The Electrolytic Reduction-pH Control Method of Separation of U From Contaminants Page: 1 of 7
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" Washington 25, D. C. 7/17L c515
The Electrolytic Reduction - pH Control Method of Separation
of T from Contaminants
E. L. laener
Recent consideration of the electrolytic means of reduction in conjunction with
the pH-control method of separation has led to this preliminary report.
The electrolytic reduction, as now employed, is carried out on an acid chloride
solution in a water-jacketed glass cell with an agitated mercury pool cathode
and a graphite anode. The anode is surrounded by a porous alundum cup which
prevents the liberated chlorine from contacting the tuballous ion and reoxidizing
it to tubanyl ion. This cell, using a current density of 0.3 ampere per square
centimeter at ten volts, reduces about 60 grams of tuballoy, in a 5 percent solu-
tion, per hour. Another cell, now in the process of development, built of
different geometry for continuous operation will, at the present time, reduce
between 500 and 600 milliliters of 5 percent tuballoy solution (25 to 30 grams of
tuballoy) per hour with a current density of about 0.1 ampere per square centi-
meter at 3.5 volts. The solutions from these cells will contain varying amounts
of trivalent tuballoy, up to 25 percent in the batch reductions and 1 to 5 percent
in the continuous operating cell.
* The pH-control method of separation in this case consists of adjusting the pH to
the value to be used on the reduced chloride solution of the metallic constituents.
The solution will consist mainly of tuballous ion, ferrous ion, chromic (and
chromous) ion, nickelous ion, with smaller amounts of trivalent tuballoy, copper,
manganese, molybdenum, etc., all mainly as the chlorides.
Previous experience with this method has shown that chromium will not be separated
under these conditions of precipitation at pH 4.5. It was hoped that precipita-
tion at a low enough pH could be used such that a good tuballoy recovery might be
obtained and that the Aajority of the chromium would remain in the filtrate. The
loss of tuballoy from a 4 percent solution precipitated at pH 3.5 is 0.8 percent,
at pH 4.0 the loss is .02 percent, and at and above pH 4.5 the loss is not detect-
qble by gravimetric means of analysis for tuballoy. (cf. Figure 1) Apparently,
then, it is possible to lower the precipitation pH without too great a buballoy
loss. The precipitate obtained at and below pH 3.0 at room temperature is so un-
filterable that not enough filtrate could be obtained for analysis. The filtra-
tion time at pH 3.5 is seven times that at pH 4.5 and three times greater than at
pH 4.0 with precipitations at higher pH values even shorter filtration times are
obtained. (cf. Figure 2, curve A) Heating such precipitates appears to give a
less hydrated and more filterable form and it may be that the filtration diffi-
culty can to a large degree be eliminated by this means. However, when 'gunk'
solutions are precipitated at these lower pH values, the precipitate obtained is
considerably more filterable than with tuballoy solutions alone (cf. Figure 2,
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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/m1/1/: accessed September 26, 2018), University of North Texas Libraries, Digital Library, digital.library.unt.edu; crediting UNT Libraries Government Documents Department.