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u 2.4. PRODUCTION OF FUELS
c G. J. Nessle G. M. Watson
L. G. Overholser
I EXPERIMENTAL PREPARATION OF
c
tid
VARIOUS FLUORIDES
B. J. Sturm
Continued use of structural metal fluorides for
research necessitated the preparation of additional
quantities of these materials by the several methods
developed previously. As in the past, use was
made of chemical, x-ray, and petrographic examinations
to establish the identity and purity of the
materials.
Additional CrF, was prepared by hydrofluorination
of anhydrous CrCI,, as well as by the thermal
decomposition of (NH ) CrF6. The latter is pre-
4.3
pared by the interaction of hydrated CrF, with
NH,F.HF, and it may also be reduced by hydrogen
to yield CrF,. Several batches of NiF, were prepared
by the hydrofluorination of either hydrated
NiF, or hydrated NiCI,. One batch of AgF was
prepared by hydrofluorination of AG,CO,. Methods
described previously’ were used for the preparation
of additional quantities of CeF, and of LaF,.
An attempt to remove oxide from a KF-ZrF, mixture
by hydrofluorination was unsuccessful. Runs
at 60OOC failed to remove the oxide completely
and, while this could be accomplished at 85OOC,
the loss of ZrF, was sufficient to alter the composition
to the point where the material was unsatisfactory
for its intended purpose.
A batch of CuF, was prepared for use as a carrier
in certain spectrographic boron analyses. Material
low in boron and silicon was requested for
this purpose. Anhydrous CuF, was hydrofluorinated
for 4 hr at 4OO0C, but this short period of
treatment failed to reduce the boron content to a
sufficiently low level. However, extending the
period of hydrofluorination to 20 hr
terial that was acceptable.
A fuel mixture containing Li7 and
nium was prepared for radiation damage studies.
Since Li7 was available only as the carbonate, a
preliminary run was made with normal Li,CO,
UF, KF, NaF, and excess NH,F*HF to establish
whether fusion of this mixture would yield an
oxide-free product. After the prel iminary run proved
successful the procedure was applied to the mixture
containing Li’ and U2,’. The material was
PERIOD ENDING JUNE 10, 1956
oxide free, but a sulfur content of 170 ppm was
reported, most of which came from the LiiCO,.
The fuel was subjected to 5 cycles, each of which
entailed a 10- to 15-hr hydrogen treatment and 1 hr
of hydrofluorination at 80OoC. The product then
contained 45 ppm of sulfur and a trace of oxide,
Hydrofluorination at 70O0C for 6 hr then produced
an oxide-free product.
LABORATORY-SCALE PURIFICATION
OPE RATIONS
F. L. Daley W. T. Ward
With appropriate modifications, the standard hy-
drofluorination-hydrogenation process was used
to prepare a number of especially pure materials
requested for various purposes. Of these only an
NaF-ZrF,-UF, mixture containing additives of
BaF,, LaF,, and RbF had not previously been pre-
pared by the standard procedure. operational foci I-
ities to transfer and dispense small samples (200
to 500 g), especially into apparatus for accurate
evaluation of physical properties of materials, were
constructed and used successfully during this quar-
ter. There is evidence that direct transfer of the
purified melt into the apparatus has significantly
improved the purity of the test material and, ac-
cordingly, increased confidence in the test results.
Copper-I ined stainless steel reactors were used
successfully in the purification operations.
P ILOT-SC AL E PUR I FICATION OP ER AT IONS
J. P. Blakely C. R. Croft
J. Truitt
e pilot-scale purification facility processed 68
es totaling approximately 1300 Ib of various
de compositions for use in small-scale corro-
sion testing, phase equilibrium studies, and phys-
ical property studies. The bulk of the materiai
was produced during February when the facility
was operating on a threeshift, 24-hr-day basis. As
a result, the backlog reported last quarter was
eliminated and normal operations were resumed.
’B. J. Sturm, ANP Quat. Pmg. Rep. March 10, 1956.
ORNL-2061, p 100.
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