ASTM C1413-05(2011)
(Test Method)Standard Test Method for Isotopic Analysis of Hydrolyzed Uranium Hexafluoride and Uranyl Nitrate Solutions by Thermal Ionization Mass Spectrometry
Standard Test Method for Isotopic Analysis of Hydrolyzed Uranium Hexafluoride and Uranyl Nitrate Solutions by Thermal Ionization Mass Spectrometry
SIGNIFICANCE AND USE
Uranium hexafluoride used to produce nuclear fuel must meet certain criteria for its isotopic composition as described in Specifications C787 and C996.
SCOPE
1.1 This method applies to the determination of isotopic composition in hydrolyzed nuclear grade uranium hexafluoride. It covers isotopic abundance of 235U between 0.1 and 5.0 % mass fraction, abundance of 234U between 0.0055 and 0.05 % mass fraction, and abundance of 236U between 0.0003 and 0.5 % mass fraction. This test method may be applicable to other isotopic abundance providing that corresponding standards are available.
1.2 This test method can apply to uranyl nitrate solutions. This can be achieved either by transforming the uranyl nitrate solution to a uranyl fluoride solution prior to the deposition on the filaments or directly by depositing the uranyl nitrate solution on the filaments. In the latter case, a calibration with uranyl nitrate standards must be performed.
1.3 This test method can also apply to other nuclear grade matrices (for example, uranium oxides) by providing a chemical transformation to uranyl fluoride or uranyl nitrate solution.
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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Standards Content (Sample)
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Designation:C1413 −05 (Reapproved 2011)
Standard Test Method for
Isotopic Analysis of Hydrolyzed Uranium Hexafluoride and
Uranyl Nitrate Solutions by Thermal Ionization Mass
Spectrometry
This standard is issued under the fixed designation C1413; 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 C761Test Methods for Chemical, Mass Spectrometric,
Spectrochemical, Nuclear, and RadiochemicalAnalysis of
1.1 This method applies to the determination of isotopic
Uranium Hexafluoride
composition in hydrolyzed nuclear grade uranium hexafluo-
C776Specification for Sintered Uranium Dioxide Pellets
ride. It covers isotopic abundance of U between 0.1 and
C787Specification for Uranium Hexafluoride for Enrich-
5.0% mass fraction, abundance of U between 0.0055 and
ment
0.05% mass fraction, and abundance of U between 0.0003
C788Specification for Nuclear-Grade Uranyl Nitrate Solu-
and0.5%massfraction.Thistestmethodmaybeapplicableto
tion or Crystals
other isotopic abundance providing that corresponding stan-
C996Specification for Uranium Hexafluoride Enriched to
dards are available.
Less Than 5 % U
1.2 This test method can apply to uranyl nitrate solutions.
C1334Specification for Uranium Oxides with a U Con-
This can be achieved either by transforming the uranyl nitrate
tent of LessThan 5 % for Dissolution Prior to Conversion
solution to a uranyl fluoride solution prior to the deposition on
to Nuclear-Grade Uranium Dioxide
the filaments or directly by depositing the uranyl nitrate
,
C1346Practice for Dissolution of UF from P-10 Tubes
solution on the filaments. In the latter case, a calibration with
C1347Practice for Preparation and Dissolution of Uranium
uranyl nitrate standards must be performed.
Materials for Analysis
1.3 This test method can also apply to other nuclear grade 235
C1348Specification for Blended Uranium Oxides with U
matrices (for example, uranium oxides) by providing a chemi-
Content of LessThan 5 % for Direct Hydrogen Reduction
cal transformation to uranyl fluoride or uranyl nitrate solution.
to Nuclear Grade Uranium Dioxide
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
3. Summary of Test Method
responsibility of the user of this standard to establish appro-
3.1 After dilution of uranyl fluoride or uranyl nitrate
priate safety and health practices and determine the applica-
solution, approximatively 2 µg of uranium are deposited on a
bility of regulatory limitations prior to use.
rheniumfilament.Analysisisperformedinathermalionization
2. Referenced Documents
mass spectrometer (TIMS), uranium is vaporized and ionized
through electrons emitted by a second filament; ions are
2.1 ASTM Standards:
extractedbyanelectricfield,separatedbyamagneticfield,and
C696Test Methods for Chemical, Mass Spectrometric, and
collected by four collectors on mass 234, 235, 236, 238. The
SpectrochemicalAnalysis of Nuclear-Grade Uranium Di-
oxide Powders and Pellets collectors are either faraday cups or electron multipliers
C753Specification for Nuclear-Grade, Sinterable Uranium collectors (ion counting).
Dioxide Powder
3.2 Evaporation sequence and ion counting time are ad-
justed with the analysis of standard solutions of certified
ThistestmethodisunderthejurisdictionofASTMCommitteeC26onNuclear
isotopic content. Nitrate and fluoride solutions lead to two
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
different calibrations.
Test.
Current edition approved June 1, 2011. Published June 2011. Originally
approved in 1999. Last previous edition approved in 2005 as C1413–05. DOI:
4. Significance and Use
10.1520/C1413-05R11.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4.1 Uraniumhexafluorideusedtoproducenuclearfuelmust
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
meetcertaincriteriaforitsisotopiccompositionasdescribedin
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. Specifications C787 and C996.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1413−05 (2011)
5. Interferences 7.4 Isotopic Uranium Standards
236 235
7.4.1 UF of certified U, U isotopic composition,
5.1 This test method only applies to nuclear grade uranium
such as COG 006, 008, 009, 010, 013, 014, 015.
matrices(asdefinedinSpecificationC753,C776,C787,C788,
7.4.2 U O of certified isotopic composition, such as NBL
3 8
C1334,or C1348). Large amount of impurities, which are
CRM U-010, U-020, U-030, U-050, CEA 014.
found, for example, in uranium ore concentrates, may bias
7.4.3 U O from reprocessed origin and of certified U
3 8
results. A purification step may be necessary, as described in
composition, such as MIR 1.
Specification C696.
7.5 Hydrofluoric Acid (0.05 M)—Dilute 173 µL of HF
5.2 The type of acid used (HF or HNO ) and its concentra-
solution (sp gr 1.18, 28.9 M) to 100 mL with water.
tion will strongly influence the obtained isotopic results (see
9.2). 7.6 Nitric Acid (0.1 M)—Dilute 0.6 mL of concentrated
HNO (sp gr 1.42, 16 M) to 100 mL with water.
6. Apparatus
8. Preparation of Apparatus
6.1 Thermal Ionization Mass Spectrometer (TIMS)—
Configured with four detectors.
8.1 Prepare the thermal ionization mass spectrometer in
6.1.1 This test method requires a mass spectrometer with a
accordance with the manufacturer’s recommendations.Averi-
resolution greater than 400 (full width at 1% of peak height)
fication of collector yield and an optimisation of the ion beam
–5
and an abundance sensitivity of less than 10 (contribution of
may be necessary on a daily basis. This can be achieved by
mass 238 on the mass 237). A typical instrument would have
heating the ionizing filament, locating the Re peak and
230 mm radius of curvature, single or double focussing, and
focusing for maximum intensity. The Re signal is normally
–11
single or multiple filament design. The pressure in the ioniza-
above 0.1 to 0.2 × 10 A.
–6 –7
tion chamber should be below 3 × 10 torr (typically 10
8.2 A verification of mass calibration is usually performed
torr).
on a weekly basis in order to optimize the value for the
6.2 Preconditioning Unit for the TIMS—To dry filament
magnetic field.
after deposition of uranyl solution.
9. Calibration and Standardization
6.3 Rhenium Filament Loading Assembly for the TIMS—In
9.1 Because of mass segregation during the evaporation of
this test method, a double filament set up is used.
uranium, it is necessary to adjust the ion acquisition time
6.4 Pipets—Automatic or equivalent, 1, 20, 50, and 100 µL.
program with the analysis of uranium standards. The number
6.5 Pipets Tips—In accordance with 6.4.
of standards and the range covered will depend on the
instrument used, the evaporation sequence, and the accuracy
6.6 Liquid Dispenser—2.5 mL.
which is required.
6.7 Disposable Polypropylene Vials.
9.1.1 Fortheanalysisof Uinthe0.1to5.0mass%range
and of U in the 0.0055 to 0.05 mass % range, four to seven
7. Reagents and Materials
standardsshouldbeused(seeTable1).Foranalysisof Uin
7.1 Purity of Materials—Reagent grade chemicals shall be
the0.0003to0.5mass%range,onlytwostandardswereused.
used in all tests. Unless otherwise indicated, it is intended that
9.2 Preparation of the Standards—Separate calibrations are
all reagents conform to the specification of the Committee on
required for uranyl fluoride solutions and uranyl nitrate solu-
Analytical Reagents of theAmerican Chemical Society where
tions.
such specifications are available. Other grades may be used
9.2.1 Uranyl Fluoride Calibration:
provided it is first ascertained that the reagent is of sufficiently
9.2.1.1 UF Standards—Generalprinciplesforhydrolysisof
highprioritytopermititsusewithoutlesseningtheaccuracyof
UF are described in Test Methods C761 and Practice C1346.
the determination.
Hydrolysis should be done in pure water (no HNO added).
7.2 Purity of Water—Demineralized or distilled water is
Final concentration is for example 266 g uranium per litre
found acceptable for this uranium isotopic analysis.
(20% mass U).
7.3 High Purity Rhenium Filaments (> 99.95 %), with
NOTE 1—Other concentrations may be used (for example, 10% mass
geometricalcharacteristicsinaccordancewiththeTIMSmanu-
U),providedthatvolumesin10.2areadaptedtodepositthesameuranium
facturer’s recommendations (typically thickness is 0.04 mm
amount on the rhenium filament.
and width is 0.70 mm). Some equipment may accept tungsten
NOTE 2—2 µg of uranium are deposited on the filaments. In case of
filaments. other filament geometries (see 7.3), other uranium amounts may be more
adapted (up to 10 µg U).
9.2.1.2 In a polypropylene vial, pour 2.5 mL of water and
Areducednumberofdetectorsmaybeusedwhichwillcorrespondtoareduced
numberofisotopesanalyzed.Forsinglecollectorinstruments,refertoSpecification
add 20 µLof solution prepared in 9.2.1.1. Mix the vial content
C696.
byinvertingvigorouslytoobtainasolutioncontainingapproxi-
Reagent Chemicals, American Chemical Society Specificati
...
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