In this contribution, the amounts of Ni (nickel) and Al (aluminum) in tilapias (Oreochromis niloticus) were determined using square wave voltammetry (SWV) with glassy carbon working microelectrode with a mercury thin film, platinum counter electrode, and Ag/AgCl reference electrode. Ni was studied through the formation of the dimethylglyoxime-Ni (Ni-DMG) complex, while Al was studied through the formation of the Alizarin R-Al complex. The detection limit found for Ni-DMG and Alizarin R-Al complexes were 1.70 x 10(-7) and 1.0 x 10(-8) mol L(-1), respectively. The voltammetric anodic curves for the Alizarin R-Al complex were recorded over the potential range from -0.8 to -0.05 V while the voltammetric cathodic curve for the Ni-DMG complex was recorded over the potential range from -0.7 to -1.2 V. These methods detected low concentrations of Ni and Al in biological samples efficiently.