Modification of carbon electrode with hydroxyapatite (HA) and Bismuth (II) was carried out to enhance Cd2+ and Pb2+ deposition through HA ion-exchange. The interacting ability of the Bi film and HA on the electrode surface was evaluated for simultaneous determination of Cd2+ and Pb2+ using cyclic and square wave anodic stripping voltammetry, at deposition potential of -1.0 V in 0.1M acetate buffer for 240 sec, followed by square wave potential scan from -1.0 V to -0.2V. Stripping voltammogram showed current peaks corresponding to Cd2+ and Pb2+ limit of detection (LOD) of 5 μg/l and consistent up to 150 μg/l. Sensitivity and selectivity of the modified electrodes for Cd2+ and Pb2+ were also determined. © 2013 by ESG.