Scientific interest in the processes of forming the structure of magnetic spinels and composites based on them is due to the possibility of synthesis of materials with multifunctional properties. The process of formation of cobalt (II) nanocrystalline ferrite and CoFe2O4/C composite material is studied. The mechanism of formation of structure of materials including a stage of formation of hydroxides of transition elements, precursors on the basis of complex connections of cations of iron and cobalt with citric acid and their subsequent destruction at heating is offered. The synthesized materials were characterized by x-ray phase analysis, electron microscopy, low-temperature nitrogen adsorption, Debye-Scherrer methods. It is shown that cobalt (II) ferrite has a developed surface, the value of the surface area according to the BET method is 16 m2/g, the average size of the crystallites determined by the Debye-Scherrer equation is 4.0 nm. Activated carbon with a specific surface area of 685 m2/g was used to prepare the composite material. The resulting composite material has a surface area of 222 m2/g, the average crystallite size of 1.1 nm. Cobalt (II) ferrite, included in the composition of the composite material CoFe2O4/C, has a slightly higher value of the lattice parameter, compared with pure cobalt (II) ferrite, which is associated with a decrease in the degree of spinel inversion. The synthesized composite material was tested in the process of adsorption of copper (II) cations from an aqueous solution. It is shown that CoFe2O4/C exhibits an increased adsorption capacity for copper (II) cations in comparison with pure activated carbon, despite a decrease in the specific surface area. The result is explained by the involvement of cobalt (II) ferrite in the adsorption process. The obtained materials may be of interest as catalysts, adsorbents.