ASTM C1380-97

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 1380 – 97
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 C 1380; 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 6. Apparatus
6.1 Thermal ionization mass spectrometer (TIMS) config-
1.1 This test method covers a method for the determination
of the uranium concentration in uranium oxides by isotope ured with Faraday cup detectors and an automated operating
dilution mass spectrometry (IDMS). The isotopic composition system.
of the oxide is measure simultaneously. 6.2 Preconditioning unit for the TIMS.
1.2 This standard does not purport to address all of the 6.3 Filament loading assembly for the TIMS.
safety concerns, if any, associated with its use. It is the 6.4 Balance, analytical, with five-place range.
responsibility of the user of this standard to establish appro- 6.5 Vials, glass, disposable with plastic caps.
priate safety and health practices and determine the applica- 6.6 Pipet, automatic, Ranin or equivalent, variable to 1000
bility of regulatory limitations prior to use. μL.
6.7 Pipet tips, disposable plastic, 100–1000 μL.
2. Referenced Documents
6.8 Liquid dispenser, Repipettey or equivalent.
2.1 ASTM Standards:
7. Reagents and Materials
D 1193 Specification for Reagent Water
7.1 Purity of Materials—Reagent grade chemicals shall be
3. Summary of Test Method
used in all tests. Unless otherwise indicated, it is intended that
3.1 For measurement of the elemental uranium concentra- all reagents conform to the specification of the Committee on
tion of uranium oxides by IDMS, a representative and accu-
Analytical Reagents of the American Chemical Society where
rately measured aliquot of the sample is prepared. A known such specifications are available. Other grades may be used
quantity of U (“spike”) is added to an aliquot of the sample.
provided it is first ascertained that the reagent is of sufficiently
The sample aliquot and spike are taken to dryness, redissolved high purity to permit its use without lessening the accuracy of
in dilute nitric acid, and loaded on a filament for analysis in a the determination.
thermal ionization mass spectrometer (TIMS). After measure-
7.2 Purity of Water—Unless otherwise indicated, references
ment of the isotopic ratios in the spiked sample, the uranium to water shall mean reagent water in conformance with
content and isotopic composition of sample are calculated.
Specification D 1193.
7.3 Nitric Acid, HNO , concentrated (70 %).
4. Significance and Use
7.4 Nitric Acid, 0.8 M (5 % v/v)—Cautiously add 50 mL of
4.1 Determination of percent uranium content and U
concentrated nitric acid to 950 mL of water.
abundance in oxides and other materials containing high
7.5 Nitric Acid, 0.1 M—Add 6.5 mL concentrated nitric acid
concentrations of uranium is required for special nuclear
to ’900 mL of water, mix, and bring to 1000 mL with water.
materials accountability, regulatory requirements, and process
7.6 Hydrogen Peroxide H O ,30%.
2 2
control.
7.7 Elemental and Isotopic Uranium Standards (New Brun-
swick Laboratory CRM 114, CRM 116 CRM 129, or equiva-
5. Interferences 4
lent ).
5.1 The calculations assume any U in the sample is
negligible. If the sample contains significant U, the sample
must be analyzed for isotopic composition with and without 3
Reagent Chemicals, American Chemical Society Specifications, American
added spike, and the calculations adjusted accordingly. Chemical Society, Washington, D. C. For suggestions on the testing of reagents not
listed by the American Chemical Society, Washington, D. C. For suggestions on the
testing of reagents not listed by the American Chemical Society, see Analar
This test method is under the jurisdiction of ASTM Committee C-26 on Nuclear Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U. K., and the
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of United States Pharmacopeia and National Formulary, U.S. Pharmaceutical Con-
Test. vention (USPC), Rockville, MD.
Current edition approved December 10, 1997. Published May 1998. Available from the US Department of Energy, New Brunswick Laboratory, D
Annual Book of ASTM Standards, Vol 11.01. 350, 9800 South Cass Avenue, Argonne, IL 60439.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
C 1380
7.8 Uranium-233 spike assay and isotopic standard (NBL 10.11 Add 0.5 mL of the original dilution (from step 10.8),
CRM 111–A or equivalent)—Dilute NBL CRM 111–A 1:50 set the cap on the vial, and record the weight to the nearest 0.01
by weight with a 5 % nitric acid to give a U concentration of mg.
approximately 10 μg U/g solution. 10.12 Tare the balance, add 20 mL of 0.8 M HNO , and
record the weight to the nearest 0.01 mg.
NOTE 1—An exact 1:50 dilution is not required. The requirement is for
10.13 Cap the vial and mix the contents thoroughly by
precise and accurate weights of standard and diluent. Calculate the exact
inverting vigorously.
concentration of each isotope in the diluted spike standard in accordance
with 11.2. Other dilutions of CRM-111A may be used if accurate weights 10.14 Label a third vial with sample identification and “Dil
are known, and the aliquot of CRM 111–A used in the measurement of test
2,” place the vial and a plastic lined cap on the balance, and
233 23X
samples yields a U/ U ratio of at least 0.02, where X is the major
zero the balance.
uranium isotope.
10.15 Add 0.5 mL of Dilution 1, set the cap on the vial, and
record the weight to the nearest 0.01 mg.
8. Preparation of Apparatus
10.16 Tare the balance, add 0.5 mL of U spike solution to
8.1 Prepare the thermal ionization mass spectrometer
the vial, and record the weight to the nearest 0.01 mg.
(TIMS) in accordance with manufacturer’s recommendations.
10.17 Add five drops of 30 % H O and 1 mL of concen-
2 2
trated HNO to the vial, set it on the hot plate, and heat to
9. Calibration and Standardization
dryness.
9.1 Standardization of U Spike Solution:
10.18 Remove from the hot plate, cool, and add 0.02 mL 0.1
9.1.1 Prior to using a new diluted spike solution, verify the
M HNO .
concentration of the solution with CRM 129 uranium oxide or
10.19 Swirl or agitate the vial to dissolve the sample.
its equivalent. If the new spike solution does not give
...