ASTM C1343-96(2002)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 2002)
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 C 1343; 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 Dispersive X-Ray Fluorescence (XRF) Systems
D 1193 Specification for Reagent Water
1.1 This test method covers the steps necessary for the
E 135 Terminology Relating to Analytical Chemistry for
preparation and analysis by X-ray fluorescence (XRF) of oils
Metals, Ores, and Related Materials
and organic solutions containing uranium.
2.2 NIST Document:
1.2 The procedure is valid for those solutions containing 20
NBS Handbook 111, Radiation Safety for X-ray Diffraction
to 2000 µg uranium/mL as presented to the spectrometer.
and X-ray Fluorescence Analysis Equipment
1.3 This test method requires the use of an appropriate
internal standard. Care must be taken to ascertain that samples
3. Terminology
analyzed by this test method do not contain the internal
3.1 Definitions—See definitions in Terminology E 135.
standardorthatthiscontamination,wheneverpresent,hasbeen
corrected for mathematically. Such corrections are not ad-
4. Summary of Test Method
dressed in this procedure. Care must be taken that the internal
4.1 Solution standards containing 20 µg uranium/mL to
standard and sample medium are compatible; that is, samples
2000 µg uranium/mL and an internal standard are placed in a
must be miscible with tri-n-butyl phosphate (TBP) and must
liquid sample holder of an X-ray spectrometer and exposed to
not remove the internal standard from solution.Alternatively, a
2 an X-ray beam capable of exciting the uranium L-a emission
scatter line may be used as the internal standard.
line and the appropriate internal standard line. The intensities
1.4 The values stated in SI units are to be regarded as the
generated are measured by an appropriate detector. The inten-
standard. The values given in parentheses are for information
sity ratio values obtained from these data are used to calibrate
only.
the X-ray analyzer. Samples are prepared having a similar
1.5 This standard does not purport to address all of the
matrix to fit the calibration range and measured using the same
safety concerns, if any, associated with its use. It is the
analytical parameters.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
NOTE 1—Yttrium, strontium, and bromine K-a and thorium L-a lines
have been used successfully as internal standard lines. Explanation of the
bility of regulatory limitations prior to use. Specific precau-
internal standard method of analysis is outside the scope of this test
tionary statements are given in Section 9 and Note 2.
7,8
method and is found in several sources.
2. Referenced Documents
5. Significance and Use
2.1 ASTM Standards:
5.1 This test method is applicable to organic solutions
C 982 Guide for Selecting Components for Energy-
containing 20 to 2000 µg uranium/mL of solution presented to
Dispersive X-Ray Fluorescence (XRF) Systems
the spectrometer.
C 1118 Guide for Selecting Components for Wavelength-
Annual Book of ASTM Standards, Vol 11.01.
1 5
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear Annual Book of ASTM Standards, Vol 03.05.
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of Available from U.S. Department of Commerce, National Institute of Standards
Test. and Technology, Gaithersburg, MD 20899.
Current edition approved July 10, 1996. Published September 1996. Bertin, E. P., Introduction to X-ray Spectrometric Analysis, Plenum Press, New
Andermann, G., and Kemp, J. W., “Scattered X-rays as Internal Standards in York and London, 1978.
X-ray Spectroscopy,” Analytical Chemistry, Vol 20, No. 8, 1958. Tertian, R., and Claisse, F., Principles of Quantitative X-ray Fluorescence
Annual Book of ASTM Standards, Vol 12.01. 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 (2002)
5.2 Either wavelength-dispersive or energy-dispersive XRF 9. Technical Precautions
systems may be used, provided that the software accompany-
9.1 X-ray fluorescence equipment analyzes by the interac-
ing the system is able to accommodate the use of internal
tion of ionizing radiation with the sample. Applicable safety
standards.
regulations and standard operating procedures must be re-
viewed prior to the use of such equipment. All current XRF
6. Interferences
spectrometers are equipped with safety interlock to prevent
accidental penetration of the X-ray beam by the user. Do not
6.1 Thistestmethodrequirestheuseofaninternalstandard.
override these interlocks (see NBS Handbook 111).
Care must be taken that the samples analyzed by this test
9.2 Instrument performance may be influenced by environ-
method do not contain the internal standard or chemicals that
mental factors such as heat, vibration, humidity, dust, stray
wouldremovetheinternalstandardfromsolution.Thesamples
electronic noise, and line voltage stability. These factors and
must also be miscible with TBP.
performancecharacteristicsshouldbereviewedpriortotheuse
of this test method.
7. Apparatus
7.1 X-ray Spectrometer—See Guide C 982 or Guide C 1118
10. Preparation of Apparatus
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
chosen before the insertion of samples into the instrument.
NOTE 2—Caution: Allow sufficient stabilization time before analysis.
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
of dispensing the internal standard reproducibly to a level of
10.2 X-ray Power Supply—If the power to the X-ray tube is
0.5 % relative standard deviation of the volume dispensed.
not controlled by the instrument software, set the proper
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 D 1193.
11.1.2 Dissolve the material in TBP; heat on a hot plate, if
8.3 Nitric Acid, HNO , concentrated (70 %).
necessary.
11.1.3 Transfer the dissolved material to a 1000-mL volu-
8.4 1,3,5-Tribromobenzene, technical grade (or substitute
for internal standard). metric flask, and dilute to volume with TBP. (Storage of the
solution in an opaque container with a screw cap is recom-
8.5 Tri-n-Butyl Phosphate (TBP), techni
...