Abstarct: The performance of glassy carbon electrodes (GCEs) coated with poly(pyrocatechol violet) -multiwalled carbon nanotube (MWCNT–CO–PCV) composite was investigated in the simultaneous determination of cd2+ and pb2+ ions in a 0.1 M acetate buffer solution at pH=5.0 using Differential pulse anodic stripping voltammetry (DPASV). The presence of the bismuth film improves the sensitivity and reproducibility of electrode. It was found that the MWCNT–CO– PCV coated electrode shows a better performance than the bare GCEs. Several parameters such as pH, deposition potentials, deposition time, sweep rate and pulse amplitude affecting the stripping current response were investigated and optimized. Under optimal conditions, the electrode showed a good linear response to cd2+ and Pb2+ in the concentration range of 1.0 – 300.0 µg.L-1 and 1.0 – 200.0 µg.L-1, respectively. The detection limits were 0.09 µg.L-1 for cd2+and 0.327 µg.L-1 for pb2+. The effects of interferences ions were studied and it was found that the sensor has least interference from most of the common ions due to specific and selective interaction of the modifier functionalities with lead and cadmium ions.The response of the electrode remained constant for at least 3 weeks of successive operation.The proposed method was applied for simultaneous determining cd2+ and pb2+ contents in real water samples.