Electrodeposition of Pb from electrolyte containing CH3COONH4, CH3COOH, and Cl- was in-vestigated at 25 ‡C in stirred and quiescent solutions on different substrates: Pb, Cu, Al, and C. The deposited lead from the acetate bath was crystalline and showed a marked tendency to form dendrites. The addition of organic additives, phenol, ethyl alcohol, and gelatine, was found necessary in order to obtain a bright, smooth, and compact lead deposit on Pb and Cu electrode. Even with the additives, dendritic lead was observed on Al and C electrodes. Systematic studies of electrodeposition of Pb from these media—such as investigation of the effect of concentration of chemicals in the electrolyte, the effect of temperature, the effect of current density, and the nature of the subtrates—were carried out. Electrochemical techniques such as cyclic voltammetry, potentiodynamic studies, chrono-amperometry, and chronopotentiometry have been employed to shed light on the nature of the reaction mechanism. The deposit quality and purity was examined by X-ray diffraction analysis, SEM, and Auger spectroscopy. The results were compared with those obtained from a fluoborate bath. The quality of a lead deposit from fluoborate bath proved to be similar to that obtained from acetate bath in the presence of organic additives where the deposit was always of a compact, dense, and smooth form.