A procedure to determine cadmium, lead, zinc and copper in urban aerosol samples was developed. Differential-pulse anodic stripping voltammetry (DPASV) at a hanging mercury drop electrode (HMDE) was used as the analytical method, and accuracy of the procedure was checked using certified standard solutions. Metal concentrations were calculated from the corresponding regression line using the standard addition method; limits of detection of the four metals were also calculated. Detection and quantification of these metals by DPASV can substitute for other common techniques such as electrothermal atomic absorption spectrometry (EAAS) and inductively coupled plasma – atomic emission spectrometry (ICP-AES) as a confirmatory method.