Department of Chemistry, Govt. Polytechnic College. Ujjain (M.P.), India Manuscript received 6 April 1976: accepted 10 November 1976 A rapid method for the simultaneous solvent extraction and spectrophotometric determination of micro amounts of hexavalent molybdenum with benzohydroxamic acid is described. The intense yellow-greenish coloured complex thus extracted from hexanol at pH 2.0 absorbs at around 370 nm. A clear cut separation from many commonly occurring metal ions is easily accomplished. Effect of acidity, reagent concentration and diverse ions on the visible absorption of the extracted complex have also been investigated.