A rapid method for the simultaneous solvent extraction and spectrophotometric determination of hexavalent uranium with N-p-tolylbenzohydroxamic acid is described. The intense red complex with uranium can be extracted by chloroform at ph ∼4. 3. The red colored complex obeys Beer's law at 515 nm. A satisfactory separation from many commonly occurring metal ions is easily accomplished. Effects of acidity, reagent concentration and diverse ions on the visible absorption spectrum of the extracted complex have also been investigated.