Chemical Stability of Purex and Uranium Recovery Process Solvent Page: 4 of 16
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(5) Impurities isolated chromatographically from refluxed Shell
Spray Base when added (at the four per cent level) to "as
received" Shell Spray Base, 20 per cent in TBP, caused
markedly increased fission product retention in the organic
phase after one extraction contact followed by three scrub
(6) A partial chromatographic analysis followed by infrared
(a) Products isolated from Shell Spray Base are similar
to those found in Uranium Recovery Process RCW.
(b) Soltrol 170 yields products similar to those from
Shell Spray Base, but higher in nitroso compounds.
(c) Methyl cyclohexane* yields organic acids, nitrite
esters, and nitro compounds. At least ten discrete
colored bands, each indicative of a single substance,
were resolved on the alumina column. Time did not
permit their complete isolation and identification,
but these observations give some insight into the
complexity of the analytical problem of analyzing
diluents for impurities.
B. Chemical Stability at 71 C
(1) Effect of Nitrous Acid
Actual boiling of aqueous-organic systems is a condition never
anticipated in Purex columns, though had the solvents proved
stable, chemical effects at lower temperatures could hardly be
of consequence. Close observation of the refluxing systems
revealed that the reaction was slow at first but accelerated
in later stages with accompanying evolution of nitrogen oxides.
This suggested the possibility that nitrous acid was participating.
To check this point under less stringent conditions, samples were
placed in flasks equipped with stirrers and condensers and immersed a
in a bath at 71 C. Two volumes of aqueous to one of organic were
used with mild stirring at the interface. Samples were taken at
intervals and measured spectrophotometrically. A final sample
was taken for the remaining tests. These data are recorded in
It is evident from these data that as little as 0.01 M NO2 has
a marked effect in accelerating the decomposition of the solvent.
In the absence of nitrite ion, the diluent or solvent appears to be
*The sample employed was chromatographed on silica gel until spectrophotometrically
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Moore, R. H. Chemical Stability of Purex and Uranium Recovery Process Solvent, report, March 1, 1955; Richland, Washington. (digital.library.unt.edu/ark:/67531/metadc1017318/m1/4/: accessed July 19, 2018), University of North Texas Libraries, Digital Library, digital.library.unt.edu; crediting UNT Libraries Government Documents Department.