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ANP PROJECT QIJARTERX,Y PRQCRESS REPORT
mixture intimately mixed. The capsule
is then tilted so that the ball closes
the lower valve and isolates the upper
part of the salt phase, which is then
solidified 2nd analyzed for its
potassium content. The data obtained
are summarized in Table 10.4.
PRODUCTION AND PURIFICATION OF
FLUORIDE MIXTURES
F. F. Blankenship G. J. Nessle
Materials Chemistry Division
IJse of the hydrogenation-hydro-
fluorination process previously
described for fuel-sample preparation
has been continued on laboratory and
pilot scales for production of standard
materials for corrosion testing,
physical property evaluat,ion, and
1 arge -component t es t ing .
Construction of the production
equipment to furnish 3000 lb of NaZrFS
for the ARE is in an advanced stage.
Raw materials are being accumulated at
a satisfactory rate.
A modification of the purification
treatment has been adopted for micro-
scale processing of samples containing
enriched uranium for radiation-damage
testing.
Aslight modification of the standard
procedure has been used successfully
to purify mixtures containing 50
mole % NaF, 25 mole % ZrF4, and 25
mole % UF,.
Preparation of NaZrF5 by direct
hydrofluorination of ZrO, in the
presence of NaF has been moderately
successful in simple equipnien t. Further
study of this process is planned.
-
122
Labor at0 ry - Sc a1 e Foe 1 P reparation
(13. E. Thoma, C. M. Blood, F. P. Boody,
Materials Chemistry Division) . Fourteen
batches of purified molten fluoride
compositions, both coolant and fuel,
have been prepared for loop tests,
measurement of physical properties,
and corrosion testing. These were
treated in essentially the same manner
as previously reported.(")
To explore the unlikely possibility
that hydrogen reduces UF, or ZrF,,
two of the fuel batches were given an
additional hydrogenation for 1 hr
following the regular procedure. No
evidence of reduced phases in the
products from these runs was shown by
examination with the petrographic
microscope. However there is evidence
that the material so prepared was
slightly less corrosive in small-scale
tests than was the standard fuel. No
explanation for this effect has been
suggested; however, further study of
this behavior is planned.
Modifications of techniques of
assembling and disassembling apparatus
have resulted in less frequent failure
than was experienced at the beginning
of the hydrofluorination program.
Corrosion of the reactors has not yet
been a problem when the standard
treatment is applied to relatively
pure fluoride mixtures.
Pilot-Scale Fuel Purification
(G. J. Nessle, J. E. Eorgan, Materials
Chemistry Division). Two apparatus
capable of producing up to 3 kg of
('"C. M. Blood, F. P. Boody, A. J. Weinberger,
and G. J. Nessle, ANP Quar. Prog. Rep. June 10.
1952, ORNL-1294, p. 97.
TABLE 10.4. SOLUBILITY OF POTASSIUM IN NaF-KF-LiF
........ ._._____-
_.
TEMPERATURE OF NO. OF
POTASSIUM CONTENT
EXPERIMENT (OC) E XP En I ME NT S
(mol@ %)
..... ....... .... .... ......
544
68 6
9 20
10 40
....... 1
I L
.... ......... ._-I.
3.8
3. 5
3.7 * 0.5
3.9