ASTM C1296-95(2007)
(Test Method)Standard Test Method for Determination of Sulfur in Uranium Oxides and Uranyl Nitrate Solutions by X-Ray Fluorescence (XRF) (Withdrawn 2007)
Standard Test Method for Determination of Sulfur in Uranium Oxides and Uranyl Nitrate Solutions by X-Ray Fluorescence (XRF) (Withdrawn 2007)
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 g sulfur/mL. Higher concentrations may be measured by appropriate dilutions.
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.
WITHDRAWN RATIONALE
This test method covers the sample preparation and analysis by X-ray fluorescence (XRF) of sulfur in uranium oxides and uranyl nitrate solutions.
Formerly under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle, this test method was withdrawn in June 2007 due to lack of use in the industry.
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:C1296–95(Reapproved 2007)
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 mLin a matrix of 0.08 g uranium per mLare 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 or Crystals
C 967 Specification for Uranium Ore Concentrate test method can be used to determine conformance to specifi-
C 982 Guide for Selecting Components for Energy- cation for uranium ore concentrate (see Specification C 967),
uranium trioxide (UO ), uranium dioxide (UO ), and uranyl
Dispersive X-Ray Fluorescence (XRF) Systems
3 2
C 1118 Guide for Selecting Components for Wavelength- nitrate (see Specification C 788). For uranium solutions, the
uranium content should be between 0.07 g/mLand 0.10 g/mL.
Dispersive X-Ray Fluorescence (XRF) Systems
D 1193 Specification for Reagent Water
6. Interferences
E 135 Terminology Relating to Analytical Chemistry for
6.1 Sulfur X-rays (53.7 nm) are extremely soft (long wave-
Metals, Ores, and Related Materials
length) X-rays and are easily absorbed by uranium; therefore,
2.2 Other Documents:
it is important to match the uranium concentration in the
NBS Handbook 111, Radiation Safety for X-Ray Diffraction
standards and test samples to compensate for this absorption
and X-Ray Fluorescence Analysis Equipment
effect since no internal standard is used in this test method.
Even if the sulfur content of the sample is in the correct range,
errors can result if the uranium concentration is not matched.
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
6.2 As with all XRF methods, the choice of X-ray tube
Test.
targetisimportant.Becauseofthelineoverlapofmolybdenum
Current edition approved Feb. 1, 2007. Published March 2007. Originally
and sulfur, molybdenum target tubes are not recommended.
approved in 1995. Last previous edition approved in 2001 as C 1296–95(2001).
Chromium, rhodium, and scandium target tubes have been
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
found to be satisfactory.
Standards volume information, refer to the standard’s Document Summary page on
6.3 The presence of impurities such as zirconium and cobalt
the ASTM website.
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.
C1296–95 (2007)
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 mat
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