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The two dimensional separation of low molecular weight polystyrene oligomers and stereoisomers was achieved using a liquid chromatographic system designed for ‘heart-cutting’ multidimensional chromatography. The first separation process incorporated a C18 column and a methanol mobile phase to separate the oligomers, whilst the second separation process utilised the change in selectivity associated with a carbon clad zirconia stationary phase and an acetonitrile mobile phase for the separation of the isomers. The two dimensional separation that was achieved using this automated system was comparable to the individual separations following manual sample manipulation in each individual separation step. Furthermore, the multidimensional LC system was shown to be highly reproducible in routine continuous operation over an eight hour period.