The thermal degradation of poly(methyl methacrylate) (PMMA) in the presence of iron(II) chloride, iron(III) chloride, copper(I) chloride, copper(II) chloride, and nickel(II) chloride has been studied by the combined technique of thermogravimetric analysis coupled to a Fourier transform IR spectrometer. In those cases where coordination occurs between the transition metal ion and the carbonyl oxygens of the polymer, there is an effect on the degradation of the polymer; in those cases where coordination does not occur, the degradation is unaffected by the presence of the additive. The presence of methyl chloride as one of the gases evolved is diagnostic for a coordination; when this gas is absent, the degradation of the PMMA proceeds unaffected by the presence of the transition metal ion.