The Electrolytic Reduction-pH Control Method of Separation of U From Contaminants Page: 4 of 7
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Synthetic 'gunkt solutions containing 5 percent tuballoy, 0.2 percent iron, .05
percent nickel, and .02 percent chromium as tuballous, ferrous, nickelous and
chromic chlorides when adjusted to pH 4.0 and pH 5.0 contained in the unwashed
precipitates the following proportions of the original constituents:
Precipitated at DH 4.0 Precipitated at pH 5.0
tuballoy.... 99.0 percent tuballoy.... 99.9 percent
chromium.... 100 " chromium.... 100 "
iron........ 20 " iron....... 18 "
nickel...... 15 " nickel...... 14 "
Another wash with hot dilute ammonia would have removed most of the remaining
The presence of so much iron in the precipitate seems to be due to partial air
oxidation of ferrous to ferric hydroxide. Tuballous ion, when tied up as the
hydroxide, apparently will not keep the iron reduced and a scum of ferric
hydroxide forms on the surface. Solutions containing 5 percent tuballoy and
from 0.1 to 0.5 percent ferrous ion, when precipitated at pH 4.5, contained in
the tuballoy precipitate from 50 to 5 percent of the original iron (cf. Figure 5).
The iron in the precipitate seemed to be in the form of ferric hydroxide as in all
cases a reddish-brown scum formed on the surface of the solution. The addition of
'x 0, 0.1, 0.5, and 0.5 percent hydroxylamine to a 5 percent tuballoy solution contain-
ing 0.5 percent iron, reduced the iron content in the precipitate obtained at pH 4.5
from 10 to 9, 4 and 2 percent of the original, respectively. (cf. Figure A). The
maximum loss of tuballoy occurred with the higher percent of hydroxylamine and was
' It seems probable that the extra reducing power of the actual electrolytic solutions,
which contain trivalent tuballoy, will be sufficient to prevent air oxidation of the
iron and this appears to be the case. A solution containing 5 percent tuballoy and
0.25 percent iron electrolytically reduced until a few percent of the tuballoy were
present in the trivalent form, contained only one percent of the original iron in
the tuballous hydroxide precipitate obtained at pH 4.5. However, if the amount of
trivalent tuballoy in the electrolytically reduced solutions is found not sufficient
to keep the iron in the ferrous state when exposed to air, it may be necessary to
add a small quantity of some other reducing agent such as ammonium hyposulfite or
hydroxylamine. The possibility of keeping the solution out of contact with air
while ammonia is being added should also be considered.
Synthetic 'gunk' solutions containing
5 percent tuballoy
0.4 " iron
0.15 " nickel
0.075 " chromium
0.05 " copper
when separated by pH control and washed twice by slurrying with 50 percent aliquots
of two percent ammonium nitrate contained in the precipitate the following percent-
ages of the constituents originally present:
Precipitated at pH 5.5 Precinitated at pH 4.0 Precinitated at BH 4.5
tuballoy.. 96.0 percent tuballoy.. 99.0 percent tuballoy.. 99.6 percent
iron...... 0.0 " iron...... 0.0 ^ iron...... 0.0 "
nickel.... 0.0 " nickel.... 0.0 " nickel.... 0.0 "
chromium.. 82.2 " chromium.. 95.5 " chromium.. 98.8 "
copper.... 0.0 " copper.... 0.0 " copper.... 0.0 "
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Wagner, E. L. The Electrolytic Reduction-pH Control Method of Separation of U From Contaminants, report, July 28, 1943; [California]. (digital.library.unt.edu/ark:/67531/metadc1018392/m1/4/: accessed July 21, 2018), University of North Texas Libraries, Digital Library, digital.library.unt.edu; crediting UNT Libraries Government Documents Department.