ASTM C1296-95
(Test Method)Standard Test Method for Determination of Sulfur in Uranium Oxides and Uranyl Nitrate Solutions by X-Ray Fluorescence (XRF)
Standard Test Method for Determination of Sulfur in Uranium Oxides and Uranyl Nitrate Solutions by X-Ray Fluorescence (XRF)
SCOPE
1.1 This test method covers the sample preparation and analysis by X-ray fluorescence (XRF) of sulfur in uranium oxides and uranyl nitrate solutions.
1.2 This test method is valid for those solutions containing 100 to 500 µg sulfur/mL. Higher concentrations may be measured by appropriate dilutions.
1.3 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 determine the applicability of regulatory limitations prior to use. See Section 9 and Note 1 for specific hazards statements.
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Designation: C 1296 – 95
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Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Determination of Sulfur in Uranium Oxides and Uranyl
1
Nitrate Solutions by X-Ray Fluorescence (XRF)
This standard is issued under the fixed designation C 1296; 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 per mL in a matrix of 0.08 g uranium per mL are placed in the
liquid sample holder of an X-ray spectrometer and exposed to
1.1 This test method covers the sample preparation and
an X-ray beam capable of exciting the sulfur K-alpha emission
analysis by X-ray fluorescence (XRF) of sulfur in uranium
line. The intensity values obtained from these standard solu-
oxides and uranyl nitrate solutions.
tions are used to calibrate the X-ray spectrometer.
1.2 This test method is valid for those solutions containing
4.2 Either wavelength-dispersive or energy-dispersive
100 to 500 μg sulfur/mL. Higher concentrations may be
X-ray fluorescence systems may be used for this analysis.
measured by appropriate dilutions.
1.3 This standard does not purport to address all of the
5. Significance and Use
safety concerns, if any, associated with its use. It is the
5.1 This test method is applicable to uranium solutions,
responsibility of the user of this standard to establish appro-
uranium oxides, and other uranium compounds that are soluble
priate safety and health practices and determine the applica-
in nitric acid and contain sulfur up to 5000 μg/g sample. This
bility of regulatory limitations prior to use. See Section 9 and
test method can be used to determine conformance to specifi-
Note 1 for specific hazards statements.
cation for uranium ore concentrate (see Specification C 967),
2. Referenced Documents
uranium trioxide (UO ), uranium dioxide (UO ), and uranyl
3 2
2.1 ASTM Standards: nitrate (see Specification C 788). For uranium solutions, the
uranium content should be between 0.07 g/mL and 0.10 g/mL.
C 788 Specification for Nuclear-Grade Uranyl Nitrate So-
2
lution
6. Interferences
2
C 967 Specification for Uranium Ore Concentrate
6.1 Sulfur X-rays (53.7 nm) are extremely soft (long wave-
C 982 Guide for Selecting Components for Generic Energy-
length) X-rays and are easily absorbed by uranium; therefore,
Dispersive X-Ray Fluorescence (XRF) Systems for
2
it is important to match the uranium concentration in the
Nuclear-Related Material, Analysis
standards and test samples to compensate for this absorption
C 1118 Guide for Selecting Components for Wavelength-
2
effect since no internal standard is used in this test method.
Dispersive X-Ray Fluorescence (XRF) Systems
3
Even if the sulfur content of the sample is in the correct range,
D 1193 Specification for Reagent Water
errors can result if the uranium concentration is not matched.
E 135 Terminology Relating to Analytical Atomic Spectros-
4
6.2 As with all XRF methods, the choice of X-ray tube
copy
target is important. Because of the line overlap of molybdenum
2.2 Other Documents:
and sulfur, molybdenum target tubes are not recommended.
NBS Handbook 111, Radiation Safety for X-Ray Diffraction
5
Chromium, rhodium, and scandium target tubes have been
and X-Ray Fluorescence Analysis Equipment
found to be satisfactory.
3. Terminology
6.3 The presence of impurities such as zirconium and cobalt
3.1 For definitions of terms used in this test method, refer to
also should be considered for their interfering effects. Such
Terminology E 135.
considerations are outside the scope of this test method.
4. Summary of Test Method
7. Apparatus
4.1 Solution standards containing 0 (blank) to 500 μg sulfur
7.1 X-ray spectrometer—See Specification C 982 or Guide
C 1118 for the selection of the X-ray spectrometer. This test
1
This test method is under the jurisdiction of ASTM Committee C-26 on Nuclear
method is valid for either energy-dispersive or wavelength-
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
dispersive systems. The system must be equipped with an inert
Test.
Current edition approved April 15, 1995. Published June 1995. gas flush system (normally helium). (See Section 11 on
2
Annual Book of ASTM Standards, Vol 12.01.
Preparation of Apparatus.)
3
Annual Book of ASTM Standards, Vol 11.01.
7.2 Sample cups—Prepare liquid sample cups for the X-ray
4
Annual Book of ASTM Standards, Vol 03.05.
5
spectrometer as described by the manufacturer. Vented, dispos-
Available from the U.S. Department of Commerce, National Institute of
Standards and
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