ASTM C1456-13(2018)
(Test Method)Standard Test Method for Determination of Uranium or Gadolinium (or both) in Gadolinium Oxide-Uranium Oxide Pellets or by X-Ray Fluorescence (XRF)
Standard Test Method for Determination of Uranium or Gadolinium (or both) in Gadolinium Oxide-Uranium Oxide Pellets or by X-Ray Fluorescence (XRF)
SIGNIFICANCE AND USE
5.1 This test method is applicable to samples containing 1 to 10 % gadolinium oxide and 90 to 99 % uranium oxide on the “as received” basis. The method may be used to determine concentration of either uranium, gadolinium, or both.
5.2 Either wavelength-dispersive or energy-dispersive X-ray fluorescence systems may be used provided the software accompanying the system is able to accommodate the use of internal standards.
SCOPE
1.1 This test method describes the steps necessary for the preparation and analysis by X-ray fluorescence (XRF) of gadolinium or uranium (or both) in gadolinium oxide-uranium oxide pellets or powders.
1.2 This test method requires the use of appropriate internal standard(s). Care must be taken to ascertain that samples analyzed by this method do not contain the internal standard element(s) or that this contamination has been corrected for mathematically whenever present. Such corrections are not addressed in this test method.
1.3 This standard contains notes that are explanatory and are not part of the mandatory requirements of the standard.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautions are given in Section 8 and various notes throughout the method.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: C1456 − 13 (Reapproved 2018)
Standard Test Method for
Determination of Uranium or Gadolinium (or both) in
Gadolinium Oxide-Uranium Oxide Pellets or by X-Ray
Fluorescence (XRF)
This standard is issued under the fixed designation C1456; 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 2. Referenced Documents
1.1 This test method describes the steps necessary for the 2.1 ASTM Standards:
preparation and analysis by X-ray fluorescence (XRF) of D1193 Specification for Reagent Water
gadolinium or uranium (or both) in gadolinium oxide-uranium E135 Terminology Relating to Analytical Chemistry for
oxide pellets or powders. Metals, Ores, and Related Materials
2.2 Other Document
1.2 This test method requires the use of appropriate internal
ANSI/HPS N43.2-2001 Radiation Safety for X-ray Diffrac-
standard(s). Care must be taken to ascertain that samples
tion and X-ray Fluorescence Analysis Equipment
analyzed by this method do not contain the internal standard
element(s) or that this contamination has been corrected for
3. Terminology
mathematically whenever present. Such corrections are not
3.1 Definitions—For definitions of terms used in this guide,
addressed in this test method.
see Terminology E135.
1.3 Thisstandardcontainsnotesthatareexplanatoryandare
3.2 Symbol: LiTB = lithium tetraborate (see 7.4).
not part of the mandatory requirements of the standard.
1.4 The values stated in SI units are to be regarded as
4. Summary of Test Method
standard. No other units of measurement are included in this
4.1 Solution or pellet standards containing the equivalent of
standard.
1–10 % gadolinium oxide and 90–99 % uranium oxide and
1.5 This standard does not purport to address all of the
appropriate internal standards are placed in the sample holder
safety concerns, if any, associated with its use. It is the
of an X-ray spectrometer and exposed to an X-ray beam
responsibility of the user of this standard to establish appro-
capable of exciting the uranium and gadolinium L-α emission
priate safety, health, and environmental practices and deter-
lines and the appropriate emission line for the internal stan-
mine the applicability of regulatory limitations prior to use.
dard. The intensities generated are measured by an appropriate
Specific precautions are given in Section 8 and various notes
detector. The intensity ratio values obtained from this data are
throughout the method.
used to calibrate the X-ray analyzer.
1.6 This international standard was developed in accor-
4.2 Samples are prepared in the same manner as the
dance with internationally recognized principles on standard-
standards and analyzed using conditions and curves generated
ization established in the Decision on Principles for the
from those standards.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical NOTE1—Yttriumandstrontiumhavebeenusedsuccessfullyasinternal
standards for uranium and samarium for gadolinium. Scatter lines also
Barriers to Trade (TBT) Committee.
1 2
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Test. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Nov. 1, 2018. Published December 2018. Originally the ASTM website.
approved in 2000. Last previous edition approved in 2013 as C1456 – 13. DOI: Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
10.1520/C1456-13R18. 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1456 − 13 (2018)
have been used as internal standard lines. An explanation of internal
7.2 Purity of Water—Unless otherwise indicated, references
5, 6
standard method is found in several sources.
to water shall mean reagent water conforming to Specification
D1193.
5. Significance and Use
7.3 Gadolinium Oxide, Gd O —It is recommended that the
2 3
5.1 Thistestmethodisapplicabletosamplescontaining1to
standards be prepared using same batch as in pellets/powder.
10 % gadolinium oxide and 90 to 99 % uranium oxide on the
7.4 Lithium Tetraborate, Li B O , fusion grade.
“as received” basis. The method may be used to determine 2 4 7
concentration of either uranium, gadolinium, or both.
7.5 Nitric Acid, HNO , concentrated (70 %).
5.2 Either wavelength-dispersive or energy-dispersive
7.6 Samarium Oxide, Sm O , or other suitable internal
2 3
X-ray fluorescence systems may be used provided the software
standard for gadolinium (see Note 1).
accompanying the system is able to accommodate the use of
7.7 Uranium Oxide, U O , NBLCRM-129 (or equivalent).
3 8
internal standards.
NOTE 2—High purity UO may be used if certification of uranium
analysis is not required.
6. Apparatus
7.8 Yttrium Oxide, Y O , or other suitable internal standard
2 3
6.1 X-Ray Spectrometer—See the manufacturer’s operating
for uranium (see Note 1).
manuals for the selection of the X-ray spectrometer. The
method is valid for either energy-dispersive or wavelength-
8. Technical Precautions
dispersive systems.
8.1 XRF equipment analyzes by the interaction of ionizing
6.2 Sample Cups/Holders—Prepare liquid sample cups for
radiation with the sample. Applicable safety regulations and
the X-ray spectrometer as described by the manufacturer.
standard operating procedures must be reviewed prior to the
Vented, disposable sample cups with snap-on caps are satis-
use of such equipment. All modern XRF spectrometers are
factory for most such analyses; such cups decrease the likeli-
equipped with safety interlocks to prevent accidental penetra-
hood of contamination between samples. Sample holders for
tion of the X-ray beam by the user. Do NOT override these
fused pellets should keep any pellet chips from getting into the
interlocks without proper training (See ANSI/HPS N43.2-
moving parts of the instrument.
2001).
6.3 Window Film—Polyester, polyethylene, and polypropyl-
8.2 Instrument performance may be influenced by environ-
ene films have been used successfully as the film window for
mental factors such as heat, vibration, humidity, dust, stray
cups or holders, or both. Tests should be performed to
electronic noise and line voltage stability. These factors and
determinetheserviceabilityofanyfilmchosenbeforeinsertion
performance characteristics should be reviewed prior to use of
into the instrument.
this test method.
6.4 Solution Dispenser (optional)—The dispenser for the
internal standard solution, if used, should be capable of 9. Preparation of Apparatus
reproduciblydispensingtheinternalstandardsolutiontoalevel
9.1 Chamber Environment—The liquid standards and
of 0.1 % relative standard deviation of the volume dispensed.
samples used in this method are corrosive. Some fumes will be
emittedfromthesamplecups.Thesefumesmaybedetrimental
6.5 Muffle Furnace, 1100°C capacity.
to the spectrometer chamber. It is desirable to flush this
7. Reagents and Materials chamber with an inert gas (usually helium) before and during
analysis. Some X-ray spectrometers control the change of
7.1 Purity of Materials—Reagent grade chemicals shall be
sample chamber atmosphere (air, vacuum, helium) automati-
used in all tests. Unless otherwise indicated, it is intended that
cally through the software; in others, it must be done manually.
all reagents conform to the specifications of the Committee of
Follow the instrument manufacturer’s recommendations to
Analytical Reagents of the American Chemical Society where
achieve the inert gas environment. Allow sufficient stabiliza-
such specifications are available. Other grades may be used
tion time before analysis. Fused pellet standards and samples
provided it is first ascertained that the reagent is of sufficiently
maybeanalyzedusingeitheravacuumorheliumenvironment.
high purity to permit its use without lessening the accuracy of
Line intensities will be slightly higher using a vacuum envi-
the determination.
ronment. Warning—Care must be taken to assure that a
vacuum environment is not chosen with liquid samples. Ana-
lyze standards and samples under the same environment.
Andermann, G, and Kemp, J.W., “Scattered X-Rays as Internal Standards in
X-Ray Spectroscopy,” Analytical Chemistry, Vol 20 (8), 1958.
9.2 X-Ray Power Supply—If the power to the X-ray tube is
Bertin, E.P., Introduction to X-Ray Spectrometric Analysis, Plenum Press, New
not controlled by the instrument software, set the proper
York and London, 1978.
Tertian, R. and Claisse, F., Principles of Quantitative X-Ray Fluorescence
Analysis, Heyden and Son, London, Philadelphia and Rheine, 1982.
7 8
Reagent Chemicals, American Chemical Society Specifications, American The sole source of supply of the apparatus known to the committee at this time
Chemical Society, Washington, DC. For
...
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