Pyrolysis GC-MS was used to profile residual solids after drying aged whiskey samples. The samples in question were both 20 years old from the same unaged parent distillate but matured in the very different wood species of Quercus Robur and Quercus Alba. Fractionated pyrolysis chromatograms generated at 450°C were obtained for both the different whiskey residues and samples of the respective wood species. The whiskey residues showed differences in peak pattern profiles and the same differences were observed between each residue and it’s originating wood. Pyrolysis GC-MS could be applied to whiskey maturation investigations and can help to establish a link between the spirit non-volatile fraction and the type of wood used for maturation.