Thermal analysis of some transition metal ferrimaleate precursors, M3[Fe(mal)3]2·xH2O (M=Mn, Co, Ni, Cu) has been studied in static air atmosphere from ambient to 600°C. Various physico-chemical techniques, i.e. TG, DTG, DTA, XRD, IR, Mössbauer spectrometry, have been employed to characterize both the intermediates and final products. After dehydration the anhydrous precursors undergo decomposition to yield an iron(II) intermediate, M[FeII(mal)2] (M=Mn, Co, Ni, Cu) in the temperature range 160-275°C. A subsequent oxidative decomposition of iron(II) species leads to the formation of α-Fe2O3 and MO in the successive stages. Finally a solid-state reaction occurs between the oxides above 400°C resulting in the formation of transition metal ferrites, MFe2O4. The ferrites have been obtained at much lower temperature and in less time than in the conventional ceramic method.