Carbon rod electrodes (CREs) were obtained from recycled zinc–carbon batteries and were used without further modification for the measurement of trace concentrations of lead (Pb). The electrochemical behavior of Pb at these electrodes in a variety of supporting electrolytes was investigated by cyclic voltammetry. The anodic peaks obtained on the reverse scans were indicative of Pb being deposited as a thin layer on the electrode surface. The greatest signal–to–noise ratios were obtained in organic acids compared to mineral acids, and acetic acid was selected as the supporting electrolyte for further studies. Conditions were optimized, and it was possible to determine trace concentrations of Pb by differential pulse anodic stripping voltammetry. A supporting electrolyte of 4% v/v acetic acid, with a deposition potential of −1.5 V (vs. SCE) and a deposition time of 1100 s, was found to be optimum. A linear range of 2.8 μg/L to 110 μg/L was obtained, with an associated detection limit (3σ) of 2.8 μg/L. A mean recovery of 95.6% (CV=3.9%) was obtained for a tap water sample fortified with 21.3 μg/L.