ASTM E1085-95(2004)e1

Standard Test Method for X-Ray Emission Spectrometric Analysis of Low-Alloy Steels

SIGNIFICANCE AND USE
This procedure is suitable for manufacturing control and for verifying that the product meets specifications. This test method provides rapid, multielement determinations with sufficient accuracy to ensure product quality and minimize production delays. The analytical performance data 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 X-ray spectrometer has changed.
Calcium is sometimes added to steel to effect inclusion shape control in order to enhance certain mechanical properties of steel. This test method is useful for determining the residual calcium in the steel after such treatment.
Because calcium occurs primarily in inclusions, the precision of this test method is a function of the distribution of the calcium-bearing inclusions in the steel. The variation of determinations on freshly prepared surfaces will give some indication of the distribution of these inclusions.
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 3.0 Chromium0.04 to 2.5 Manganese0.04 to 2.5 Silicon 0.06 to 1.5 Molybdenum0.005 to 1.5 Copper 0.03 to 0.6 Vanadium0.012 to 0.6 Cobalt 0.03 to 0.2 Sulfur 0.009 to 0.1 Niobium 0.002 to 0.1 Phosphorus0.010 to 0.08 Calcium 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.

General Information

• Status: Historical
• Publication Date: 30-Sep-2004
• ICS: 77.040.30 - Chemical analysis of metals
• Technical Committee: E01 - Analytical Chemistry for Metals, Ores, and Related Materials
• Drafting Committee: E01.01 - Iron, Steel, and Ferroalloys

Relations

• Replaces: ASTM E1085-95(2004) - Standard Test Method for X-Ray Emission Spectrometric Analysis of Low-Alloy Steels
• Effective Date: 01-Oct-2004
• Replaced By: ASTM E1085-09 - Standard Test Method for Analysis of Low-Alloy Steels by X-Ray Fluorescence Spectrometry
• Effective Date: 01-Oct-2009
• Referred By: ASTM A751-21 - Standard Test Methods and Practices for Chemical Analysis of Steel Products
• Effective Date: 01-Oct-2004

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.
´1
Designation:E1085–95(Reapproved 2004)
Standard Test Method for
X-Ray Emission Spectrometric Analysis of Low-Alloy
Steels
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.
´ NOTE—Reference to the Research Report in Section 16 and the footnote were editorially removed in January 2009.
1. Scope X-Ray Spectrometric Analysis
E1622 Practice for Correction of Spectral Line Overlap in
1.1 This test method covers the wavelength dispersive
Wavelength-Dispersive X-Ray Spectrometry
X-ray spectrometric analysis of low-alloy steels for the follow-
ing elements:
3. Terminology
Element Concentration Range, %
3.1 For definitions of terms used in this test method, refer to
Nickel 0.04 to 3.0
Chromium 0.04 to 2.5
Terminology E135.
Manganese 0.04 to 2.5
Silicon 0.06 to 1.5
4. Summary of Test Method
Molybdenum 0.005 to 1.5
Copper 0.03 to 0.6
4.1 The test specimen is finished to a clean uniform surface
Vanadium 0.012 to 0.6
and then irradiated with an X-ray beam of high energy. The
Cobalt 0.03 to 0.2
secondary X rays produced are dispersed by means of crystals,
Sulfur 0.009 to 0.1
Niobium 0.002 to 0.1
and the intensities are measured by suitable detectors at
Phosphorus 0.010 to 0.08
selected wavelengths. Radiation measurements are made based
Calcium 0.001 to 0.007
on the time required to reach a fixed number of counts, or on
1.2 This standard does not purport to address all of the
thetotalcountsobtainedforafixedtime.Concentrationsofthe
safety concerns, if any, associated with its use. It is the
elements are determined by relating the measured radiation of
responsibility of the user of this standard to establish appro-
unknownspecimenstoanalyticalcurvespreparedwithsuitable
priate safety and health practices and determine the applica-
reference materials. Either a fixed-channel, polychromator
bility of regulatory limitations prior to use. Specific precau-
system or a sequential, monochromator system may be used to
tionary statements are given in Section 10.
providesimultaneousorsequentialdeterminationsofelements.
2. Referenced Documents
5. Significance and Use
2.1 ASTM Standards:
5.1 Thisprocedureissuitableformanufacturingcontroland
E135 Terminology Relating to Analytical Chemistry for
for verifying that the product meets specifications. This test
Metals, Ores, and Related Materials
method provides rapid, multielement determinations with suf-
E305 Practice for Establishing and Controlling Atomic
ficient accuracy to ensure product quality and minimize pro-
Emission Spectrochemical Analytical Curves
duction delays. The analytical performance data may be used
E691 Practice for Conducting an Interlaboratory Study to
as a benchmark to determine if similar X-ray spectrometers
Determine the Precision of a Test Method
provide equivalent precision and accuracy, or if the perfor-
E1361 Guide for Correction of Interelement Effects in
mance of a particular X-ray spectrometer has changed.
5.2 Calcium is sometimes added to steel to effect inclusion
shapecontrolinordertoenhancecertainmechanicalproperties
This test method is under the jurisdiction of ASTM Committee E01 on
of steel. This test method is useful for determining the residual
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
calcium in the steel after such treatment.
responsibility of Subcommittee E01.01 on Iron, Steel, and Ferroalloys.
5.2.1 Because calcium occurs primarily in inclusions, the
Current edition approved Oct. 1, 2004. Published November 2004. Originally
approved in 1987. Last previous edition approved in 2000 as E1085 – 95 (2000). precision of this test method is a function of the distribution of
DOI: 10.1520/E1085-95R04E01.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on Withdrawn. The last approved version of this historical standard is referenced
the ASTM website. on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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E1085–95 (2004)
the calcium-bearing inclusions in the steel. The variation of a controlled pressure, usually 13 Pa (100 µm Hg) or less,
determinations on freshly prepared surfaces will give some controlled to 63Pa(6 20 µm Hg).
indication of the distribution of these inclusions. 7.4 Measuring System, consisting of electronic circuits ca-
pable of amplifying and integrating pulses received from the
6. Interferences
detectors. For some measurements, pulse height analyzers may
6.1 Interelement or matrix effects may exist for some of the
be required to provide more accurate measurements. The
elementsin1.1.Mathematicalcorrectionsmaybeusedtosolve
system shall be equipped with an appropriate recording device.
for these effects. Various mathematical correction procedures
8. Reagents and Materials
are commonly utilized. See Guide E1361 and Practice E1622.
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
with this test method, exercise care not to contaminate the 9. Reference Materials
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
7.1 Specimen Preparation Equipment:
methods.These reference materials shall be homogeneous, and
7.1.1 Surface Grinder or Sander WithAbrasive Belts, Disks,
free of voids or porosity.
or Lathe, capable of providing a flat, uniform surface on the
9.3 The reference materials shall cover the concentration
reference materials and test specimens.
ranges of the elements being sought. A minimum of three
7.1.1.1 When calcium is to be determined, 240-grit,
reference materials shall be used for each element.
calcium-free silicon carbide belts or disks shall be used.
7.2 Excitation Source:
10. Hazards
7.2.1 X-Ray Tube Power Supply, providing a constant po-
10.1 Occupational Health and Safety standards for ionizing
tential or rectified power of sufficient energy to produce
radiation shall be observed at all X-ray emission spectrometer
secondary radiation of the specimen for the elements specified.
installations. It is also recommended that operating and main-
The generator may be equipped with a line voltage regulator
tenance personnel follow the guidelines of safe operating
and current stabilizer.
procedures given in current handbooks and publications from
7.2.2 X-Ray Tubes, with targets of various high-purity
6,7
the National Institute of Standards and Technology and the
elements, that are capable of continuous operation at required
U.S. Government Printing Office, or similar handbooks on
potentials and currents, and will excite the elements to be
radiation safety.
determined.
10.2 X-rayequipmentshallbeusedonlyundertheguidance
7.2.2.1 For the determination of calcium only chromium
and supervision of a responsible, qualified person.
target tubes were tested. Other targets shall be tested prior to
10.3 Monitoring Devices, either film badges or dosimeters
use.
may be worn by all operating and maintenance personnel.
7.3 Spectrometer,designedforX-rayemissionanalysis,and
Safety regulations shall conform to applicable local, state, and
equipped with specimen holders and a specimen chamber. The
federal regulations. To meet local, state, and federal radiation
chamber may contain a specimen spinner, and must be
standards,periodicradiationsurveysoftheequipmentforleaks
equipped for vacuum or helium-flushed operation for the
determination of elements of Atomic Number 20 (calcium) or
lower.
Office of Standard Reference Materials, National Institute of Standards and
7.3.1 Analyzing Crystals, flat or curved crystals with opti-
Technology (NIST), 100 Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070,
mized capability for the diffraction of the wavelengths of http://www.nist.gov.
ANSI/NBS Handbook 114, General Safety Standard for Installations Using
interest.
Non-Medical X-Ray and Sealed Gamma-Ram Sources, available from American
7.3.2 Collimator, for limiting the characteristic X rays to a
National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY
parallel bundle when flat crystals are used in the instrument.
10036, http://www.ansi.org.
NBS Handbook 76, Medical X-Ray Protection Up to Three Million Volts,
For curved crystal optics, a collimator is not necessary.
availableasNCRP33fromNCRPPublications,7910WoodmontAvenue,Suite400,
7.3.3 Detectors, sealed or gas-flow proportional-type, scin-
Bethesda, Maryland 20814-3095, http://www.ncrponline.org.
tillation counters, or equivalent. 7
ANSI N43.2-1977/NBS Handbook 111, Radiation Safety for X-Ray Diffraction
7.3.4 Vacuum System, providing for the determination of
and Fluorescence Analysis, available from American National Standards Institute
(ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.org.
elements whose radiation is absorbed by air (for example,
Moore, T. M., and McDonald, D. J., Radiation Safety Recommendations for
calcium, silicon, phosphorus, and sulfur). The system shall
X-Ray Diffraction and Spectrographic Equipment, MORP 68-14, 1968, available
consist of a vacuum pump, gage, and electrical controls to
from National Technical Information Service (NTIS), 5285 Port Royal Rd.,
provide automatic pumpdown of the optical path and maintain Springfield, VA 22161, http://www.ntis.gov.
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E1085–95 (2004)
and excessive scattered radiation shall be made by a qualified
_________
A
person using an ionization-chamber detector.The personal film
L1 = LiF(200),L2 = LiF(220),SP = SealedProportional,Sc = Scintillation,and
FP = Flow Proportional.
badge survey record, the radiation survey record, and an
12.4.2 Counting Time—Collect a sufficient number of
equipment maintenance record shall be available upon request.
counts so that the precision of the analysis will not be affected
10.4 Special precautions for operators and maintenance
by the variation in the counting statistics. A minimum of
personnel shall be posted at the equipment site.
10 000 counts is required for 1 % precision of the counting
10.5 Radiation caution signs shall be posted near the X-ray
statistics and 40 000 for 0.5 %.
equipment and at all entrances to the radiation area, consistent
with state and federal regulations.
13. Calibration and Standardization
10.6 Fail-safe “X-Ray On” warning lights shall be used on
13.1 Calibration (Preparation of Analytical Curves)—
the equipment.
Using the conditions given in Section 12, measure a series of
11. Preparation of Reference Materials and Test reference materials that cover the required concentration
ranges. Use at least three reference materials for each element.
Specimens
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
provideaclean,flatuniformsurfacetobeexposedtotheX-ray
element being determined (refer to Practice E305).
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 E305 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
minute details relative to the preparation of the apparatus. For a descrip-
14. Procedure
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
12.1.1 Start-up—Turn on the power supply and electronic
between the X-ray beam and the grinding striations is the same
circuits and allow sufficient time for instrument warm-up prior
for all measurements. This is an essential requirement if the
to taking measurements.
spectrometer is not equipped with a specimen spinner, but is
12.2 Tube Power Supply—Adjust the voltage of the power
not necessary when a spinner is used.
supply to produce optimum conditions.
14.2 Excitation—Expose the specimen to primary X radia-
12.2.1 The voltage and current established as optimum for
tion in accordance with Section 12.
the X-ray emission power supply in an individual laboratory
14.3 Radiation Measurements—Obtain and record the
shall be reproduced for subsequent measurements.
countingratemeasurementforeachelement.Eitherfixedcount
12.3 Proportional Counter Gas Flow— When a gas-flow
or fixed time modes may be used. Obtain at least the prede-
proportional counter is used, adjust flow of the P-10 gas in
termined minimum counts for all specimens.
accordance with the equipment manufacturer’s instructions.
14.4 Spectral Interferences—Some X-ray spectrometers
When changing P-10 tanks, the detectors should be adequately
will not completely resolve radiation from several elemental
flushed with detector gas and adjusted before the instrument is
combinations (for examp
...