Thermal dehydration and decomposition processes of some intercalation compounds were studied by simultaneous TG/DSC and evolved gas analysis (EGA). gamma-Zirconium and gamma-titanium phosphates were intercalated with 1,10-phenanthroline and subsequently reacted with copper ions to form the complex in situ. Reaction mechanisms for thermal decomposition of all the materials were investigated and proposed according to the mass losses recorded by TG and confirmed by EGA (TG-FTIR). The Ozawa-Flynn-Wall isoconversional method provided dependencies of activation energy on the degree of conversion. A "single point" model-free method was also applied using Kissinger equation and the derived results were compared to those of the former method. (C) 2005 Elsevier B.V. All rights reserved.