3-Nitro-1,2,4-triazol-5-one (NTO) rubidium and cesium complexes were synthesized by mixing the aqueous solution of NTO and their respective metal carbonates. Their thermal decomposition and the non-isothermal kinetics of the dehydration reaction were studied under the non-isothermal condition by DSC and TG-DTG methods. The kinetic parameters were obtained from analysis of the DSC and TG-DTG curves by Kissinger method, Ozawa method, the differential method and the integral method. The most probable mechanism functions for the dehydration reaction of the title complexes were suggested by comparing the kinetic parameters. The dehydration decomposition reaction of (RbNTOH2O)-H-. and CsNTO.H2O appears to be the same as Avrami-Erofeev equation: f(alpha) = (5/2)(1 - alpha)[-ln(1 - alpha)](3/5), G(alpha) [-ln(1 - alpha)](2/5), n = 2/5. The critical temperature of thermal explosion is 240.88 degrees C for (RbNTOH2O)-H-. and 246.27 degrees C for (CsNTOH2O)-H-.. (c) 2005 Elsevier B.V. All rights reserved.