Abstract: Transfer behavior of nickle ion extracted electrochemically by 2,2′-bipyridine at the water/nitrobenzene interface has been investigated by cyclic voitammetry. The preceding or following chemical reaction was coupied to the electrolytic transfer process,respectively. The extracted species are successive complexes between Ni(Ⅱ) and 2,2′-bipyridine An irreversible phenomenon similar to that observed at the metal electrode/electrolyte solution interface was observed directly. Voltam metric behaviors with coupled chemical reactions have been discussed.