A simple, rapid and interference free spectrophotometric method for the determination of micro amounts of molybdenum (V) is reported The method is based on the quantitative extraction of Mo(V) by 0.05 M 2-benzylpyridine (BPy) solution in benzene from 3 M HCl solution containing 1 M thiocyanate and 0.4 M ascorbic acid The maximum absorption of Mo(V)-SCN-BPY complex in benzene occurs at 470 ma The Beer's law is obeyed in the concentration range 0.2-2 mug/g. The molar absorptivity and Sandell's sensitivity of the benzene extracted complex is 1.76x10(4) M-1 cm(-1) and 5.4x10(-4) mug cm(-2) respectively. The effect of foreign ions has been studied. The method permits the determination of molybdenum in presence of commonly associated elements.