In this paper the authors present the experimental results of the thermal analysis of heteropolynuclear coordination compound [Co2NiL3(OH)(3)(H2O)(3)](n), where L is lactate anion, obtained by a new method, through the reaction of 1,2-propanediol with M(NO3)(2)center dot 6H(2)O (M: Co, Ni). The reaction between 1,2-propanediol and M(NO3)(2)center dot 6H(2)O (M: Co, Ni) occurs with the oxidation of 1,2-propanediol to the lactate anion (L), coordinated to M(II). The thermal properties of the synthesized polynuclear coordination compound, [Co2NiL3(OH)(3)(H2O)(3)](n), have been investigated by TG, DTG and DTA. The mixed oxide of spinel type, NiCo2O4, impurified with NiO, obtained by thermal decomposition of heteropolynuclear coordination compound was characterized by IR spectroscopy, X-ray powder diffraction (XRD) and elemental analysis. (C) 2008 Elsevier B.V. All rights reserved.