Studies of factors affecting uranium determinations by automated coulometric titration (New Brunswick Laboratory/Davies--Gray Method)

The method's errors are defined to ascertain its absolute accuracy. An analytical technique was developed to examine vanadyl sulfate diluent for vanadium (V). None could be found in any of the lots tested. Certain lots of reagent-grade phosphoric acid contained an unidentified impurity that caused high generator-electrode potentials and a positive error. The current-potential characteristics of the generator electrode were measured. The data indicated that a significant fraction of uranium (IV) was oxidized directly during the early stages of titration. Using equations theoretically applicable to such a titration, a negligible difference was found between the inflection point of the titration curve and the equivalence point in the titration. However, the actual experimental curves did not agree with the theoretical curves early in the titration. Measurements of the background current indicated a level equivalent to approximately 0.2 mg uranium. The evaluation of the reagent delivery system used in the automated analyzer revealed adequate reproducibility. 8 tables