ASTM C1453 - 19

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Designation: C1453 −19
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
1
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. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This test method covers the determination of uranium
and the oxygen to uranium atomic ratio in nuclear grade
uranium dioxide powder and pellets.
1.2 This test method does not include provisions for pre-
venting criticality accidents or requirements for health and
safety. Observance of this test method does not relieve the user
of the obligation to be aware of and conform to all
international, national, or federal, state and local regulations
pertaining to possessing, shipping, processing, or using source
or special nuclear material.
1.3 This test method also is applicable to UO
3
and U
3
O
8
powder.
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 appro-
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accor-
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
2
C696 Test Methods for Chemical, Mass Spectrometric, and
Spectrochemical Analysis of Nuclear-Grade Uranium Di-
oxide Powders and Pellets
C753 Speciﬁcation for Nuclear-Grade, Sinterable Uranium
Dioxide Powder
C776 Speciﬁcation for Sintered Uranium Dioxide Pellets for
Light Water Reactors
C859 Terminology Relating to Nuclear Materials
C1267 Test Method for Uranium by Iron (II) Reduction in
Phosphoric Acid Followed by Chromium (VI) Titration in
the Presence of Vanadium
C1287 Test Method for Determination of Impurities in
Nuclear Grade Uranium Compounds by Inductively
Coupled Plasma Mass Spectrometry
3. Terminology
3.1 For deﬁnitions of terms used in this test method but not
deﬁned herein, refer to Terminology C859.
4. Summary of Test Method
4.1 A weighed portion of UO
2
is converted to U
3
O
8
by
repeated ignition at 900°C in air, to a constant weight.
Corrections are made for nonvolatile and volatile impurities
including moisture, based on independent determinations de-
scribed in Test Methods C696 and C1287.
3,4
5. Signiﬁcance and Use
5.1 The test method is designed to show whether or not a
material meets the speciﬁcations as given in Speciﬁcations
C753 or C776.
5.2 The powder’s stoichiometry is useful for predicting the
oxide’s sintering behavior in the pellet production process.
6. Interferences
6.1 The moisture content must be determined and a correc-
tion must be made for the moisture content otherwise a high
bias will occur for the O/U ratio.
1
This test method is under the jurisdiction of ASTM committee C26 on Nuclear
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
Test.
Current edition approved July 1, 2019. Published August 2019. Originally
approved in 2000. Last previous edition approved in 2011 as C1453 – 00 (2011).
DOI: 10.1520/C1453-19.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
3
Jones, R.J., Ed., “Selected Measurement Methods for Plutonium and Uranium
in the Nuclear Fuel Cycle,” USAEC Document TID-7029, 1963, AERDB, pp.
91–93.
4
Petit, G.D. and Keinberger, C.A., “Preparation of Stoichiometric U
3
O
8
,”
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
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
1
 

6.2 A nonvolatile impurity correction must be made other-
wise a high bias will occur for the uranium value. An extended
ignition time may be required if signiﬁcant amounts of anions
that are difficult to decompose are present.
6.3 The U
3
O
8
to uranium conversion factor and the uranium
atomic weight will require adjustment for nonnatural isotopic
concentrations otherwise a bias will be present.
7. Apparatus
7.1 Desiccator, containing a moisture absorbent.
7.2 Muffle Furnace, capable of maintaining and controlling
temperatures to 900 625°C.
7.3 Analytical Balance, capable of weighing to 60.1 mg.
7.4 Platinumware.
8. Reagents and Materials
8.1 Anhydrous magnesium perchlorate − Mg (ClO
4
)
2
, mois-
ture absorbent, or equivalent.
9. Procedure
9.1 Transfer 2 to 12 g of UO
2
powder or pellets to a tared
platinum crucible and weigh to within 0.1 mg.
9.1.1 UO
2
Powder—Place the platinum crucible containing
the UO
2
powder sample in a muffle furnace and ignite for 3 h
at 900 625°C.
9.1.2 UO
2
Pellets—Preheat the pellets at 500°C for 3 h, in
the muffle furnace, then ignite for3hat900625°C.
9.2 Remove the crucible from the furnace, allow to cool in
the air 2 to 3 minutes, then place the crucible in a desiccator
and cool to room temperature. Weigh the crucible.
9.3 Repeat the ignition for 3 h at 900°C and repeat step 9.2
until a constant weight of 60.3 mg is obtained.
9.4 Other ignition and cooling schemes may be used as long
as the analyst veriﬁes the precision and the bias of the
measurement.
10. Calculation
10.1 Uranium Content—Calculate as follows:
U,wt%5
@
~
0.8480
~
W2WI
!
/S
!
X100
#
2C(1)
where:
0.8480 = U
3
O
8
to uranium conversion factor for natural
uranium. This factor will require adjustment when
the uranium isotopic abundance deviates from
natural uranium. See Appendix X1.2.
W= Grams of U
3
O
8
after ignition.
I= Total of all detected nonvolatile impurities ex-
pressed as grams of oxide per gram of ignited
U
3
O
8
. See Table 1 to obtain oxide conversion
factors for many common impurity elements en-
countered. The impurities are determined as de-
scribed in either Test Method C696 or C1287.
S= Initial sample weight, in g.
C= Total of all nonvolatile impurities analyzed as less
than the lower detection limit of the analytical
method. The detection limit values shall be taken
as the concentration of that element. The total is
expressed as percent. These impurities are deter-
mined as described in Test Method C696 or C1287.
Alternatively, the these impurities can be consid-
ered to contribute a total correction of 0.01 % to
the uranium percent.
10.2 Oxygen-to-Uranium Ratio—Calculate as follows from
the original sample U, wt%:
O/U 5
@
~
100 2Uwt%2Z2m
!~
A
!
#
/
@
~
15.999
!~
Uwt%
!
#
(2)
where:
O = atom % of oxygen
U = atom % of uranium
U wt% = U, weight %, as calculated in 10.1
Z = total non-volatile impurities correction, %, as de-
termined in Test Method C696 or C1287.
m = moisture and volatile impurity content, %, deter-
mined in Test Method C696 or C1287.
A = atomic weight of uranium based on isotopic abun-
dance. See X1.1.
15.999 = atomic weight of oxygen
TABLE 1 Oxide Conversion Factors for Impurity Correction
Impurity Assumed Oxide Form Oxide Conversion Factor
A
Al Al
2
O
3
1.89
BB
2
O
3
3.23
Ba BaO 1.12
Be BeO 2.78
Bi Bi
2
O
3
1.11
Ca CaO 1.40
Cd CdO 1.14
Co Co
2
O
3
1.41
Cr Cr
2
O
3
1.46
Cu CuO 1.25
Fe Fe
2
O
3
1.43
In
B
In
2
O
3
1.21
Li Li
2
O 2.15
Mg MgO 1.66
Mn MnO
2
1.58
Mo MoO
3
1.50
Na Na
2
O 1.35
Ni NiO 1.27
PP
2
O
5
2.29
Pb PbO
2
1.15
Sb Sb
2
O
4
1.26
Si SiO
2
2.14
Sn SnO
2
1.27
Ti TiO
2
1.67
VV
2
O
5
1.79
Zn ZnO 1.24
Zr ZrO
2
1.35
Ta Ta
2
O
5
1.22
WWO
3
1.26
A
Oxide conversion factor is deﬁned as grams oxide per gram of element.
B
This element is not required by the UO
2
Speciﬁcations C753 and C776 but is
included for information only.
TABLE 2 UO
2
Powder Results
Sample Type Uranium wt
% Absolute
Standard
Deviation O/U Ratio Standard
Deviation
No. of
Determinations
Sample A 87.796 0.005 2.065 0.001 12
Sample B 86.996 0.004 2.225 0.001 12
C1453 − 19
2
 

11. Precision and Bias

11.1 UO

Powder—The precision for the O/U ratio for UO

powder is shown in Table 2. The bias was not determined as

there are no standards due to the relative reactivity of the

powder. The data in Table 2 were determined by one analyst

over a three-day period.

11.2 UO

Pellets:

11.2.1 The precision for the O/U ratio for UO

pellets is

shown in Table 3.

The data were determined by two different

laboratories. The data for Laboratory A were determined over

several days by one analyst. The data for Laboratory B were

determined over seven days by four analysts using three

furnaces.

11.2.2 The precision for the uranium content for UO

pellets

is shown in Table 4. The data were determined as described for

Table 3.

11.2.3 The reference value for G-2 working pellet standard

was obtained from the weighted average of eight ferrous

sulphate type titration measurements and nine ignition type

measurements. The measurements were standardized against

NBL 125 standard. One analyst performed the measurements

over two weeks. The determined uranium value was 88.103 %

with a standard deviation of 0.053 %. The value is not

statistically different from the values determined by this test

method. The data does not indicate any statistically signiﬁcant

bias at the 88.103 % level.

12. Keywords

12.1 gravimetric; ignition; O/U ratio; oxygen; oxygen to

uranium ratio; uranium

Supporting data for Tables 2–X1.1 are available from ASTM Headquarters.

TABLE 3 Comparison of Interlab O/U Results

Laboratory Sample Type O/U Ratio Standard

Deviation

No. of

Determinations

A Sintered depleted UO

pellet G-2

2.001 0.001 4

B Sintered depleted UO

pellet G-2

2.000 0.002 18

TABLE 4 Comparison of Interlab Uranium Results

Method Laboratory Sample Type

Uranium

wt%

Absolute

Standard

Deviation

No. of

Determinations

Gravimetric A Sintered depleted

pellet G-2

88.106 0.003 4

Gravimetric B Sintered depleted

pellet G-2

88.114 0.010 18

Reference

value, see

11.2.3

B Sintered depleted

pellet G-2

88.103 0.053 See 11.2.3

C1453 − 19

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摘要：

ASTM C1453 - 19 是一项由美国材料与试验协会（ASTM）发布的标准测试方法，专门用于通过闪光法测定固体材料的热扩散率。该标准适用于陶瓷、耐火材料、金属、复合材料等非均匀或致密固体材料，在室温至高温范围内进行测量。热扩散率是评估材料导热性能与热响应特性的关键参数，广泛应用于航空航天、能源、电子封装及工业隔热领域。ASTM C1453 - 19 明确了样品制备要求、测量设备校准步骤以及数据分析方法，以确保测试结果的可重复性与准确性。通过遵循本标准，研究人员和工程师能够可靠地比较不同材料

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