A procedure for the determination of gallium by differential pulse adsorptive stripping voltammetry (DPADSV), using different complexing agents (ammonium pyrrolidine dithiocarbamate (APDC), pyrocatechol violet (PCV) and diethyldithiocarbamate (DDTC)), has been optimized. The selection of the experimental conditions was made using experimental design methodology. Under these conditions, the calibration was made and the detection limit was determined for each gallium-ligand complex. A robust regression method was applied which allowed the elimination of anomalous points. The detection limit, with alpha=beta=0.05, for gallium-APDC complex was 5.0x10(-8)moldm(-3), for gallium-PCV complex was 9.9x10(-9)moldm(-3), and the lowest detection limit (1.3x10(-9)moldm(-3)) was obtained with DDTC. For this reason, DDTC was selected for the determination of the gallium concentration in a certificate sample and in a spiked tap water sample. The linear dynamic range for gallium-APDC complex was from 5.0x10(-8) to 2.7x10(-7)moldm(-3), for gallium-PCV complex was from 5.0x10(-9) to 4.8x10(-7)moldm(-3), and for gallium-DDTC complex was from 1.0x10(-9) to 2.1x10(-7)moldm(-3).