ASTM C1287-95

Standard Test Method for Determination of Impurities in Uranium Dioxide by Inductively Coupled Plasma Mass Spectrometry

SCOPE
1.1 This test method covers the determination of 61 elements in uranium dioxide samples by inductively coupled plasma mass spectrometry (ICP-MS). The elements are listed in Table 1 along with their lower reporting limits.  
1.2 Similar levels of these elements in other uranic compounds can also be determined if they are treated and converted to the same uranium concentration solution.  
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.  For a specific warning statement, see Note 1.  Note 1—The ICP-MS is a source of intense ultra-violet radiation from the radio frequency induced plasma. Protection from radio frequency radiation and UV radiation is provided by the instrument under normal operation.
1.4 The test method for the additional elements boron, sodium, silicon, phosphorus, potassium, and calcium is given in Appendix X1.  
1.5 The test method for technetium-99 is given in Appendix X2.

General Information

• Status: Historical
• Publication Date: 09-Sep-1995
• Technical Committee: C26 - Nuclear Fuel Cycle
• Drafting Committee: C26.05 - Methods of Test

Relations

• Replaced By: ASTM C1287-95(2001) - Standard Test Method for Determination of Impurities in Uranium Dioxide by Inductively Coupled Plasma Mass Spectrometry
• Effective Date: 10-Sep-1995

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NOTICE: This standard has either been superseded and replaced by a new version or
withdrawn.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: C 1287 – 95
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Determination of Impurities in Uranium Dioxide by
1
Inductively Coupled Plasma Mass Spectrometry
This standard is issued under the fixed designation C 1287; 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.
3
1. Scope D 1193 Specification for Reagent Water
1.1 This test method covers the determination of 61 ele-
3. Summary of Test Method
ments in uranium dioxide samples by inductively coupled
3.1 The sample is dissolved in acid. A fixed quantity of
plasma mass spectrometry (ICP-MS). The elements are listed
internal standard is added to monitor and correct for signal
in Table 1 along with their lower reporting limits.
instability. The level of impurities in the solution is measured
1.2 Similar levels of these elements in other uranic com-
by ICP-MS. Customized software calculates the concentration
pounds can also be determined if they are treated and converted
of each element.
to the same uranium concentration solution.
3.2 Uranium-concentration-matched standard solutions are
1.3 This standard does not purport to address all of the
used to calibrate the ICP-MS instrument. The calibration is
safety concerns, if any, associated with its use. It is the
4,5
linear up to at least 0.2 μg/ml (100 μg/g U) for each analyte.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
4. Significance and Use
bility of regulatory limitations prior to use. For a specific
4.1 This test method is capable of measuring the elements in
warning statement, see Note 1.
Table 1, some of which are required by Specifications C 753,
NOTE 1—Warning: The ICP-MS is a source of intense ultra-violet C 776, C 787, C 788, C 967 and C 996.
radiation from the radio frequency induced plasma. Protection from radio
5. Apparatus
frequency radiation and UV radiation is provided by the instrument under
normal operation.
5.1 ICP-MS, controlled by computer and fitted with the
associated software and peripherals.
1.4 The test method for the additional elements boron,
5.2 Autosampler, with tube racks and disposable plastic
sodium, silicon, phosphorus, potassium, and calcium is given
sample tubes compatible with 5.1 (optional).
in Appendix X1.
5.3 Variable Micropipettes:
1.5 The test method for technetium-99 is given in Appendix
5.3.1 10 μL to 100 μL capacity.
X2.
5.3.2 100 μL to 1000 μL capacity.
5.3.3 1000 μL to 10.00 mL capacity.
2. Referenced Documents
5.4 Volumetric Flasks:
2.1 ASTM Standards:
5.4.1 50 mL capacity—polypropylene.
C 753 Specification for Nuclear-Grade, Sinterable Uranium
5.4.2 100 mL capacity—polypropylene.
2
Dioxide Powder
5.4.3 1 L capacity—glass.
2
C 776 Specification for Sintered Uranium Dioxide Pellets
5.5 Platinum Dish—100 mL capacity.
C 787 Specification for Uranium Hexafluoride for Enrich-
5.6 Silica Beaker—250 mL capacity.
2
ment
5.7 Watch Glasses—75 mm diameter.
C 788 Specification for Nuclear-Grade Uranyl Nitrate So-
2
lution
6. Reagents
2
C 967 Specification for Uranium Ore Concentrate
6.1 The sensitivity of the ICP-MS technique requires the use
C 996 Specification for Uranium Hexafluoride Enriched to
235
2
Less Than 5 % U
3
Annual Book of ASTM Standards, Vol 11.01.
4
“ICP-MS Versus Conventional Methods for the Analysis of Trace Impurities in
Nuclear Fuel,” by Allenby, P., Clarkson, A. S., Makinson, P. R., presented at 2nd
1
This test method is under the jurisdiction of ASTM Committee C-26 on Nuclear
Surrey Conference on Plasma Source Mass Spectrometry, Guildford, UK, July
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of 1987.
5
Test. “Trace Metals in NBL Uranium Standard CRM 124 Using ICP-MS,” by
Current edition approved Sept. 10, 1995. Published November 1995. Originally Aldridge, A. J., Clarkson, A. S., Makinson, P. R., Dawson, K. W., presented at 1st
published as C 1287 – 94. Last previous edition C 1287 – 94. Durham International Conference on Plasma Source Mass Spectrometry, Durham,
2
Annual Book of ASTM Standards, Vol 12.01. UK, September 1988.
1

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C 1287
TABLE 1 Reporting Limits of Impurity Elements in Uranium
of ultra high purity reagents in order to be able to obtain the
Dioxide
low levels of detection. All the reagents below are ultra high
purity grade unless otherwise stated:
NOTE 1—Acquisition time 5 10 s/isotope using peak jump mode.
NOTE 2—103 Rh was used a
...