A simple, sensitive and selective spectrophotometric method for determination of molybdenum is described. A solution containing 100 mug of Mo in 2.5M hydrochloric acid is treated with ascorbic acid and ammonium thiocyanate and after standing for 8 min is shaken with an equal volume of ethyl methyl ketone for 30 sec. The absorbance of the complex is measured at 465 nm against a reagent blank. The complex is stable for 1 hour. There is no interference from Re(VII), SO(2-)(4), Cl(-), CH(3)COO(-), PO(3-)(4), NO(-)(3), C(2)O(2-)(4), citrate or tartrate, and at least 5 mg of U(VI), 10 mg of Cr(III, VI), Th, or Ni, and 20 mg of W(VI) Can be tolerated. Vanadium(V) interferes at the 500 mug level, and fluoride slightly decreases the absorbance.