A miniature glow discharge atom reservoir has been designed for laser excited atomic fluorescence spectrometric measurements of nanoliter-sized solution residues. A copper vapor laser pumped dye laser was used to measure the fluorescence of (\mathrm{Pb}) atoms sputtered from the (\mathrm{Ni}) cathode of the discharge. Excitation of (\mathrm{Pb}) occurred at (283.3 \mathrm{~nm}), and fluorescence was monitored at (405.8 \mathrm{~nm}). The optimal discharge operating pressure and current were 5.5 Torr and (20 \mathrm{~mA}) with continuous fill gas introduction. No improvement was found in (\mathrm{S} / \mathrm{N}) with stop flow versus flowing operation; however, considerable improvement in the (\mathrm{S} / \mathrm{N}) was achieved when gated peak integration, in contrast to peak detection, was employed. The temporal profiles indicated that the (\mathrm{Pb}) atoms were rapidly sputtered from the surface of the cathode and that a high percentage of these atoms diffused back toward the cathode. The redeposition of the (\mathrm{Pb}) atoms led to peak tailing with signals lasting more than (60 \mathrm{~s}). In effect, atoms were sputtered, atomized, and excited several times during a measurement. The limit of detection for (\mathrm{Pb}) was (0.6 \mathrm{pg}) based on peak detection and (0.03 \mathrm{pg}) based on peak area measurements. These detection limits were several orders of magnitude higher than the theoretical, intrinsic detection limit due to the interfering background emission of molecular impurities, such as (\mathrm{N}{2}) and (\mathrm{H}{2} \mathrm{O}), present in the discharge. ol 1995 Academic Press, Inc