Mercury film microelectrodes (MFMs) were used to quantify trace levels of nickel accumulated in mice organs samples after dosing the mice with a physiological solution containing 150 ppm of Ni ions over a period of time, by performing adsorptive cathodic stripping square wave voltammetry (AdSWV). The residues obtained after digestion of the biological organs with nitric acid which affects the electrochemical response of Ni were investigated by XRD and IR spectrometry and found po be mainly composed by p-nitrobenzoic acid. Electrochemical conditions for the quantification of Niwith MFMs in the biological solutions were optimized. The electrochemical data compared favorably with that obtained by atomic absorption spectrometry.