Polychelates were synthesized by the addition of aqueous solutions of copper(II), cadmium(IT), and nickel(II) chlorides to aqueous solutions of poly(maleic anhydride-alt-acrylic acid) [poly(MA-alt-AA)] in different pH media. The thermal properties of poly(MA-alt-AA) and its metal complexes were investigated with thermogravimetry and differential scanning calorimetry (DSC) measurements. The polychelates showed higher thermal stability than poly(MA-alt-AA). The thermogravimetry of the polymer-metal complexes revealed variations of the thermal stability by complexation with metal ions. The relative thermal stabilities of the systems under investigation were as follows: poly(MA-alt-AA)-Cd(II) > poly(MA-alt-AA)-Cu(II) > poly(MA-alt-AA)-Ni(II) > poly(MA-alt-AA). The effects of pH on the complexation and gravimetric analysis of the polychelates were also studied. (c) 2006 Wiley Periodicals, Inc.