Abstract: The conditions of the determination of gold were studied on glass carbon electrode by the anodic stripping voltammetry(ASV).The experiments showed that in the optimum electrolytic system of 0.lM HCl-1.4×10^-6M HgCl₂, there was a stable stripping peak for Au at about + 0.8V (vs. S.C.E). Its determination limit reached 5 ppb. By adopting of cotton cellulose xanthate (CCX) for entichment, the separation of Au achieved good results.This method was used for some practical sample analyses with good results. The coefficient variation was 0.73% and 2.53% respectively when two gold samples were repeatedly determined for 7 times.