A simple method is described for the rapid spectrophotometric determination of molybdenum in samples containing 1-60% Mo, with satisfactory accuracy. Molybdenum is reduced with excess of hydrazine sulphate in boiling 5.5M hydrochloric acid and extracted with isoamyl acetate from 7M hydrochloric acid. The green colour is measured at 720 nm against a reagent blank. Beer's law is obeyed over the range 0.08-5.4 mg of molybdenum per ml. Interference from iron and copper is removed by adding stannous chloride and thiourea respectively in slight excess. Titanium, vanadium, niobium, chromium, tungsten, nickel, uranium, and antimony do not interfere even in large amounts. Only cobalt interferes seriously.