Rare earth complexes ofm-nitrobenzoic acid (LnL3·2H2O,Ln=La-Lu and Y, except Pm, HL=m-nitrobenzoic acid) were synthesized and characterized by elemental analysis, chemical analysis, IR spectroscopy and X-ray diffraction analysis. The dehydration behaviour of these complexes was studied in detail by means of TG-DTA and DSC. Dehydration occurs over the temperature range 76–215°C, and the temperature of formation of the anhydrous complexes decreases with increasing atomic number of the rare earth. The activation energies and enthalpy changes for te dehydration were obtained.