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| DOE-STD-3028-2000
specification for the material prepared for the light-water breeder reactor (LWBR)
program [Parrott, Sr. et al, 1979]. Given that the material has already seen
elevated temperatures for extended time, it is unlikely that further heating will
show extensive enhancement.
4. The Standard requires verification that materials have been adequately stabilized.
Stabilizing above 750C (1382F) and appropriate handling prior to packaging
ensure that the only significant mechanism for container pressurization is radiolysis
of readsorbed water into pressurizing gases. Thus, verification of adequate
stabilization requires measurement (e.g., LOI) to ensure that residual volatiles in the
packaged material is below the threshold specified in Criterion 6.1.2.1. The LOI test
is accomplished by heating the oxide sample to at least 800C (1472F) for at least
one hour and determining the resulting weight loss. The temperature selected must
be higher than the stabilization temperature. However, the temperature should not
be so high as to decompose U3O8, which forms gaseous UO3 from 900-1500C
(1652-2732F) depending on surface area [Kirk-Othmer 1997]. Therefore, 800C
(1472F) was chosen as the LOI temperature. The LOI test has great attractiveness
because of its simplicity and low cost. However, LOI does not directly measure the
parameter of greatest interest hydrogenous material content. Indeed, because of
the chemistry of uranium oxides, LOI may give false results when applied to the
forms UO3 and UO2. At temperatures greater than 450C (842F) in air, UO3 will
begin to convert to U3O8. Thus, a portion of the LOI result will be from oxygen loss
and the LOI measurement will be greater than the volatiles loss. UO2 will also
convert to U3O8 at temperatures greater than 450C (842F) in air. In the case of
UO2 the LOI measurement will be less than the volatiles loss and may even show a
"gain on ignition." Even U3O8 heated above 500-700C (932-1292F) may give off
oxygen to form substoichiometric U3O8-x [Gmelin 1978]. This Standard therefore
encourages use of LOI with mass spectroscopy analysis of the off gas. Note that if
the material is stabilized as part of the repackaging process, it should be U3O8 (see
Section A.6.1.2.3).
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