Adsorptive catalytic polargraphic wave of the complex of molybdenum(Ⅵ)-8-hydroxy-5-sulfonic-quinoline complex is studied. Its peak potential is-0.30 V(vs,SCE). The optimum conditions are 5.0×10~(-3) mol/L HCl and NaNO_2, the detection limit and linear range of molybdenum(Ⅵ) are 0.1 ng/mL and 0.2~400 ng/mL respectively. Several electron chemical methods are used to prove that a polargraphic wave is a complex adsorptive one. The molar ration of molybdenum(Ⅵ) to 8-hydroxy-5-sulfonic in the complex is found to be 1∶1. The effect of more 8-hyd...