ORNL-1771 - Oak Ridge National Laboratory

ORNL-1771 - Oak Ridge National Laboratory ORNL-1771 - Oak Ridge National Laboratory

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75 UI > S . PERlOD ENDING SEPTEMBER IO, 7954

ANP QUARTERLY PROGRESS REPORT cathode was found to be about 8 amp,/cm2 of nominal gauze area. In all runs under hydrogen, the effluent gas was bubbled through KOH solution to remove HF. A sample of the gas after removal of HF was analyzed by mass spectrometry and found to contain 3.17% CH, 1.25% H,O (from the KQH solution), 0.73% N, and only about 0.02% CF,. Evidently the predominant anode product is HF. The anodes disappeared at a rate corresponding to Q life ex- pectancy longer than 50 ump-hr. The cathode de- posits were expected to contain zirconium metal, and this was qualitatively confirmed by the high zirconium analysis (53.9 wt 5% for the cathode that gained 0.2 g of iron) in the scrapings sf mixed metal and salt from the cathode, However, the zirconium metal could not be distinguished by x-ray diffraction. 76 The conclusion was reached that electrolysis with removable cathodes wus a practical and effi- cient means of purifying fluoride melts containing structural metal impurities. Experiments to investi- gate the removal of sulfates and oxides by elec- trolysis and an attempt to electralytical Iy reduce UF, to UF, are in progress. A typical set of current-voltage curves is shown in Fig, 5.9. These curves apply to the experiment with ternovable cathodes wnd illustrate the churac- teristic “knees” or breaks in the current-voltage curves as the voltage is increased or decreased. The “knees” are apparently due to a polarization phenora-ienon and show considerable hysteresis. A correlation between the current at which breaks occur and the ornpere-hours passed is presented in Fig, 5.10.

ANP QUARTERLY PROGRESS REPORT<br />

cathode was found to be about 8 amp,/cm2 of<br />

nominal gauze area.<br />

In all runs under hydrogen, the effluent gas was<br />

bubbled through KOH solution to remove HF. A<br />

sample of the gas after removal of HF was analyzed<br />

by mass spectrometry and found to contain 3.17%<br />

CH, 1.25% H,O (from the KQH solution), 0.73%<br />

N, and only about 0.02% CF,. Evidently the<br />

predominant anode product is HF. The anodes<br />

disappeared at a rate corresponding to Q life ex-<br />

pectancy longer than 50 ump-hr. The cathode de-<br />

posits were expected to contain zirconium metal,<br />

and this was qualitatively confirmed by the high<br />

zirconium analysis (53.9 wt 5% for the cathode that<br />

gained 0.2 g of iron) in the scrapings sf mixed<br />

metal and salt from the cathode, However, the<br />

zirconium metal could not be distinguished by x-ray<br />

diffraction.<br />

76<br />

The conclusion was reached that electrolysis<br />

with removable cathodes wus a practical and effi-<br />

cient means of purifying fluoride melts containing<br />

structural metal impurities. Experiments to investi-<br />

gate the removal of sulfates and oxides by elec-<br />

trolysis and an attempt to electralytical Iy reduce<br />

UF, to UF, are in progress.<br />

A typical set of current-voltage curves is shown<br />

in Fig, 5.9. These curves apply to the experiment<br />

with ternovable cathodes wnd illustrate the churac-<br />

teristic “knees” or breaks in the current-voltage<br />

curves as the voltage is increased or decreased.<br />

The “knees” are apparently due to a polarization<br />

phenora-ienon and show considerable hysteresis.<br />

A correlation between the current at which breaks<br />

occur and the ornpere-hours passed is presented in<br />

Fig, 5.10.

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