RI 4882 Volumetric Determination of Small Quantities of Uranium - With Special Reference to Errors Associated with Use of Jones Reductor (2b4914c2-e697-47ab-9da8-dccd8a6cadf8)

"INTRODUCTION In the usual volumetric determination of uranium, the solution containing uranium is reduced in a Jones reductor, yielding a mixture of trivalent and tetravalent uranium; the trivalent uranium is oxidized to the tetravalent state by bubbling a stream of air through the solution. The resulting solution of tetravalent uranium is titrated with a standard oxidant, generally sulfatoceric acid, dichromate, or permanganate. It seemed likely that the same general procedure could be used in determining semimicro quantities pf uranium if the conditions affecting the variables involved were understood more clearly than at present. In the method described below, the use of ferric sulfate to oxidize tetravalent uranium allows the titration to be made at room temperature in an essentially colorless solution with sulfatoceric acid. The latter oxidant in turn permits the use of the very stable indicator, ferroin; with its sharp color change and exactly reproducible blanks.Solutions of uranyl sulfate were prepared by diluting a stock solution that had been standardized gravimetrically according to the method of Lundell and Knowles (8).3/ Solutions of sulfatoceric acid were prepared according to the directions of G. F. Smith (12) and were standardized against arsenic trioxide in the presence of osmic acid according to the directions of Glen (5). The cerium solutions were stored in 18-liter carboys fitted with siphon arrangements so that the bottles did not need to be opened and protected from light in a dark cupboard. Under these conditions, even the 0.01 N solution changed by less than 1 part per thousand over a period of about 6 months."