The objective of this study is to investigate the efficient method to maximize both color and TOC removal of the azo dye solution by reduction and oxidation with a laboratory synthesized nano-sized zero valent iron (nZVI). The decolorization efficiency increased with the decrease of pH and increase of zero valent iron dosage. The optimum dosage of nano-sized zero-valent iron was 20mg/L at pH 3. The surface normalized constant of nZVI was higher than those reported for the discoloring of azo dye with other ZVIs. The sequential dose of nZVI/H2O2 remove color and TOC more effectively than the simultaneous dose. Pre-reduction by nZVI could convert azo dye to products whose oxidation is more degradable and therefore enhances the removal efficiency.