Abstract: A new method for degradation of 1-naphthylamine by glow discharge electrolysis is proposed. The degradation process was examined by using ultraviolet (UV) absorption spectrum and high performance liquid chromatography (HPLC). The chemical oxygen demand (COD) of sample was also measured. The results showed that 1-naphthylamine can be removed completely within 40 min in the absence of Fe2+ and within 2 min in the presence of Fe2+. The optimum voltage used was at 600 V. The concentration of Fe2+ ion and the pH of solution exhibit an appreciable effect on the degradation rate. The COD of degradation sample was even higher than the original sample. This is because the benzene rings or naphthalene rings were destroyed and some organic acids were produced in this process.