A nanocrystalline pyrolytic carbon film was employed as working electrode to detect micromolar-level concentrations of lead by anodic stripping voltammetery as an example of its potential applications in environmental analysis. The response was compared with conventional carbon-based electrodes such as glassy carbon, edge-plane pyrolytic graphite, and basal-plane pyrolytic graphite electrodes. The favorable properties of this carbon coating for Pb detection lie in its high degree of sensitivity, high response stability, low memory effect, and a good repeatability. The applicability of this sensor was tested on spiked tap water and river water samples.