The bismuth particles are synthesized via sol-gel route using acetic acid precursor. The prepared nanoparticles have been characterized by X-ray diffractometry, and Fourier Transform Infrared spectrometry. The X-ray diffractometry result demonstrates the synthesized powder has a tetrahedral crystalline structure with particle size of 30.8 nm. Cyclic voltammetry was used to evaluate the electrochemical behavior of the two metal ions at the modified and unmodified electrode. Experimental parameters including carbon paste composition, accumulation potential and accumulation time were investigated. The optimum voltammetric response was observed for a paste composition of 15 mg (BFO to graphite powder in the carbon paste). Accumulation potential of -1.2 V and accumulation time of 180 s were optimized. Under the above optimal experimental conditions the differential anodic stripping voltammetric (DPSV) signal were linearly dependent on the Pb(II) and Cd(II) concentration in the range of (2-200 μM) with determination coefficient (R2 ) of 0.9769 and 0.988 for Pb(II) and Cd(II) respectively. The method also showed low detection limit of 0.03 μM for Pb2+ and 0.06 μM for Cd2+. The analytical application of the developed method was tested on Pb(II) in tap water sample giving a recoveries in the range of the range of 96.2-102 % validating the applicability of the method