Studies of the non-isothermal decomposition of Pb0.25Ba0.75(TNR).H2O (TNR= 2.4.6-trinitro-1,3-dihydroxy-benzene) were carried out by means of TG-DTA, DSC and IR techniques. The thermal decomposition mechanism and the associated kinetics have been investigated. The kinetic parameters were obtained from the analysis of the DSC curves by integral and differential methods. The most probable kinetic model function of the dehydration reaction of Pb0.25Ba0.75(TNR).H2O were suggested by comparison of the kinetic parameters. (C) 2004 Published by Elsevier B.V.