Variable-temperature (VT) solid-state 19 F NMR spectroscopy with high-speed magic-angle spinning (MAS) has been used to study copolymers of vinylidene fluoride and hexafluoropropylene and of vinylidene fluoride and chlorotrifluoroethylene, and terpolymers of vinylidene fluoride, tetrafluoroethylene, and hexafluoropropylene. High-resolution spectra were obtained by simultaneously using MAS speeds up to 25 kHz and heating to 250°C. Sufficient resolution was achieved to assign peaks by comparison to results obtained from solution-state NMR studies and to determine the monomer composition of the polymer.