ASTM C1343-96(2007)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
Designation:C1343–96 (Reapproved 2007)
Standard Test Method for
Determination of Low Concentrations of Uranium in Oils
and Organic Liquids by X-ray Fluorescence
This standard is issued under the fixed designation C1343; 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 C1118 Guide for Selecting Components for Wavelength-
Dispersive X-Ray Fluorescence (XRF) Systems
1.1 This test method covers the steps necessary for the
D1193 Specification for Reagent Water
preparation and analysis by X-ray fluorescence (XRF) of oils
E135 Terminology Relating to Analytical Chemistry for
and organic solutions containing uranium.
Metals, Ores, and Related Materials
1.2 The procedure is valid for those solutions containing 20
2.2 NIST Document:
to 2000 µg uranium/mL as presented to the spectrometer.
NBS Handbook 111, Radiation Safety for X-ray Diffraction
1.3 This test method requires the use of an appropriate
and X-ray Fluorescence Analysis Equipment
internal standard. Care must be taken to ascertain that samples
analyzed by this test method do not contain the internal
3. Terminology
standardorthatthiscontamination,wheneverpresent,hasbeen
3.1 Definitions—See definitions in Terminology E135.
corrected for mathematically. Such corrections are not ad-
dressed in this procedure. Care must be taken that the internal
4. Summary of Test Method
standard and sample medium are compatible; that is, samples
4.1 Solution standards containing 20 µg uranium/mL to
must be miscible with tri-n-butyl phosphate (TBP) and must
2000 µg uranium/mL and an internal standard are placed in a
not remove the internal standard from solution.Alternatively, a
2 liquid sample holder of an X-ray spectrometer and exposed to
scatter line may be used as the internal standard.
an X-ray beam capable of exciting the uranium L-a emission
1.4 The values stated in SI units are to be regarded as the
line and the appropriate internal standard line. The intensities
standard. The values given in parentheses are for information
generated are measured by an appropriate detector. The inten-
only.
sity ratio values obtained from these data are used to calibrate
1.5 This standard does not purport to address all of the
the X-ray analyzer. Samples are prepared having a similar
safety concerns, if any, associated with its use. It is the
matrix to fit the calibration range and measured using the same
responsibility of the user of this standard to establish appro-
analytical parameters.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific precau-
NOTE 1—Yttrium, strontium, and bromine K-a and thorium L-a lines
tionary statements are given in Section 9 and Note 2. have been used successfully as internal standard lines. Explanation of the
internal standard method of analysis is outside the scope of this test
,
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2. Referenced Documents method and is found in several sources.
2.1 ASTM Standards:
5. Significance and Use
C982 Guide for Selecting Components for Energy-
5.1 This test method is applicable to organic solutions
Dispersive X-Ray Fluorescence (XRF) Systems
containing 20 to 2000 µg uranium/mL of solution presented to
the spectrometer.
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear
5.2 Either wavelength-dispersive or energy-dispersive XRF
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
systems may be used, provided that the software accompany-
Test.
ing the system is able to accommodate the use of internal
CurrenteditionapprovedJune1,2007.PublishedJuly2007.Originallyapproved
in 1996. Last previous edition approved in 2002 as C1343–96(2002). DOI: standards.
10.1520/C1343-96R07.
Andermann, G., and Kemp, J. W., “Scattered X-rays as Internal Standards in
X-ray Spectroscopy,” Analytical Chemistry , Vol 20, No. 8, 1958.
3 5
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Available from U.S. Department of Commerce, National Institute of Standards
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM and Technology, Gaithersburg, MD 20899.
Standards volume information, refer to the standard’s Document Summary page on Bertin, E. P., Introduction to X-ray Spectrometric Analysis, Plenum Press, New
the ASTM website. York and London, 1978.
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Withdrawn. The last approved version of this historical standard is referenced Tertian, R., and Claisse, F., Principles of Quantitative X-ray Fluorescence
on www.astm.org. Analysis, Heyden & Son, London, Philadelphia, and Rheine, 1982.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
C1343–96 (2007)
6. Interferences accidental penetration of the X-ray beam by the user. Do not
override these interlocks (see NBS Handbook 111).
6.1 Thistestmethodrequirestheuseofaninternalstandard.
9.2 Instrument performance may be influenced by environ-
Care must be taken that the samples analyzed by this test
mental factors such as heat, vibration, humidity, dust, stray
method do not contain the internal standard or chemicals that
electronic noise, and line voltage stability. These factors and
wouldremovetheinternalstandardfromsolution.Thesamples
performancecharacteristicsshouldbereviewedpriortotheuse
must also be miscible with TBP.
of this test method.
7. Apparatus
10. Preparation of Apparatus
7.1 X-ray Spectrometer—See Guide C982 or Guide C1118
for selection of the X-ray spectrometer. The procedure is valid
10.1 Chamber Environment—The standards and samples
for either energy-dispersive or wavelength-dispersive systems.
used in this test method are corrosive liquids. Some fumes will
7.2 Sample Cups:
be emitted from the sample cups. These fumes may be
7.2.1 Prepare liquid sample cups for the X-ray spectrometer
detrimental to the spectrometer chamber. It is desirable to flush
as described by the manufacturer. Vented, disposable sample
this chamber with an inert gas (usually helium) before and
cups with snap-on caps are satisfactory for most such analyses;
during analysis. Some X-ray spectrometers control the change
such cups decrease the likelihood of contamination of the
of sample chamber environment (air, vacuum, and helium)
samples.
automatically through the software; in others, it must be done
7.2.2 Polyester, polyethylene, and polypropylene films have
manually. Follow the instrument manufacturer’s recommenda-
been used successfully as the film window for such cups.Tests
tions to achieve the inert gas environment.
shouldbeperformedtodeterminetheserviceabilityofanyfilm
NOTE 2—Caution: Allow sufficient stabilization time before analysis.
chosen before the insertion of samples into the instrument.
Care must be taken to ensure that a vacuum environment is not chosen
7.3 Solution Dispenser (Optional)—If used, the solution
with liquid samples.
dispenser for the internal standard solution should be capable
10.2 X-ray Power Supply—If the power to the X-ray tube is
of dispensing the internal standard reproducibly to a level of
not controlled by the instrument software, set the proper
0.5 % relative standard deviation of the volume dispensed.
combination of voltage and current for the instrument in use.
8. Reagents and Materials
These settings must be ascertained by the user for his instru-
ment and choice of X-ray tube. Rhodium, gold, tungsten, and
8.1 Purity of Reagents—Reagent grade chemicals shall be
molybdenum target X-ray tubes have been used successfully
used in all tests. Unless otherwise indicated, it is intended that
for this analysis. Allow sufficient stabilization time prior to
all reagents conform to the specifications of the Committee on
analysis.
Analytical Reagents of the American Chemical Society where
such specifications are available. Other grades may be used,
11. Calibration and Standardization
provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of
11.1 Internal Standard Solution:
the determination.
11.1.1 Weigh 65.64 g of 1,3,5-tribromobenzene to the near-
8.2 Purity of Water—Unless otherwise indicated, references
est 0.1 mg. Transfer the material to a 400-mL beaker; add 200
to water shall be understood to mean reagent water in con-
mL of TBP.
formance with Specification D1193.
11.1.2 Dissolve the material in TBP; heat on a hot plate, if
8.3 Nitric Acid, HNO , concentrated (70 %).
necessary.
8.4 1,3,5-Tribromobenzene, technical grade (or substitute
11.1.3 Transfer the dissolved material to a 1000-mL volu-
for internal standard).
metric flask, and dilute to volume with TBP. (Storage of the
8.5 Tri-n-Butyl Phosphate (TBP), technical grade.
solution in an opaque container with a screw cap is recom-
8.6 Uranium Oxide,U O , NBL CRM 129, or equivalent.
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mended; see Note 5.)
11.2 “Master” Standards:
9. Technical Precautions
9.1 X-ray fluorescence equipment analyzes
...