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In this study, polymer–graphite oxide (GO) interactions are demonstrated to induce thermal instability in both the polymer and GO phase in conditions of maximum polymer uptake, in which the polymer chains are either intercalated into the GO interlayer or adsorbed on the GO sheets. We investigate the thermal stability of poly(ethylene oxide) (PEO) intercalated in GO (PEO/GO) in detail, using a combination of techniques including X-ray diffraction (XRD), thermogravimetry (TGA) and TGA–mass spectroscopy (TGA–MS) in dynamic (nonisothermal) and static (isothermal) modes. Our results show that intercalated PEO decomposes at 160 °C lower than neat PEO, and that GO decomposes at 50 °C lower than pristine GO, due to a synergistic instability between GO and intercalated PEO upon heating. Other hydrophilic polymerssuch as poly(vinyl methyl ether) (PVME), poly(vinyl alcohol) (PAA), poly(vinylpyrrolidone …