ASTM C1380-04(2011)
(Test Method)Standard Test Method for Determination of Uranium Content and Isotopic Composition by Isotope Dilution Mass Spectrometry (Withdrawn 2018)
Standard Test Method for Determination of Uranium Content and Isotopic Composition by Isotope Dilution Mass Spectrometry (Withdrawn 2018)
SIGNIFICANCE AND USE
Determination of percent uranium content and 235U abundance in oxides and other materials containing high concentrations of uranium is required for special nuclear materials accountability, regulatory requirements, and process control.
SCOPE
1.1 This test method covers a method for the determination of the uranium concentration in uranium oxides by isotope dilution mass spectrometry (IDMS). The isotopic composition of the oxide is measured simultaneously.
1.2 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.
WITHDRAWN RATIONALE
This test method covered a method for the determination of the uranium concentration in uranium oxides by isotope dilution mass spectrometry (IDMS). The isotopic composition of the oxide was measured simultaneously.
Formerly under the jurisdiction of Committee C26 on Nuclear Fuel Cycle, this test method was withdrawn in June 2018. This standard is being withdrawn without replacement because the information in this test method is duplicated in more detail in other ASTM standards; specifically, the dissolution of uranium oxide is covered in Practice C1347 and TIMS IDMS measurements in Test Methods C1625 and C1672.
General Information
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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: C1380 − 04 (Reapproved 2011)
Standard Test Method for
the Determination of Uranium Content and Isotopic
Composition by Isotope Dilution Mass Spectrometry
This standard is issued under the fixed designation C1380; 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 5. Interferences
1.1 This test method covers a method for the determination 5.1 The calculations assume any U in the sample is
of the uranium concentration in uranium oxides by isotope negligible. If the sample contains significant U, the sample
dilution mass spectrometry (IDMS). The isotopic composition must be analyzed for isotopic composition with and without
of the oxide is measured simultaneously. added spike, and the calculations adjusted accordingly.
1.2 This standard does not purport to address all of the
6. Apparatus
safety concerns, if any, associated with its use. It is the
6.1 Thermal ionization mass spectrometer (TIMS) config-
responsibility of the user of this standard to establish appro-
ured with Faraday cup detectors and an automated operating
priate safety and health practices and determine the applica-
system.
bility of regulatory limitations prior to use.
6.2 Preconditioning unit for the TIMS.
2. Referenced Documents
6.3 Filament loading assembly for the TIMS.
2.1 ASTM Standards:
6.4 Balance, analytical, with five-place range.
D1193Specification for Reagent Water
6.5 Vials, glass, disposable with plastic caps.
3. Summary of Test Method
6.6 Pipet, automatic, Ranin or equivalent, variable to 1000
3.1 For measurement of the elemental uranium concentra-
µL.
tion of uranium oxides by IDMS, a representative and accu-
6.7 Pipet tips, disposable plastic, 100–1000 µL.
rately measured aliquot of the sample is prepared. A known
6.8 Liquid dispenser, Repipette™ or equivalent.
quantityof U(“spike”)isaddedtoanaliquotofthesample.
The sample aliquot and spike are taken to dryness, redissolved
7. Reagents and Materials
in dilute nitric acid, and loaded on a filament for analysis in a
thermal ionization mass spectrometer (TIMS). After measure-
7.1 Purity of Materials—Reagent grade chemicals shall be
ment of the isotopic ratios in the spiked sample, the uranium used in all tests. Unless otherwise indicated, it is intended that
content and isotopic composition of sample are calculated.
all reagents conform to the specification of the Committee on
Analytical Reagents of theAmerican Chemical Society where
4. Significance and Use
such specifications are available. Other grades may be used
provided it is first ascertained that the reagent is of sufficiently
4.1 Determination of percent uranium content and U
high purity to permit its use without lessening the accuracy of
abundance in oxides and other materials containing high
the determination.
concentrations of uranium is required for special nuclear
materials accountability, regulatory requirements, and process
7.2 Purity of Water—Unless otherwise indicated, references
control.
to water shall mean reagent water in conformance with
Specification D1193.
1 7.3 Nitric Acid, HNO , concentrated (70%).
ThistestmethodisunderthejurisdictionofASTMCommitteeC26onNuclear 3
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
Test.
Current edition approved June 1, 2011. Published June 2011. Originally Reagent Chemicals, American Chemical Society Specifications, American
approved in 1997. Last previous edition approved in 2004 as C1380–04. DOI: Chemical Society,Washington, D. C. For suggestions on the testing of reagents not
10.1520/C1380-04R11. listedbytheAmericanChemicalSociety,Washington,D.C.Forsuggestionsonthe
For referenced ASTM standards, visit the ASTM website, www.astm.org, or testing of reagents not listed by the American Chemical Society, see Analar
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U. K., and the
Standards volume information, refer to the standard’s Document Summary page on United States Pharmacopeia and National Formulary, U.S. Pharmacopeial Con-
the ASTM website. vention (USPC), Rockville, MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1380 − 04 (2011)
7.4 Nitric Acid, 0.8 M (5% v/v)—Cautiously add 50 mLof 10.5 Removethesamplefromthehotplateandexaminethe
concentrated nitric acid to 950 mL of water. residue.
7.5 Nitric Acid,0.1 M—Add6.5mLconcentratednitricacid
NOTE 3—If conversion of the sample to orange/red uranium nitrate/
to ≈900 mL of water, mix, and bring to 1000 mL with water. oxide was incomplete, repeat Steps 10.3-10.5.
7.6 Hydrogen Peroxide H O , 30%. 10.6 After conversion is complete and the sample is dry,
2 2
cool the vial, add 40 mL 0.8 M HNO , and cap with the
7.7 Elemental and Isotopic Uranium Standards (New
appropriate plastic lined cap.
Brunswick Laboratory CRM 114, CRM 116, CRM 129, or
equivalent ). 10.7 Mix the vial contents thoroughly by inverting vigor-
ously.
7.8 Uranium-233 spike assay and isotopic standard (NBL
CRM111–A orequivalent)—DiluteNBLCRM111–A1:50by
10.8 Weigh the vial and its contents to the nearest 0.1 mg
weight with a 5% nitric acid to give a U concentration of
and record the weight.
approximately 10 µg U/g solution.
10.9 Label a new 20–mL vial with sample identification
NOTE 1—An exact 1:50 dilution is not required.The requirement is for
number and “Dil 1.”
precise and accurate weights of standard and diluent. Calculate the exact
10.10 Place the labeled vial and a plastic lined cap on the
concentration of each isotope in the diluted spike standard in accordance
with11.2.OtherdilutionsofCRM111-Amaybeusedifaccurateweights
balance, and zero the balance.
areknown,andthealiquotofCRM111–Ausedinthemeasurementoftest
233 23X
10.11 Add 0.5 mLof the original dilution (from step 10.8),
samples yields a U/ U ratio of at least 0.02, where X is the major
uranium isotope. setthecaponthevial,andrecordtheweighttothenearest0.01
mg.
8. Preparation of Apparatus
10.12 Tare the balance, add 20 mL of 0.8 M HNO , and
8.1 Prepare the thermal ionization mass spectrometer
record the weight to the nearest 0.01 mg.
(TIMS) in accordance with manufacturer’s recommendations.
10.13 Cap the vial and mix the contents thoroughly by
inverting vigorously.
9. Calibration and Standardization
233 10.14 Label a third vial with sample identification and “Dil
9.1 Standardization of U Spike Solution:
2,” place the vial and a plastic lined cap on the balance, and
9.1.1 Prior to using a new diluted spike solution, verify the
zero the balance.
concentration of the solution with CRM 129 uranium oxide or
its equivalent. If the new spike solution does not give results
10.15 Add0.5mLofDilution1,setthecaponthevial,and
within control limits, its standardized concentration must be record the weight to the nearest 0.01 mg.
verified with another NBL certified reference material for
10.16 Tarethebalance,add0.5mLof Uspikesolutionto
elemental uranium, such as CRM 114 or equivalent.
the vial, and record the weight to the nearest 0.01 mg.
9.2 Calibration of TIMS:
10.17 Add five drops of 30% H O and 1 mL of concen-
2 2
9.2.1 CalibratetheTIMSinaccordancewithmanufacturer’s
trated HNO to the vial, set it on the hot plate, and heat to
recommendations to achieve the user’s performance and qual-
dryness.
ity
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