Small-volume measurements of lead and cadmium have been accomplished using a mercury-coated nanoband electrode. The band electrodes are fabricated from ultrathin carbonized polyacrylonitrile films. The coupling of the inherent sensitivity of stripping analysis, with submicroliter sample volumes and enhanced plating efficiency (due to enhanced diffusional flux) results in remarkably low detection limits of 100 femtograms (5 x 10(-16) mole) lead. To our knowledge, this detection limit is significantly lower than previously reported values for electrochemical stripping work. Air-saturated quiescent sample droplets can thus be assayed by the square-wave or potentiometric stripping modes. Variables influencing the stripping response are explored and the stripping performance is characterized. Applicability to direct measurements of lead microliter blood samples is illustrated.