ASTM C1296-95(2001)
(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:C1296–95(Reapproved 2001)
Standard Test Method for
Determination of Sulfur in Uranium Oxides and Uranyl
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 3. Terminology
1.1 This test method covers the sample preparation and 3.1 For definitions of terms used in this test method, refer to
analysis by X-ray fluorescence (XRF) of sulfur in uranium Terminology E 135.
oxides and uranyl nitrate solutions.
4. Summary of Test Method
1.2 This test method is valid for those solutions containing
100 to 500 µg sulfur/mL. Higher concentrations may be 4.1 Solution standards containing 0 (blank) to 500 µg sulfur
per mL in a matrix of 0.08 g uranium per mL are placed in the
measured by appropriate dilutions.
1.3 This standard does not purport to address all of the liquid sample holder of an X-ray spectrometer and exposed to
an X-ray beam capable of exciting the sulfur K-alpha emission
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- line. The intensity values obtained from these standard solu-
tions are used to calibrate the X-ray spectrometer.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. See Section 9 and 4.2 Either wavelength-dispersive or energy-dispersive
X-ray fluorescence systems may be used for this analysis.
Note 1 for specific hazards statements.
2. Referenced Documents 5. Significance and Use
5.1 This test method is applicable to uranium solutions,
2.1 ASTM Standards:
C 788 Specification for Nuclear-Grade Uranyl Nitrate So- uranium oxides, and other uranium compounds that are soluble
in nitric acid and contain sulfur up to 5000 µg/g sample. This
lution
C 967 Specification for Uranium Ore Concentrate test method can be used to determine conformance to specifi-
C 982 GuideforSelectingComponentsforGenericEnergy- cation for uranium ore concentrate (see Specification C 967),
uranium trioxide (UO ), uranium dioxide (UO ), and uranyl
Dispersive X-Ray Fluorescence (XRF) Systems for
3 2
Nuclear-Related Material, Analysis nitrate (see Specification C 788). For uranium solutions, the
uranium content should be between 0.07 g/mL and 0.10 g/mL.
C 1118 Guide for Selecting Components for Wavelength-
Dispersive X-Ray Fluorescence (XRF) Systems
3 6. Interferences
D 1193 Specification for Reagent Water
6.1 Sulfur X-rays (53.7 nm) are extremely soft (long wave-
E 135 TerminologyRelatingtoAnalyticalAtomicSpectros-
length) X-rays and are easily absorbed by uranium; therefore,
copy
it is important to match the uranium concentration in the
2.2 Other Documents:
standards and test samples to compensate for this absorption
NBS Handbook 111, Radiation Safety for X-Ray Diffraction
effect since no internal standard is used in this test method.
and X-Ray Fluorescence Analysis Equipment
Even if the sulfur content of the sample is in the correct range,
errors can result if the uranium concentration is not matched.
6.2 As with all XRF methods, the choice of X-ray tube
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear
targetisimportant.Becauseofthelineoverlapofmolybdenum
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
and sulfur, molybdenum target tubes are not recommended.
Test.
Chromium, rhodium, and scandium target tubes have been
Current edition approved April 15, 1995. Published June 1995.
Annual Book of ASTM Standards, Vol 12.01.
found to be satisfactory.
Annual Book of ASTM Standards, Vol 11.01.
6.3 The presence of impurities such as zirconium and cobalt
Annual Book of ASTM Standards, Vol 03.05.
also should be considered for their interfering effects. Such
Available from the U.S. Department of Commerce, National Institute of
Standards and Technology, Gaithersburg, MD 20899. considerations are outside the scope of this test method.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
C1296
7. Apparatus equipment, or system, performance characteristics should be
reviewed prior to use of this test method.
7.1 X-ray spectrometer—See Specification C 982 or Guide
C 1118 for the selection of the X-ray spectrometer. This test
10. Preparation of Apparatus
method is valid for either energy-dispersive or wavelength-
10.1 Chamber environment:
dispersive systems.The system must be equipped with an inert
10.1.1 The standards and samples used in this test method
gas flush system (normally helium). (See Section 11 on
are corrosive liquids. Some fumes will be emitted from the
Preparation of Apparatus.)
sample cups.These fumes may be detrimental to the spectrom-
7.2 Sample cups—Prepare liquid sample cups for the X-ray
eter chamber. It is desirable to flush this chamber with an inert
spectrometer as described by the manufacturer.Vented, dispos-
gas (usually helium) before and during analysis. Some X-ray
able sample cups with snap-on caps are satisfactory for most
spectrometers control the change of sample chamber atmo-
such analyses; such cups decrease the likelihood of contami-
sphere (air, vacuum, helium) automatically through the soft-
nation between samples.
ware; in others, it must be done manually. Follow the instru-
7.2.1 Polypropylene film has been used successfully as the
ment manufacturer’s recommendations to achieve the inert gas
film window for such cups. Tests should be performed to
environment. Allow sufficient stabilization time before analy-
determinetheserviceabilityofanyfilmchosenbeforeinsertion
sis.
into the instrument. Care must be taken to ensure that the film
chosen does not excessively or irreproducibly affect the net
NOTE 1—Caution: Take care to ensure that a vacuum environment is
intensity of the sulfur X-rays.
not chosen with liquid samples.
10.2 X-ray power supply:
8. Reagents and Materials
10.2.1 IfthepowertotheX-raytubeisnotcontrolledbythe
8.1 Purity of Reagents—Reagent grade chemicals shall be
instrument software, set the proper combination of voltage and
used in all tests. Unless otherwise indicated, it is intended that
current for the instrument in use. These settings must be
all reagents conform to the specifications of the Committee of
determined by the user for his instrument and choice of X-ray
Analytical Reagents of the American Chemical Society where
tube. Allow sufficient stabilization time prior to analysis.
such specifications are available. Other grades may be used
provided it is first ascertained that the reagent is of sufficiently
11. Calibration and Standardization
high purity to permit its use without lessening the accuracy of
11.1 Uranium Stock Solution, 0.20 g/mL:
the determination.
11.1.1 Weigh into a 600-mL beaker 118.01 g of uranium
8.2 Purity of Water—Unless otherwise indicated, references
oxide (NBL CRM-129 or equivalent) that has been dried
to water shall mean reagent water conforming to Specification
according to the instructions received with the material (each
D 1193.
batch has the conditions under which its value was deter-
8.3
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