ASTM C1453-00(2006)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:C1453–00(Reapproved2006)
Standard Test Method for
the Determination of Uranium by Ignition and the Oxygen to
Uranium (O/U) Atomic Ratio of Nuclear Grade Uranium
Dioxide Powders and Pellets
This standard is issued under the fixed designation C1453; 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 C1287 Test Method for Determination of Impurities in
Nuclear Grade Uranium Compounds by Inductively
1.1 This test method covers the determination of uranium
Coupled Plasma Mass Spectrometry
and the oxygen to uranium atomic ratio in nuclear grade
uranium dioxide powder and pellets.
3. Summary of Test Method
1.2 This test method does not include provisions for pre-
3.1 A weighed portion of UO is converted to U O by
2 3 8
venting criticality accidents or requirements for health and
repeated ignition at 900°C in air, to a constant weight.
safety.Observanceofthistestmethoddoesnotrelievetheuser
Corrections are made for nonvolatile and volatile impurities
of the obligation to be aware of and conform to all interna-
including moisture, based on independent determinations de-
tional, national, or federal, state and local regulations pertain-
,
scribed in Test Methods C696 and C1287.
ing to possessing, shipping, processing, or using source or
special nuclear material.
4. Significance and Use
1.3 This standard does not purport to address all of the
4.1 The test method is designed to show whether or not a
safety concerns, if any, associated with its use. It is the
material meets the specifications as given in Specifications
responsibility of the user of this standard to establish appro-
C753 or C776.
priate safety and health practices and determine the applica-
4.2 The powder’s stoichiometry is useful for predicting the
bility of regulatory limitations prior to use.
oxide’s sintering behavior in the pellet production process.
1.4 This test method also is applicable to UO and U O
3 3 8
powder.
5. Interferences
5.1 The moisture content must be determined and a correc-
2. Referenced Documents
2 tion must be made for the moisture content otherwise a high
2.1 ASTM Standards:
bias will occur for the O/U ratio.
C696 Test Methods for Chemical, Mass Spectrometric, and
5.2 A nonvolatile impurity correction must be made other-
Spectrochemical Analysis of Nuclear-Grade Uranium Di-
wiseahighbiaswilloccurfortheuraniumvalue.Anextended
oxide Powders and Pellets
ignition time may be required if significant amounts of anions
C753 Specification for Nuclear-Grade, Sinterable Uranium
that are difficult to decompose are present.
Dioxide Powder
5.3 TheU O touraniumconversionfactorandtheuranium
3 8
C776 Specification for Sintered Uranium Dioxide Pellets
atomic weight will require adjustment for nonnatural isotopic
C1267 Test Method for Uranium by Iron (II) Reduction in
concentrations otherwise a bias will be present.
PhosphoricAcid Followed by Chromium (VI) Titration in
the Presence of Vanadium
6. Apparatus
6.1 Desiccator, containing a moisture absorbent.
1 6.2 Muffle Furnace, capable of maintaining and controlling
This test method is under the jurisdiction ofASTM committee C26 on Nuclear
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of temperatures to 900 6 25°C.
Test.
6.3 Analytical Balance, capable of weighing to 6 0.1 mg.
Current edition approved July 1, 2006. Published September 2006. Originally
approved in 2000. Last previous edition approved in 2000 as C1453–00. DOI:
10.1520/C1453-00R06. Jones, R.J., Ed., “Selected Measurement Methods for Plutonium and Uranium
For referenced ASTM standards, visit the ASTM website, www.astm.org, or in the Nuclear Fuel Cycle,” USAEC Document TID-7029, 1963, AERDB, pp.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM 91–93.
Standards volume information, refer to the standard’s Document Summary page on Petit, G.D. and Keinberger, C.A., “Preparation of Stoichiometric U O ,”
3 8
the ASTM website. Analytical Chemistry, ANCHA, Vol 25, 1961, p. 579.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
C1453–00 (2006)
TABLE 1 Oxide Conversion Factors for Impurity Correction
6.4 Platinumware.
A
Impurity Assumed Oxide Form Oxide Conversion Factor
7. Reagents and Materials
Al Al O 1.89
2 3
BB O 3.23
2 3
7.1 Anhydrousmagnesiumperchlorate−Mg(ClO ) ,mois-
4 2 Ba BaO 1.12
ture absorbent, or equivalent. Be BeO 2.78
Bi Bi O 1.11
2 3
Ca CaO 1.40
8. Procedure
Cd CdO 1.14
Co Co O 1.41
2 3
8.1 Transfer 2 to 12 g of UO powder or pellets to a tared
Cr Cr O 1.46
2 3
platinum crucible and weigh to within 0.1 mg.
Cu CuO 1.25
Fe Fe O 1.43
2 3
8.1.1 UO Powder—Place the platinum crucible containing
2 B
In In O 1.21
2 3
the UO powder sample in a muffle furnace and ignite for 3 h
2 Li Li O 2.15
Mg MgO 1.66
at 900 6 25°C.
Mn MnO 1.58
8.1.2 UO Pellets—Preheat the pellets at 500°C for 3 h, in
Mo MoO 1.50
the muffle furnace, then ignite for3hat900 6 25°C.
Na Na O 1.35
Ni NiO 1.27
8.2 Remove the crucible from the furnace, allow to cool in
PP O 2.29
2 5
the air 2 to 3 minutes, then place the crucible in a desiccator
Pb PbO 1.15
Sb Sb O 1.26
and cool to room temperature. Weigh the crucible.
2 4
Si SiO 2.14
8.3 Repeat the ignition for 3 h at 900°C and repeat step 8.2
Sn SnO 1.27
until a constant weight of 60.3 mg is obtained.
Ti TiO 1.67
VV O 1.79
2 5
8.4 Otherignitionandcoolingschemesmaybeusedaslong
Zn ZnO 1.24
as the analyst verifies the precision and the bias of the
Zr ZrO 1.35
measurement. Ta Ta O 1.22
2 5
WWO 1.26
A
Oxide conversion factor is defined as grams oxide per gram of element.
9. Calculation
B
This element is not required by the UO Specifications C753 and C776 but is
included for information only.
9.1 Uranium Content—Calculate as follows:
U,wt% 5[~0.8480 ~W 2WI!/S!X100] 2C (1)
where:
where:
O = atom % of oxygen
0.8480 = U O to uranium conversion factor for natural
3 8 U = atom
...