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Magnetite (Fe₃O₄) nanoparticles (NP) with sizes between 20 and 30nm have been obtained by Fe electrooxidation in the presence of an amine surfactant, which acted as a supporting electrolyte and coating agent, controlling particle size and aggregation during the synthesis. The effect of different parameters on the nature and size of the particles as well as the mechanism of formation of the particles have been studied by different techniques. It was concluded that, under the electrochemical conditions used in this work, the NP mean size was found to be constant at around 20nm when the electrooxidation current density is increased from 10 to 200mAcm⁻². However, when the potential is over 6V, particle size decreases from 30 to 20nm and metallic iron appears as an impurity. The mechanism of particles formation has being clarified and the critical effect of the distance between electrodes for obtaining magnetic …