ASTM E2465-06
(Test Method)Standard Test Method for Analysis of Ni-Base Alloys by X-ray Fluorescence Spectrometry
Standard Test Method for Analysis of Ni-Base Alloys by X-ray Fluorescence Spectrometry
SCOPE
1.1 This test method covers the analysis of Ni-base alloys 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. Once these element ranges are extended they must be verified by some experimental means. This could include but not limited to Gage Repeatability and Reproducibility studies and/or Inter-laboratory Round Robin studies. Once these studies are completed, they will satisfy the ISO 17025 requirements for capability.
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 to determine the applicability of regulatory limitations prior to use.
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Designation: E2465 – 06
Standard Test Method for
Analysis of Ni-Base Alloys by X-ray Fluorescence
Spectrometry
This standard is issued under the fixed designation E2465; 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.
1. Scope E1361 Guide for Correction of Interelement Effects in
X-Ray Spectrometric Analysis
1.1 This test method covers the analysis of Ni-base alloys
E1601 Practice for Conducting an Interlaboratory Study to
bywavelengthdispersiveX-rayFluorescenceSpectrometryfor
Evaluate the Performance of an Analytical Method
the determination of the following elements:
E1622 Practice for Correction of Spectral Line Overlap in
Element Concentration Range
Wavelength-Dispersive X-Ray Spectrometry
Manganese 0.17 to 1.6 %
Phosphorus 0.005 to 0.015 %
2.2 Other Documents:
Silicon 0.02 to 0.6 %
ISO 17025 General requirements for the competence of
Chromium 11 to 22 %
testing and calibration laboratories
Nickel 31 to 77 %
Aluminum 0.12 to 1.3 %
Molybdenum 0.045 to 10 %
3. Terminology
Copper 0.014 to 2.5 %
3.1 Definitions: For definitions of terms used in this test
Titanium 0.20 to 3.0 %
Niobium 1.43 to 5.3 %
method, refer to Terminology E135.
Iron 2 to 46 %
Tungsten 0.016 to 0.50 %
4. Summary of Test Method
Cobalt 0.014 to 0.35 %
4.1 Thetestspecimenisfinishedtoaclean,uniformsurface,
NOTE 1—Unless exceptions are noted, concentration ranges can be
then irradiated with an X-ray beam of high energy. The
extended by the use of suitable reference materials. Once these element
secondary X-rays produced are dispersed by means of crystals
ranges are extended they must be verified by some experimental means.
This could include but not limited to Gage Repeatability and Reproduc- and the intensities are measured by suitable detectors at
ibility studies and/or Inter-laboratory Round Robin studies. Once these
selected wavelengths. The outputs of the detectors in voltage
studies are completed, they will satisfy the ISO 17025 requirements for
pulsesarecounted.Radiationmeasurementsaremadebasedon
capability.
the time required to reach a fixed number of counts, or on the
1.2 This standard does not purport to address all of the total counts obtained for a fixed time (generally expressed in
safety concerns, if any, associated with its use. It is the
counts per unit time). Concentrations of the elements are
responsibility of the user of this standard to establish appro- determined by relating the measured radiation of unknown
priate safety and health practices and to determine the
specimenstoanalyticalcurvespreparedwithsuitablereference
applicability of regulatory limitations prior to use. materials.Afixed-channel, polychromator system or a sequen-
tial, monochromator can be used for measurement of the
2. Referenced Documents
elements.
2.1 ASTM Standards:
5. Significance and Use
E135 Terminology Relating to Analytical Chemistry for
Metals, Ores, and Related Materials
5.1 Thisprocedureissuitableformanufacturingcontroland
E305 Practice for Establishing and Controlling Atomic
for verifying that the product meets specifications. It provides
Emission Spectrochemical Analytical Curves
rapid, multi-element determinations with sufficient accuracy to
assure product quality. The analytical performance data in-
cluded may be used as a benchmark to determine if similar
This test method is under the jurisdiction of ASTM Committee E01 on
X-ray spectrometers provide equivalent precision and accu-
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
responsibility of Subcommittee E01.08 on Ni and Co and HighTemperatureAlloys. racy, or if the performance of a particular spectrometer has
Current edition approved May 15, 2006. Published June 2006. DOI: 10.1520/
changed.
E2465-06.
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 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.
E2465 – 06
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 Guide E1361 and
9. Reference Materials
Practice E1622.Any of these procedures that achieves analyti-
9.1 Certified Reference Materials are available from na-
cal accuracy equivalent to that provided by this test method is
tional metrology institutes, international research institutes,
acceptable.
and commercial sources.
9.2 Reference Materials with matrices similar to that of the
7. Apparatus
test specimens and containing varying amounts of the elements
7.1 Specimen Preparation Equipment:
in the scope of this test method may be used provided they
7.1.1 Surface Grinder or Sander With Abrasive Belts or
have been analyzed using validated standard methods of test.
Disks, or Lathe, capable of providing a flat, uniform surface on These reference materials shall be homogeneous and free of
the reference materials and test specimens. Aluminum oxide
voids and porosity.
and zirconium oxide belts and discs with a grit size of between 9.3 The reference materials shall cover the concentration
60 and 180 have been found suitable. ranges of the elements being sought. A minimum of three
reference materials shall be used for each element. A greater
7.2 Excitation Source:
number of calibrants may be required if the analyst chooses to
7.2.1 Tube Power Supply, providing a constant potential or
perform mathematical corrections for interelement effects. See
rectified power of sufficient energy to produce secondary
Guide E1361.
radiation of the specimen for the elements specified. The
generator may be equipped with a line voltage regulator and
10. Hazards
current stabilizer.
10.1 OSHA Standards for ionizing radiation shall be ob-
7.2.2 X-ray Tubes, with targets of various high-purity ele-
served at all X-ray emission spectrometer installations. It is
ments that are capable of continuous operation at required
also recommended that operating and maintenance personnel
potentials and currents and that will excite the elements to be
follow the guidelines of safe operating procedures given in
determined.
current handbooks and publications from National Institute of
7.3 Spectrometer, designed for X-ray emission analysis and
Standards and Technology and the U.S. Government Printing
equipped with specimen holders and a specimen chamber. The
Office, or similar handbooks on radiation safety.
chamber shall contain a specimen spinner, and must be
10.2 X-rayequipmentshallbeusedonlyundertheguidance
equipped for vacuum or helium-flushed operation for the
and supervision of a responsible, qualified person.
determination of elements of atomic number 20 (calcium) or 10.3 Monitoring Devices, either film badges or dosimeters
lower.
may be worn by all operating and maintenance personnel.
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. The use of synthetic multilayer structures can also be
11. Preparation of Reference Materials and Test
found in some 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.
specimens and reference materials must have a flat surface of
7.3.3 Detectors, sealed or gas-flow proportional type, scin-
greater diameter than the chosen viewed area.
tillation counters or equivalent.
11.2 Prepare the reference materials and test specimens to
7.3.4 Vacuum System, providing for the determination of
provideaclean,flatuniformsurfacetobeexposedtotheX-ray
elements whose radiation is absorbed by air (for example,
beam. One surface of a reference material may be designated
silicon, phosphorus, and sulfur). The system shall consist of a
by the producer as the certified surface. The same preparation
vacuum pump, gage, and electrical controls to provide auto-
medium shall be used for all reference materials and test
maticpumpdownoftheopticalpath,andmaintainacontrolled
specimens.
pressure, usually 13Pa (100 mm Hg) or less, controlled to 63
11.3 Refinish the surface of the reference materials and test
Pa (20 mm Hg).Ahelium-flushed system is an alternative to a
specimens as needed to eliminate oxidation.
vacuum system.
7.4 Measuring System, consisting of electronic circuits ca-
pable of amplifying and integrating pulses received from the
Federal Register, Vol. 36, No. 105, May 1971, Section 1910.96 or of latest
issue of Subpart G, or National Bureau of Standards Handbook 111, ANSI
detectors. For some measurements, a pulse height selector in
N43.2-1971, available from Superintendent of Documents, U.S.Government Print-
conjunction with the detectors may be used to remove high
ing Office, Washington DC 20025.
order lines and background.The system shall be equipped with 5
Available from Siemens Gammasonics, Inc., 2000 Nuclear Drive, Des Plaines
an appropriate device. Il 60018.
E2465 – 06
12. Preparation of Apparatus overlap in wavelength dispersive X-ray spectrometry can be
found in Practice E1622.
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
NOTE 2—It is not within the scope of this test method to prescribe
X-rayspectrometeratafrequencyconsistentwithSPCpractice
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 manufacturers’ manual. Refer to Practice
circuits and allow sufficient time for instrument warm-up prior
E305 for frequency of verification of standardization.
to taking measurements.
12.2 Tube Power Supply—The power supply conditions
14. Procedure
should be set according to the manufacturer’s recommenda-
14.1 Specimen Loading—Place the reference materials and
tions.
test specimens in the appropriate specimen holding container.
12.2.1 The voltage and current established as optimum for
If the spectrometer is equipped with an automated loading
the X-ray tube power supply in an individual laboratory shall
device, loading and unloading all specimens from the same
be reproduced for subsequent measurements.
holder may improve repeatability. The container shall have a
12.3 Proportional Counter Gas Flow—When a gas-flow
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
tion in accordance with Section 12.
changing P-10 tanks, check the pulse height selector according
14.3 Radiation Measurements—Obtain and record the
to the manufacturer’s instructions.
countingratemeasurementforeachelement.Eitherfixedcount
12.4 Measurement Conditions—The K-L (Ka) lines for
2,3
or fixed time modes may be used. Obtain at least the prede-
each element are used. When using a sequential spectrometer,
termined minimum counts for all specimens.
measurement angles shall be calibrated according to the
14.4 Spectral Interferences—Some X-ray spectrometers
manufacturer’s guidelines.
will not completely resolve radiation from several element
12.4.1 Crystals and Detectors—The following crystals and
combinations (for example, molybdenum and sulfur; molyb-
detectors are used for the elements indicated:
denum and phosphorus, and iron and cobalt). Therefore care
Element Crystal Detector
must be exercised in the interpretation of intensities when both
Chromium L1,L2 SP,Sc,FP
elements are present. Mathematical calculations must be used
Cobalt L1,L2 SP,Sc,FP
to correct for interferences.
Copper L1,L2 SP,Sc,FP
Manganese L1,L2 SP,Sc,FP
14.5 Replicate Measurements—Make a single measurement
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
Phosphorus Ge FP,SP
ments on the same surface of the specimen. Confidence in the
Silicon PET,InSb FP,SP
accuracy of analysis will improve by making multiple mea-
Titanium L1,L2 SP,Sc,FP
surements on freshly prepared surfaces of the same specimen.
Aluminum PET Sc,FP
Iron L1,L2 SP,Sc
Tungsten L1,L2 SP,Sc
15. Calculation of Results
L1 = LiF200 SP = Sealed Proportional
15.1 Usingtheradiationmeasurementsforthetestspecimen
L2 = LiF220 Sc = Scintillation
FP = Flow Proportional and the appropriate analytical curves, determine the concen-
trations of the various elements.
12.4.2 Counting Time—Collect a sufficient number of
15.1.1 If mathematical calculations must be made to correct
counts so that the precision of the analysis will not be affected
the concentrations for interelement effects, any of a number of
by the variation in the counting statistics. A minimum of
correction procedures may be employed. Refer to the equip-
10,000 counts is required for one percent precision of the
ment manufacturer’s manual for the recommended procedure
counting statistics, 40,000 for one-half percent.
for the instrument being used. See Guide E1361.
13. Calibration and Standardization
16. Precision and Bias
13.1 Calibration (Preparation of Analytical Curves)—
16.1 Precision—An acc
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