Cyclic voltammetry behaviors on the graphite electrode at different vanadium ion concentration, H₂SO₄ concentration, scanrate, additives has been studied by electrochemical methods. The conclusion shows that the characteristic peak of V(Ⅳ)/V(Ⅴ) redox couples has appeared. The higher the concentration of the H₂SO₄ and the scan rate are，the bigger the peak current is. But the increasing of the electrolytic liquid concentration makes the peak current decreased and there is no influence for adding additives. Cyclic voltammetry behavior on the graphite electrode at different heating temperature and the reversibility of both activated and non-activated graphite electrode has also been studied. The result indicats that heating treatment could increase activation of the graphite electrode surface and the activation treatment could not improve reversibility of V(Ⅳ)/V(Ⅴ) redox couples. However, it could enhance the reversibility of V(Ⅲ)/V(Ⅱ) redox couples.