A square-wave anodic stripping voltammetric method Is described for low parts per million determination of heavy metals separated by thin-layer chromatography (TLC). Heavy metal samples are separated on carboxymethyl cellulose TLC plates and detected by anodic stripping voltammetry (ASV) using a cellulose dialysis membrane-covered mercury film electrode (CM-MFE) placed directly on the TLC plate surface In a thin film of supporting electrolyte solution. The fast scan rates possible In square-wave voltammetry during the stripping step eliminate the need to deoxygenate the sample. Results are presented for a mixture of Pb(II), Cd(II), Cu(II), and Zn(II). Calibration curves for Pb(II) were linear over the range 10-500 ng, with a relative standard deviation of the peak current over a set of eight separate 100-ng Pb(II) samples of 15%.