Thermal analysis (TGA and DTA) of samples of PAA, PVP, PAA-PVP complexes, containing different weight fractions of PAA and ternary polymer-metal-polymer complexes, were studied. The activation energy parameters for the thermal degradation were also calculated. The study of the effect of FeCl3, NiCl2, and Ni(NO3)(2) on the TGA and DTA curves of the complexes showed that the decompositions are dependent on the concentrations and the nature of the metal ions. The DTA traces of PAA-PVP complex containing FeCl3, NiCl2, and Ni(NO3)(2) showed that the treatment of the complex with these metal ions causes considerable changes in the thermal decomposition of PAA-PVP complex. (c) 2006 Wiley Periodicals, Inc.