ASTM C1672-07
(Test Method)Standard Test Method for Determination of Uranium or Plutonium Isotopic Composition or Concentration by the Total Evaporation Method Using a Thermal Ionization Mass Spectrometer
Standard Test Method for Determination of Uranium or Plutonium Isotopic Composition or Concentration by the Total Evaporation Method Using a Thermal Ionization Mass Spectrometer
SCOPE
1.1 This method describes the determination of the isotopic composition and/or the concentration of uranium and plutonium as nitrate solutions by the thermal ionization mass spectrometric (TIMS) total evaporation method. Purified uranium or plutonium nitrate solutions are loaded onto a degassed metal filament and placed in the mass spectrometer. Under computer control, ion currents are generated by heating of the filament(s). The ion beams are continually measured until the sample is exhausted. The measured ion currents are integrated over the course of the run, and normalized to a reference isotope ion current to yield isotopic ratios.
1.2 In principle, the total evaporation method should yield isotopic ratios that do not require mass bias correction. In practice, some samples may require this bias correction. When compared to the conventional TIMS method, the total evaporation method is approximately two times faster, improves precision from two to four fold, and utilizes smaller sample sizes.
1.3 The total evaporation method may lead to biases in minor isotope ratios due to peak tailing from adjacent major isotopes, depending on sample characteristics. The use of an electron multiplier equipped with an energy filter may eliminate or diminish peak tailing effects. Measurement of instrument abundance sensitivity may be used to ensure that such biases are negligible, or may be used to bias correct minor isotope ratios.
1.4 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.
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Designation: C1672 − 07
StandardTest Method for
Determination of Uranium or Plutonium Isotopic
Composition or Concentration by the Total Evaporation
1
Method Using a Thermal Ionization Mass Spectrometer
This standard is issued under the fixed designation C1672; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
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1.1 This method describes the determination of the isotopic 2.1 ASTM Standards:
C753Specification for Nuclear-Grade, Sinterable Uranium
composition and/or the concentration of uranium and pluto-
Dioxide Powder
nium as nitrate solutions by the thermal ionization mass
spectrometric (TIMS) total evaporation method. Purified ura- C757Specification for Nuclear-Grade Plutonium Dioxide
niumorplutoniumnitratesolutionsareloadedontoadegassed Powder, Sinterable
metal filament and placed in the mass spectrometer. Under C776Specification for Sintered Uranium Dioxide Pellets
C787Specification for Uranium Hexafluoride for Enrich-
computer control, ion currents are generated by heating of the
ment
filament(s). The ion beams are continually measured until the
C833Specification for Sintered (Uranium-Plutonium) Diox-
sample is exhausted. The measured ion currents are integrated
ide Pellets
over the course of the run, and normalized to a reference
C967Specification for Uranium Ore Concentrate
isotope ion current to yield isotopic ratios.
C996Specification for Uranium Hexafluoride Enriched to
1.2 In principle, the total evaporation method should yield
235
Less Than 5 % U
isotopic ratios that do not require mass bias correction. In
C1008Specification for Sintered (Uranium-Plutonium) Di-
practice, some samples may require this bias correction.When
oxide Pellets—Fast Reactor Fuel
compared to the conventional TIMS method, the total evapo-
C1068Guide for Qualification of Measurement Methods by
ration method is approximately two times faster, improves
a Laboratory Within the Nuclear Industry
precision from two to four fold, and utilizes smaller sample
C1156Guide for Establishing Calibration for a Measure-
sizes.
ment Method Used toAnalyze Nuclear Fuel Cycle Mate-
rials
1.3 The total evaporation method may lead to biases in
C1168PracticeforPreparationandDissolutionofPlutonium
minor isotope ratios due to peak tailing from adjacent major
Materials for Analysis
isotopes, depending on sample characteristics. The use of an
C1347Practice for Preparation and Dissolution of Uranium
electron multiplier equipped with an energy filter may elimi-
Materials for Analysis
nate or diminish peak tailing effects. Measurement of instru-
C1411Practice for The Ion Exchange Separation of Ura-
ment abundance sensitivity may be used to ensure that such
nium and Plutonium Prior to Isotopic Analysis
biases are negligible, or may be used to bias correct minor
238
C1415Test Method for Pu Isotopic Abundance By Alpha
isotope ratios.
Spectrometry
1.4 This standard does not purport to address all of the
D3084Practice for Alpha-Particle Spectrometry of Water
safety concerns, if any, associated with its use. It is the
E137Practice for Evaluation of Mass Spectrometers for
responsibility of the user of this standard to establish appro-
Quantitative Analysis from a Batch Inlet (Withdrawn
3
priate safety and health practices and determine the applica-
1992)
bility of regulatory limitations prior to use.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
1
ThistestmethodisunderthejurisdictionofASTMCommitteeC26onNuclear contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of Standards volume information, refer to the standard’s Document Summary page on
Test. the ASTM website.
3
Current edition approved June 1, 2007. Published July 2007. DOI: 10.1520/ The last approved version of this historical standard is referenced on
C1672-07. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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C1672 − 07
3. Terminology 4.2 Theisotopedilutionmassspectrometry(IDMS)method
may be used to determine the uranium or plutonium concen-
3.1 Definitions:
trations.Inthismethod,aspikeofknownisotopiccomposition
3.1.1 isotopic equilibration—chemicalstepsperformedona
and element concentration is added to a sample prior to
mixture of two samples (for example, a uranium sample and a
233
chemical separation. Typical spike materials include U
uranium spike) to ensure identical valency and chemical form
235 239 242 244
or U
...
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