Volumetric determination of uranium using titanous sulfate as reductant before oxidimetric titration

Trace Elements Investigations 614
This report concerns work done on behalf of the Division of Raw Materials of the U.S. Atomic Energy Commission
By: , and 



A new method for determining uranium in samples containing 0.05 percent or more U3O8, using titanous sulfate as reducing agent, is much shorter, faster, and has fewer interferences than conventional methods using reductor columns.

The sample is dissolved with sulfuric, nitric, perchloric, and hydrofluoric acids. Elements that would otherwise form insoluble fluorides are kept in solution by complexing the fluoride ion with boric acid. A precipitation is made with cupferron to remove interfering elements. The solution is filtered to remove the precipitated cupferrates instead of extracting them with chloroform as is usually done. Filtration is preferred to extraction because any niobium that may be in solution forms an insoluble cupferrate that may be removed by filtering but is very difficult to extract with chloroform.

Excess cupferron is destroyed by oxidizing with nitric and perchloric acids, and evaporating to dense fumes of sulfuric acid. The uranium is reduced to U(IV) by the addition of titanous sulfate, with cupric sulfate used as an indicator of the completeness of the reduction. Metallic copper is formed when all the uranium is reduced. The reduced copper is then reoxidized by the addition of mercuric perchlorate, an excess of ferric sulfate added, and the solution titrated immediately with standard ceric sulfate with ferroin as an indicator.

Precision of the method compared favorable with methods in common use, both for uranium ores and for most types of uranium-rich materials.

Publication type Report
Publication Subtype USGS Numbered Series
Title Volumetric determination of uranium using titanous sulfate as reductant before oxidimetric titration
Series title Trace Elements Investigations
Series number 614
DOI 10.3133/tei614
Year Published 1956
Language English
Publisher U.S. Geological Survey
Description 20 p.
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