Determination of heavy metals such as Cd, Pb and Cu by potentiometric stripping analysis (PSA) in gasoline and dust particulate, was made. Initially optimum pH of the analyte, plating voltage and electrolysis time of the technique was established. The test samples were taken from service station and different locations at Peshawar. High octane blend, regular and super gasoline contained range mean levels of Pb 0.275-0.614 gm L-1 and Cu 0.0042-0.008 gm L-1 while Cd was not detectable. High speed diesel had mean values of Cd 0.003, Pb 0.0038 and Cu 0.023 gm L-1. The dust particulate matter contained maximum levels of 3.92, 84.23 and 49.67 gm Kg-1 of Cd, Pb and Cu respectively depending upon the position on the road-side.