ASTM C1871-22
(Test Method)Standard Test Method for Determination of Uranium Isotopic Composition by the Double Spike Method Using a Thermal Ionization Mass Spectrometer
Standard Test Method for Determination of Uranium Isotopic Composition by the Double Spike Method Using a Thermal Ionization Mass Spectrometer
SIGNIFICANCE AND USE
5.1 Uranium material is used as a fuel in certain types of nuclear reactors. To be suitable for use as nuclear fuel, the starting material shall meet certain specifications such as those described in Specifications C753, C776, C787, C833, C967, C996, and C1008, or as specified by the purchaser. The 235U/238U isotope amount ratios and the amount content of uranium material can be measured by mass spectrometry following this test method to ensure that they meet the specification.
5.2 The double spike method has been used for studies of uranium fractionation effects in isotope geochemistry and cosmochemistry, for uranium source attribution in nuclear forensics and for investigation of conversion or sampling processes in nuclear industry and nuclear safeguards (7-11). Most recently, the double spike method has been used for the validation of the Cristallini sampling method of UF6 (12 and 13). The double spike method can be used for a wide range of sample sizes even in samples containing as low as 50 μg of uranium. The concentration of the loading solution for the DS method has to be in the range of 1 to 6 mg/g to allow a sample loading of 4 to 6 μg of uranium. A minimum loading of 4 μg uranium per filament is recommended.
5.3 The measurement of 236U/238U ratios using this method is not possible due to the large isobaric interference from the 236U ion beam of the double spike onto the 236U ion beam from the sample (>50.000 times for close to natural material, for example, like IRMM-184).
5.4 The application of the double spike method for measurements of 235U/238U ratio is limited by the isobaric interference between the 236U from the double spike material and the 236U contained in the sample. As a consequence, the method is not suitable for samples which contain significant amounts of 236U due to prior neutron capture from 235U in the predecessor materials. For samples with 236U/238U ratios higher than about 10–6, the double spike method should be applied with...
SCOPE
1.1 This test method describes the determination of the isotope amount ratios of uranium material as nitrate solutions by the double spike (DS) method using a thermal ionization mass spectrometer (TIMS) instrument.
1.2 The analytical performance in the determination of the 235U/238U major isotope amount ratio by the DS method is five to ten times better in terms of the internal and external reproducibility compared to the (“classical”) total evaporation (TE) method as described in Test Method C1672 and the “modified total evaporation” (MTE) as described in Test Method C1832. This is due to the use of an internal rather than external mass fractionation correction by using a double spike material with a known or certified 233U/236U isotope ratio, which is mixed with the sample prior to the measurement, either during the sample preparation or directly on the TIMS filament.
1.3 The DS method cannot be applied for the determination of the 236U/238U minor isotope amount ratio, and is also not recommended for the determination of the 234U/238U minor isotope amount ratio.
1.4 In case the uranium amount concentration of the double spike is known or certified, the uranium amount concentration of the sample can be determined using the isotope dilution mass spectrometry (IDMS) method as described in Test Method C1672, by blending the sample gravimetrically with the double spike and performing a DS measurement.
1.5 An external mass fractionation correction by measurements of a certified reference material loaded on different filaments and measured in the same measurement sequence, as recommended for TE and required for MTE measurements, is not necessary for the DS method. However, for quality control (QC) purposes it is recommended to perform DS measurements of low enriched or natural uranium isotopic reference materials on a regular basis.
1.6 The DS method can only be applied to uranium samples with relative isotope ...
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: C1871 − 22
Standard Test Method for
Determination of Uranium Isotopic Composition by the
Double Spike Method Using a Thermal Ionization Mass
1
Spectrometer
This standard is issued under the fixed designation C1871; 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 ments of low enriched or natural uranium isotopic reference
materials on a regular basis.
1.1 This test method describes the determination of the
isotope amount ratios of uranium material as nitrate solutions 1.6 TheDSmethodcanonlybeappliedtouraniumsamples
233 –5
by the double spike (DS) method using a thermal ionization with relative isotope abundances U/U below 10 and
236 –4
mass spectrometer (TIMS) instrument. U/Ubelow5×10 ,theDSmethodisthereforemainlyused
for low enriched or close to natural uranium samples.
1.2 The analytical performance in the determination of the
235 238
U/ UmajorisotopeamountratiobytheDSmethodisfive 1.7 Units—The values stated in SI units are to be regarded
to ten times better in terms of the internal and external as the standard. When no SI units are provided, the values are
reproducibility compared to the (“classical”) total evaporation for information only.
(TE) method as described in Test Method C1672 and the
1.8 This standard does not purport to address all of the
“modified total evaporation” (MTE) as described in Test
safety concerns, if any, associated with its use. It is the
MethodC1832.Thisisduetotheuseofan internalratherthan
responsibility of the user of this standard to establish appro-
external mass fractionation correction by using a double spike
priate safety, health, and environmental practices and deter-
233 236
material with a known or certified U/ U isotope ratio,
mine the applicability of regulatory limitations prior to use.
which is mixed with the sample prior to the measurement,
1.9 This international standard was developed in accor-
either during the sample preparation or directly on the TIMS
dance with internationally recognized principles on standard-
filament.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
1.3 The DS method cannot be applied for the determination
236 238
mendations issued by the World Trade Organization Technical
of the U/ U minor isotope amount ratio, and is also not
234 238
Barriers to Trade (TBT) Committee.
recommended for the determination of the U/ U minor
isotope amount ratio.
2. Referenced Documents
1.4 In case the uranium amount concentration of the double
2
2.1 ASTM Standards:
spike is known or certified, the uranium amount concentration
C753Specification for Nuclear-Grade, Sinterable Uranium
of the sample can be determined using the isotope dilution
Dioxide Powder
mass spectrometry (IDMS) method as described in Test
C776SpecificationforSinteredUraniumDioxidePelletsfor
Method C1672, by blending the sample gravimetrically with
Light Water Reactors
the double spike and performing a DS measurement.
C787Specification for Uranium Hexafluoride for Enrich-
1.5 An external mass fractionation correction by measure-
ment
ments of a certified reference material loaded on different
C833Specification for Sintered (Uranium-Plutonium) Diox-
filaments and measured in the same measurement sequence, as
ide Pellets for Light Water Reactors
recommended for TE and required for MTE measurements, is
C859Terminology Relating to Nuclear Materials
not necessary for the DS method. However, for quality control
C967Specification for Uranium Ore Concentrate
(QC) purposes it is recommended to perform DS measure-
C996Specification for Uranium Hexafluoride Enriched to
235
Less Than 5% U
1
ThistestmethodisunderthejurisdictionofASTMCommitteeC26onNuclear
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
2
Test. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Feb. 1, 2022. Published March 2022. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 2018. Last previous edition approved in 2018 as C1871–18a. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/C1871-22. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
C1871 − 22
C1008 Specification for Sintered (Uranium-Plutoniu
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: C1871 − 18a C1871 − 22
Standard Test Method for
Determination of Uranium Isotopic Composition by the
Double Spike Method Using a Thermal Ionization Mass
1
Spectrometer
This standard is issued under the fixed designation C1871; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This test method describes the determination of the isotope amount ratios of uranium material as nitrate solutions by the double
spike (DS) method using a thermal ionization mass spectrometer (TIMS) instrument.
235 238
1.2 The analytical performance in the determination of the U/ U major isotope amount ratio by the DS method is five to ten
times better in terms of the internal and external reproducibility compared to the (“classical”) total evaporation (TE) method as
described in Test Method C1672 and the “modified total evaporation” (MTE) as described in Test Method C1832. This is due to
the use of an internal rather than external mass fractionation correction by using a double spike material with a known or certified
233 236
U/ U isotope ratio, which is mixed with the sample prior to the measurement, either during the sample preparation or directly
on the TIMS filament.
236 238
1.3 The DS method cannot be applied for the determination of the U/ U minor isotope amount ratio, and is also not
234 238
recommended for the determination of the U/ U minor isotope amount ratio.
1.4 In case the uranium amount concentration of the double spike is known or certified, the uranium amount concentration of the
sample can be determined using the isotope dilution mass spectrometry (IDMS) method as described in Test Method C1672, by
blending the sample gravimetrically with the double spike and performing a DS measurement.
1.5 An external mass fractionation correction by measurements of a certified reference material loaded on different filaments and
measured in the same measurement sequence, as recommended for TE and required for MTE measurements, is not necessary for
the DS method. However, for quality control (QC) purposes it is recommended to perform DS measurements of low enriched or
natural uranium isotopic reference materials on a regular basis.
233 –5 236
1.6 The DS method can only be applied to uranium samples with relative isotope abundances U/U below 10 and U/U
–5–4
below 5 × 10 , the DS method is therefore mainly used for low enriched or close to natural uranium samples.
1.7 Units—The values stated in SI units are to be regarded as the standard. When no SI units are provided, the values are for
information only.
1
This test method is under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of Test.
Current edition approved June 1, 2018Feb. 1, 2022. Published July 2018March 2022. Originally approved in 2018. Last previous edition approved in 2018 as
C1871 – 18.C1871 – 18a. DOI: 10.1520/C1871-18A.10.1520/C1871-22.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
C1871 − 22
1.8 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, health, and environmental practices and determine the applicability of
regulatory limitations prior to use.
1.9 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2
2.1 ASTM Standards:
C753 Specification for Nuclear-Grade, Sinterable Uranium Dioxide Powder
C776 Specification for Sintered Uranium Dioxide Pellets for Light Water Reactors
C787 Specification for Uranium Hexafluoride for Enrichment
C833 Specification for Sintered (Uranium-Plutonium) Dioxide Pellets for Light Water Reactors
C859 Terminology Relating to Nuclear Materials
C967 Specification for Uranium Ore Concentrate
235
C996 Specification for Uranium Hexafluoride Enriched to Less Than 5 % U
3
C1008 Specification for Sintered (Uranium-Plutonium) D
...
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