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ORNL-1816 - the Molten Salt Energy Technologies Web Site

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P<br />

as its chief impurity about 0.2 wt % sulfur. Purification<br />

of <strong>the</strong> RbF has proved to be difficult due to<br />

attack of <strong>the</strong> nickel purification equipment by <strong>the</strong><br />

sulfur. It has been found possible by rigorous HF<br />

5<br />

f and H, treatments to reduce <strong>the</strong> sulfur content to<br />

0<br />

- t<br />

.- %.<br />

an acceptable value, but in <strong>the</strong> process a large<br />

amount of nickel is picked up by <strong>the</strong> melt. Con-<br />

siderable treatment time is required to reduce <strong>the</strong><br />

resulting nickel fluoride so that it may be removed<br />

from <strong>the</strong> product.<br />

Preparation of Various Fluorides<br />

B. J. Sturm E. E. Ketchen<br />

structural metal fluorides and several complex<br />

from <strong>the</strong>se and alkali<br />

ed. These materials a<br />

fluorinated UF, are being utilized at increasing<br />

rates for various investigations of interest to <strong>the</strong><br />

ANP program. Chemical analysis, supplemented<br />

by x-ray and petrographic examination, has been<br />

utilized to determine purity and identity of <strong>the</strong><br />

materials.<br />

Uranium tetrafluoride, as received, may contain<br />

small amounts of oxides, moisture, and higher-<br />

ce uranium, Hydrofluorination at 6OOOC is<br />

carried out as a satisfactory method of re-<br />

P moving <strong>the</strong>se impurities. During <strong>the</strong> quarter, 11 kg<br />

of <strong>the</strong> purified material was supplied for studies<br />

requiring high-purity UF,. Additional batches of<br />

NiF, were prepared by <strong>the</strong> hydrofluorination at<br />

6OOOC of partially dehydrated NiCl ,*6H,O. Anhydrous<br />

AIF, was prepared by <strong>the</strong> <strong>the</strong>rmal de-<br />

c<br />

,.<br />

PERIOD ENDING DECEMBER 70,1954<br />

Fluorination of NiF,, CrF,, and FeF, has been<br />

discontinued because <strong>the</strong> analytical [methods<br />

available are not able to establish <strong>the</strong> fluorine-to-<br />

metal ratios accurately enough to determine <strong>the</strong><br />

effectiveness of <strong>the</strong> BrF, treatment in r'emoving<br />

small amounts of oxides that may be present.<br />

CHEMISTRY OF ALKALI HYDROXIDES<br />

L. G. Overholser F. Kertesz<br />

Materials Chemistry Division<br />

Purification of Hydroxides<br />

E. E. Ketchen<br />

Materials Chemistry Division<br />

Approximately 5 kg of NaOH was purified ei<strong>the</strong>r<br />

by filtering a 50 wt % aqueous solution through a<br />

fine sintered-glass filter or by decantinci a 50%<br />

solution to remove insoluble Na,CO,. 111 ei<strong>the</strong>r<br />

case <strong>the</strong> material was <strong>the</strong>n dehydrated at 400OC.<br />

Both methods produced material of desired purity<br />

(-0.1 wt % each of H,O and Na2C03). About<br />

1.8 kg of high-purity KOH (-0.1 wt % each K,CO,<br />

H,O, and Na) was prepared by reacting pure po-<br />

tassium with water, It is not planned to prepare<br />

more hydroxides in <strong>the</strong> near future because <strong>the</strong><br />

material on hand should supply <strong>the</strong> present limited<br />

requirements.<br />

Effect of Additives on Hydrogen Pressure<br />

Over NaOH-Ni System<br />

F. A. Knox<br />

Materia I s Chemistry Di vis ion<br />

The effects of small additions of NiO, Na,O,<br />

and mixtures of <strong>the</strong> two on <strong>the</strong> hydrogen pressure<br />

by using a modification rev i ou s I y desc r i bed<br />

<strong>the</strong> formation of<br />

Three batches of FeF, were fluorinated as a<br />

,,ANP Quar. Prog. Rep. Sept. 10, 1953, <strong>ORNL</strong>-1609,<br />

means of removing small amounts of impurities. p 84.<br />

71

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