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Extraction of U(IV) by an organic phase containing 30% tri-n-butyl phosphate (TBP) in dodecane from aqueous nitric acid solution containing large amount of U(VI), relevant to nuclear fuel reprocessing by PUREX process, was studied. While acquiring distribution data, an argon atmosphere was maintained. A potentiometric method was used for the determination of U(IV) in the two phases after equilibration. Hydrazine used as stabiliser of U(IV) in the stock solution was destroyed and sulphamic acid was added just before equilibration to avoid the interference due to hydrazine in the subsequent determination of U(IV). Uranium(IV) distribution data between 30% TBP in dodecane and aqueous solution of uranium(VI) and nitric acid of varying concentrations have been presented and compared with available literature data.