ASTM C1453-00

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Designation:C1453–00
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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Summary of Test Method
1.1 This test method covers the determination of uranium 3.1 A weighed portion of UO is converted to U O by
2 3 8
and the oxygen to uranium atomic ratio in nuclear grade repeated ignition at 900°C in air, to a constant weight.
uranium dioxide powder and pellets. Corrections are made for nonvolatile and volatile impurities
1.2 This test method does not include provisions for pre- including moisture, based on independent determinations de-
3,4
venting criticality accidents or requirements for health and scribed in Test Methods C696 and C1287.
safety.Observanceofthistestmethoddoesnotrelievetheuser
4. Significance and Use
of the obligation to be aware of and conform to all interna-
tional, national, or federal, state and local regulations pertain- 4.1 The test method is designed to show whether or not a
material meets the specifications as given in Specifications
ing to possessing, shipping, processing, or using source or
special nuclear material. C753 or C776.
4.2 The powder’s stoichiometry is useful for predicting the
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the oxide’s sintering behavior in the pellet production process.
responsibility of the user of this standard to establish appro-
5. Interferences
priate safety and health practices and determine the applica-
5.1 The moisture content must be determined and a correc-
bility of regulatory limitations prior to use.
tion must be made for the moisture content otherwise a high
1.4 This test method also is applicable to UO and U O
3 3 8
bias will occur for the O/U ratio.
powder.
5.2 A nonvolatile impurity correction must be made other-
2. Referenced Documents
wiseahighbiaswilloccurfortheuraniumvalue.Anextended
ignition time may be required if significant amounts of anions
2.1 ASTM Standards:
C696 Test Methods for Chemical, Mass Spectrometric and that are difficult to decompose are present.
5.3 TheU O touraniumconversionfactorandtheuranium
Spectrochemical Analysis of Nuclear-Grade Uranium Di-
3 8
oxide Powders and Pellets atomic weight will require adjustment for nonnatural isotopic
concentrations otherwise a bias will be present.
C753 Specification for Nuclear-Grade, Sinterable Uranium
Dioxide Powder
2 6. Apparatus
C776 Specification for Sintered Uranium Dioxide Pellets
6.1 Desiccator, containing a moisture absorbent.
C1267 Test Method for Uranium by Iron II Reduction in
6.2 Muffle Furnace, capable of maintaining and controlling
Phosphoric Acid Followed by Chromium VI Titration in
temperatures to 900 6 25°C.
the Presence of Vanadium
6.3 Analytical Balance, capable of weighing to 6 0.1 mg.
C1287 Test Method for Determination of Impurities in
6.4 Platinumware.
Uranium Dioxide by Inductively Coupled Plasma Mass
Spectrometry
7. Reagents and Materials
7.1 Anhydrousmagnesiumperchlorate−Mg(ClO ) ,mois-
4 2
ture absorbent, or equivalent.
1 3
ThistestmethodisunderthejurisdictionofASTMcommitteeC-26onNuclear Jones, R.J., Ed., “Selected Measurement Methods for Plutonium and Uranium
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of in the Nuclear Fuel Cycle,” USAEC Document TID-7029, 1963, AERDB, pp.
Test. 91–93.
Current edition approved Jan. 10, 2000. Published March 2000. Petit, G.D. and Keinberger, C.A., “Preparation of Stoichiometric U O ,”
3 8
Annual Book of ASTM Standards, Vol 12.01. Analytical Chemistry, ANCHA Vol 25, 1961, p. 579.
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C1453
TABLE 1 Oxide Conversion Factors for Impurity Correction
8. Procedure
A
Impurity Assumed Oxide Form Oxide Conversion Factor
8.1 Transfer 2 to 12 g of UO powder or pellets to a tared
Al Al O 1.89
2 3
platinum crucible and weigh to within 0.1 mg.
BB O 3.23
2 3
8.1.1 UO Powder—Place the platinum crucible containing
2 Ba BaO 1.12
the UO powder sample in a muffle furnace and ignite for 3 h Be BeO 2.78
Bi Bi O 1.11
2 3
at 900 6 25°C.
Ca CaO 1.40
8.1.2 UO Pellets—Preheat the pellets at 500°C for 3 h, in
Cd CdO 1.14
Co Co O 1.41
2 3
the muffle furnace, then ignite for3hat900 6 25°C.
Cr Cr O 1.46
2 3
8.2 Remove the crucible from the furnace, allow to cool in
Cu CuO 1.25
Fe Fe O 1.43
the air 2 to 3 minutes, then place the crucible in a desiccator
2 3
B
In In O 1.21
2 3
and cool to room temperature. Weigh the crucible.
Li Li O 2.15
8.3 Repeat the ignition for 3 h at 900°C and repeat step 8.2
Mg MgO 1.66
Mn MnO 1.58
until a constant weight of 6 0.3 mg is obtained. 2
Mo MoO 1.50
8.4 Otherignitionandcoolingschemesmaybeusedaslong
Na Na O 1.35
as the analyst verifies the precision and the bias of the Ni NiO 1.27
PP O 2.29
2 5
measurement.
Pb PbO 1.15
Sb Sb O 1.26
2 4
9. Calculation Si SiO 2.14
Sn SnO 1.27
9.1 Uranium Content—Calculate as follows:
Ti TiO 1.67
VV O 1.79
2 5
U,wt% 5 @~0.8480 ~W 2WI!/S!X100# 2C (1)
Zn ZnO 1.24
Zr ZrO 1.35
where:
Ta Ta O 1.22
2 5
0.8480 5 U O to uranium conversion factor for natural WWO 1.26
3 8
A
uranium.Thisfactorwillrequireadjustmentwhen
Oxide conversion factor is defined as grams oxide per gram of element.
B
This element is not required by the UO Specifications C 753 and C 776 but is
the uranium isotopic abundance deviates from
included for information only.
natural uranium. See Appendix X1.2.
W 5 Grams of U O a
...