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Scanning Probe Microscopy (SPM) was used to determine the volume fraction of oil-swollen particulate rubber and oil-swollen plastic in thermoplastic vulcanizates (TPVs) produced from iPP and EPDM rubber. Sample preparation and SPM imaging conditions allowed the ratio of the rubber and plastic area imaged for a TPV sample to be equated to the phase volume ratio. The hydrosilylation cured TPVs contained no filler or inorganic components (other than about 1 ppm of platinum catalyst, based on dry rubber) that would decrease the accuracy of the SPM analysis. The accuracy of the SPM method used for TPV phase volume determination was established by analysis of an oil-free TPV of known composition. The densities of the individual TPV components (rubber, oil, crystalline and amorphous plastic phase), which were assumed to be additive in the composite, were used to calculate the oil distribution between the TPV rubber and plastic phase, since the volumes of the individual components (the extent of plastic crystallinity was measured by differential scanning calorimetry) were known. Thus, the amount of oil in the oil-swollen TPV rubber and plastic phase could be quantified. This information, coupled with the Tg of the oil-swollen amorphous plastic phase, indicated that a substantial amount of oil was present as a separate oil phase that is surrounded by the oil-swollen amorphous plastic phase. To date, it has been assumed that the oil in a TPV partitions between the rubber and amorphous plastic phase, with the plastic crystallites being oil free. This work is the first demonstration of the presence of a separate oil phase in TPVs, and the first accurate determination of the oil content in the oil-swollen rubber, miscible oil in the oil-swollen amorphous plastic, and the free oil in TPVs.