loading—Orient the reference materials and
eter, refer to the manufacturer’s manual.
testspecimensinthespecimenchambersothattherelationship
between the X-ray beam and the grinding striations is the same
12.1.1 Start-up—Turn on the power supply and electronic
circuits and allow sufficient time for instrument warm-up prior for all measurements. This is an essential requirement if the
spectrometer is not equipped with a specimen spinner, but is
to taking measurements.
12.2 Tube Power Supply—Adjust the voltage of the power not necessary when a spinner is used.
14.2 Excitation—Expose the specimen to primary X radia-
supply to produce optimum conditions.
12.2.1 The voltage and current established as optimum for tion in accordance with Section 12.
14.3 Radiation Measurements—Obtain and record the
the X-ray emission power supply in an individual laboratory
shall be reproduced for subsequent measurements. countingratemeasurementforeachelement.Eitherfixedcount
or fixed time modes may be used. Obtain at least the prede-
12.3 Proportional Counter Gas Flow— When a gas-flow
proportional counter is used, adjust flow of the P-10 gas in termined minimum counts for all specimens.
14.4 Spectral Interferences—Some X-ray spectrometers
accordance with the equipment manufacturer’s instructions.
When changing P-10 tanks, the detectors should be adequately will not completely resolve radiation from several elemental
combinations (for example, molybdenum and sulfur; molyb-
flushed with detector gas and adjusted before the instrument is
denum and phosphorus; iron and cobalt). Therefore, exercise
used.
care in the interpretation of intensities when both elements are
12.4 Measurement Conditions—The K-a lines for each
present. Use mathematical calculations to correct for such
element are used. The peak location, when using a scanning
spectrometer, should be determined for each instrument. interferences. See Practice E 1622.
14.5 Replicate Measurements—Make a single measurement
12.4.1 Crystals and Detectors—The following crystals and
detectors are used for the elements indicated: on each test specimen.The performance of an X-ray spectrom-
A A
eter is not improved significantly by making multiple measure-
Element Crystal Detector
Nickel L1, L2 SP, Sc, FP
ments on the same surface of the specimen. Confidence in the
Chromium L1, L2 SP, Sc, FP
accuracy of analysis will improve by making multiple mea-
Manganese L1, L2 SP, Sc, FP
surements on freshly prepared surfaces of the same specimen
Silicon PET, InSb FP
Molybdenum L1, L2 Sc
or by analyzing more than one specimen.
Copper L1, L2 SP, Sc, FP
Vanadium L1
...
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