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ORNL-1771 - Oak Ridge National Laboratory

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2.5 kg can be prepared in this equipment. During<br />

the quarter, 27 preparations that yielded about 70 kg<br />

of material were made.<br />

Repeated attempts to prepare NaF-KF-Li F mix-<br />

tures containing 14 wt % UF, and 1 wt % UF, by<br />

reduction of UF, with uranium metal yielded mix-<br />

tures containing 5 to 7 wt % UF, by chemical<br />

analysis. These results, along with those reported<br />

elsewhere in this document, seem to show that in<br />

systems containing KF, reduction of UF, by ura-<br />

nium metal is markedly incomplete. Pending clari-<br />

fication of this point, production of material con-<br />

taining 5 wt % UF, and 10 wt % UF, is under way,<br />

Production Facility<br />

J. P. Blakely F. L. Daley<br />

Materials Chemistry Division<br />

During the past quarter, 1760 kg of processed<br />

fluorides was produced in the 250.lb facility for<br />

external and internal distribution. A breakdown of<br />

the production according to composition is given<br />

below:<br />

Amount<br />

Processed<br />

(ks)<br />

NoF-ZrF4-UF4 (50-46-4 mole %) 79 1<br />

NaF-ZrF, (50-50 mole 76) 565<br />

NoF-ZrF4-UF4 (50-43.56.5 mole %) 404<br />

Pratt & Whitney Aircraft Division received 27 kg<br />

of NaF-ZrF, (50-50 mole %) and 113 kg of NaF-<br />

ZrF,-UF, (50-46-4 mole 96). Battelle Memorial<br />

Institute received 46 kg of NaF-ZrF,-UF, (50-46-4<br />

mole %) and 68 kg of NaF-ZrF, (50-50 mole %)-<br />

The remaining processed material was distributed<br />

to various requesters in the ANP Program.<br />

The difficulties associated with the long stripping<br />

times and large hydrogen volumes required for pra-<br />

duction of rigorously pure fluoride melts from the<br />

raw materials available have not yet been over-<br />

come.32 Attempts to shorten the time required by<br />

increasing the hydrogen flow rate from 4 to 15<br />

liters/min and thus decrease labor und maintenance<br />

costs were not successful. Under these conditions<br />

._.__i_______.l-<br />

32F, F. Blankenship and G. J. Nessle, ANP Qum.<br />

Prr,g. Rep. June IO, 1954, <strong>ORNL</strong>-1729, p 61.<br />

PERIOD ENDING SEPTEMBER 70, 1954<br />

the gas inlet tubes plugged quite frequently and<br />

the HF concentration in the exit hydrogen fell<br />

much below the value obtained at lower flow rates.<br />

The over-all purification time was not appreciably<br />

shortened by the fourfold increase in hydrogen<br />

passed.<br />

Sublimation of crude ZrF, at a temperature lower<br />

than that previously used by Y-12 personnel did<br />

not appreciably improve the purity of the ZrF,<br />

product. Accordingly, the NaF-ZrF, melts produced<br />

iri the near future will be prepared from the<br />

(NaF)x*ZrF, that is available in moderately pure<br />

form from a commercial source; hafnium-free ZrF4<br />

will be used to adjust the composition as required,<br />

since this material is available in a high state of<br />

purity,<br />

Electrolytic purification of NaF-ZrF4 mixtures<br />

has been shown to be complete, and the process<br />

requires much less time than does the hydrogen<br />

stripping process. Accordingly, one of the units<br />

in the production facility is being modified slightly<br />

to test this method on Q large scale. It is antici-<br />

pated that the use of the purer taw materials and<br />

the electrolytic purification process will consider-<br />

ably decrease the cost of fuel preparation.<br />

In-Pile Loop Loading<br />

J. E. Eorgan<br />

Materials Chemistry Division<br />

The first in-pile loop was loaded on June 11 with<br />

a fuel concentrate, NaF-ZrF,-UF, (62.5- 12.5-25.0<br />

mole %), prepared from enriched uranium by Y-12<br />

personnel. The loading apparatus and confrols<br />

performed satisfactorily, and the transfer of ma-<br />

terial to the loop went smoothly. However, the<br />

electrical contact which should have indicated<br />

when the loop was filled to operating level was<br />

not activated even after 120% of the calculated<br />

charge had been added.<br />

Subsequent examination of the loop showed that<br />

a weld had given way where the loop was connected<br />

to the pump bowl, and it seems certain that this<br />

leak was present during the filling operation. The<br />

U235 is being salvaged from the loop. Examination<br />

of the filling apparatus revealed that all but 68 g<br />

of a total of 5837 g of the material was transferred<br />

to the loop.<br />

79

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