ASTM C1456-00

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:C1456–00
Standard Test Method for
the 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 C 1456; 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 4. Summary of Test Method
1.1 This standard describes the steps necessary for the 4.1 Solution or pellet standards containing the equivalent of
preparation and analysis by X-ray fluorescence (XRF) of 1–10 % gadolinium oxide and 90–99 % uranium oxide and
gadolinium and/or uranium in gadolinium oxide-uranium ox- appropriate internal standards are placed in the sample holder
ide pellets or powders. of a x-ray spectrometer and exposed to an x-ray beam capable
1.2 This method requires the use of appropriate internal of exciting the uranium and gadolinium L-a emission lines and
standard(s). Care must be taken to ascertain that samples the appropriate emission line for the internal standard. The
analyzed by this method do not contain the internal standard intensities generated are measured by an appropriate detector.
element(s) or that this contamination has been corrected for The intensity ratio values obtained from this data are used to
mathematically whenever present. Such corrections are not calibrate the x-ray analyzer.
addressed in this standard. 4.2 Samples are prepared in the same manner as the
1.3 This standard does not purport to address all of the standards and analyzed using conditions and curves generated
safety concerns, if any, associated with its use. It is the from those standards.
responsibility of the user of this standard to establish appro-
NOTE 1—Yttriumandstrontiumhavebeenusedsuccessfullyasinternal
priate safety and health practices and determine the applica-
standards for uranium and samarium for gadolinium. Scatter lines also
bility of regulatory limitations prior to use. Specific precau-
have been used as internal standard lines (1). An explanation of internal
tions are given in Section 8 and various notes throughout the standard method is found in several sources (2, 3).
method.
5. Significance and Use
2. Referenced Documents
5.1 Thisguideisapplicabletosamplescontaining2to10 %
2.1 ASTM Standards: gadolinium oxide and 90 to 98 % uranium oxide on the “as
C 982 Guide for Selecting Components for Generic Energy received” basis. The method may be used to determine
Dispersive X-Ray Fluorescence (XRF) Systems concentration of either uranium, gadolinium, or both.
C 1118 Guide for Selecting Components for Wavelength- 5.2 Either wavelength-dispersive or energy-dispersive x-ray
Dispersive X-Ray Fluorescence (XRF) Systems fluorescence systems may be used provided the software
D 1193 Specification for Reagent Water accompanying the system is able to accommodate the use of
E 135 Terminology Relating to Analytical Chemistry for internal standards.
Metals, Ores, and Related Materials
6. Apparatus
3. Terminology
6.1 X-Ray Spectrometer—See Guide C 982 or Guide
3.1 Definitions—For definitions of terms used in this guide, C 1118fortheselectionoftheX-rayspectrometer.Themethod
see Terminology E 135. is valid for either energy-dispersive or wavelength-dispersive
3.2 Symbol: systems.
LiTB 5 lithium tetraborate (see 7.4). 6.2 Sample Cups/Holders—Prepare liquid sample cups for
the x-ray spectrometer as described by the manufacturer.
Vented, disposable sample cups with snap-on caps are satis-
This guide is under the jurisdiction ofASTM Committee C-26 on Nuclear Fuel
factory for most such analyses. Such cups decrease the
Cycle and is the direct responsibility of Subcommittee C-26.05 on Methods of Test.
Current edition approved Feb. 10, 2000. Published March 2000.
Annual Book of ASTM Standards, Vol 12.01.
3 5
Annual Book of ASTM Standards, Vol 11.01. The boldface numbers in parentheses refer to the list of references at the end of
Annual Book of ASTM Standards, Vol 03.05. this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
C1456
likelihood of contamination between samples. Sample holders electronic noise and line voltage stability. These factors and
for fused pellets should keep any pellet chips from getting into performance characteristics should be reviewed prior to use of
the moving parts of the instrument. this standard.
6.3 Window Film—Polyester, polyethylene, and polypropy-
9. Preparation of Apparatus
lene films have been used successfully as the film window for
9.1 Chamber Environment—The liquid standards and
cups or holders, or both. Tests should be performed to
samples used in this method are corrosive. Some fumes will be
determinetheserviceabilityofanyfilmchosenbeforeinsertion
emittedfromthesamplecups.Thesefumesmaybedetrimental
into the instrument.
to the spectrometer chamber. It is desirable to flush this
6.4 Solution Dispenser (optional)—The dispenser for the
chamber with an inert gas (usually helium) before and during
internal standard solution, if used, should be capable of
analysis. Some x-ray spectrometers control the change of
reproducibility dispensing the internal standard solution to a
sample chamber atmosphere (air, vacuum, helium) automati-
level of 0.1 % relative standard deviation of the volume
cally through the software; in others, it must be done manually.
dispensed.
Follow the instrument manufacturer’s recommendations to
6.5 Muffle Furnace, 1100°C capacity.
achieve the inert gas environment. Allow sufficient stabiliza-
tion time before analysis. Fused pellet standards and samples
7. Reagents and Materials
maybeanalyzedusingeitheravacuumorheliumenvironment.
7.1 Purity of Materials—Reagent grade chemicals shall be
Line intensities will be slightly higher using a vacuum envi-
used in all tests. Unless otherwise indicated, it is intended that
ronment.
all reagents conform to the specifications of the Committee of
NOTE 3—Caution: Care must be taken to assure that a vacuum
Analytical Reagents of the American Chemical Society where
environment is not chosen with liquid samples. Analyze standards and
such specifications are available. Other grades may be used
samples under the same environment.
provided it is first ascertained that the reagent is of sufficiently
9.2 X-Ray Power Supply—If the power to the x-ray tube is
high purity to permit its use without lessening the accuracy of
not controlled by the instrument software, set the proper
the determination.
combination of voltage and current for the instrument in use.
7.2 Purity of Water—Unless otherwise indicated, references
These settings must be determined by the user for his instru-
to water shall mean reagent water conforming to Specification
ment and choice of x-ray tube. Allow sufficient stabilization
D 1193.
time prior to analysis.
7.3 Gadolinium Oxide, Gd O —It is recommended that the
2 3
standards be prepared using same batch as in pellets/powder.
10. Calibration and Standardization
7.4 Lithium Tetraborate, Li B O , fusion grade.
2 4 7
10.1 Internal Standard Solution:
7.5 Nitric Acid, HNO , concentrated (70 %).
10.1.1 Weigh 45 g of the internal standard compound
7.6 Samarium Oxide, Sm O , or other suitable internal
2 3
chosen for uranium and5gofthe internal standard compound
standard for gadolinium (see Note 1).
chosen for gadolinium into a beaker. Cover with a minimum
7.7 Uranium Oxide, U O , NBL CRM-129 (or equivalent)
3 8
amount of water. Add concentrated nitric acid slowly.
(4).
NOTE 4—For yttrium oxide and samarium oxide, the reaction will be
NOTE 2—High purity UO may be used if certification of uranium
slow and may require heating. If strontium carbonate is used for uranium,
analysis is not required.
thereactionwillbevigorous.Thestrengthoftheinternalstandardsolution
7.8 Yttrium Oxide, Y O , or other suitable internal standard
may be changed to achieve optimum excitation with the equipment being
2 3
for uranium (see Note 1). used. The exact concentration of the internal standard solution is not
critical; however, it is critical that the internal standard solution added to
standards and samples be the same.
8. Technical Precautions
10.1.2 Heat on a hot plate if necessary to complete the
8.1 XRF equipment analyzes by the interaction of ionizing
dissolution.
radiation with the sample. Applicable safety regulations and
10.1.3 Cool the solution to room temperature, and transfer
standard operating procedures must be reviewed prior to the
to a 1000-mL volumetric flask. Filter the solution if necessary.
use of such equipment. All modern XRF spectrometers are
Dilute to volume with water and mix thoroughly.
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