Abstract:After dried with perchloric acid to get rid of the easy-volatile components and organic matter, in a base solution of sulfuric acid-mandelic acid-Sodium chlorat, the complex of Mo(Ⅵ) with mandelic acid showed a sensitive catalytic polarogrphic wave. Based on this fact, a method of catalytic polarogrphic for the determination of trace amount of Mo(Ⅵ) has been put forward. Good linearity was obtained between the peek heights and concentration of Mo(Ⅵ).The detection limit is 0.5μg/L, values of recovery are 91.30%~103.65%, the ralative standard deviation is 9.13% after 10 times test of standard materials. The analyzing results are accordance with standard values.