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The diffusion of methanol, ethanol and toluene in a Nylon 12 and a poly(vinylidene) fluoride (PVDF) was measured using Fourier transform infrared-attenuated total reflectance (FTIR-ATR) spectroscopy, a technique which allows the quantification of the penetrant concentration diffusing in thin polymer films in situ. Furthermore, it is also possible to study multi-component diffusion using FTIR-ATR provided each component displays unique infrared absorbance peaks. Thin films of a Nylon 12 and PVDF were made by both solvent casting from either 1,1,1,3,3,3, hexafluoro-2-propanol or dimethylacetamide and by cast film extrusion. The films made by the cast film extrusion process had a more uniform thickness than those solvent cast. The diffusion coefficients of methanol, ethanol and toluene in Nylon 12 and PVDF were determined gravimetrically and by the FTIR-ATR technique. Both methods afforded comparable diffusion coefficients for similar solvent-polymer systems.