Two series of ceria zirconia mixed oxide samples with wide variation in the composition were synthesized using homogeneous precipitation with urea and template-assisted hydrothermal procedures. The samples were characterized by nitrogen physisorption, XRD, SEM, Raman, XPS, UV-vis, FTIR, pyridine-FTIR and TPR techniques. The catalytic activity in ethyl acetate total oxidation as a representative of VOCs was tested. The effect of preparation procedure on the texture, structure, morphology, acidic and redox properties was discussed in details in close relation with mixed oxides composition and possibilities for fine tuning of their catalytic activity. As compared to urea procedure, the hydrothermal treatment provides more homogeneous insertion of Zr ions within cubic ceria lattice even at high Zr content. As a result higher degree of distortion of the cubic lattice, creation of Ce3+ and oxygen vacancies and an increase in both Lewis acidity and redox ability is observed and these properties are not affected by the presence of template during the synthesis. The differences in the redox and surface acidic properties of both series of materials probably promote the realization of the catalytic process by various reaction pathways and thus influence in a complex way the catalytic activity and selectivity. (C) 2015 Elsevier B.V. All rights reserved.