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A dilution source sampling system has been incorporated into the exhaust measurement system of a research single-cylinder diesel engine. To allow more detailed assessment of the individual chemical components of the diesel particulate matter (PM) the exhaust dilution system includes a residence time chamber (RTC) to allow for residence times of 30 to 60 seconds in the second stage of dilution before sampling. Samples are collected on a range of different filters where mass loading, elemental and organic carbon (ECOC), trace metals, sulfate ions (SO4), particle-phase organic compounds, and semi-volatile organic compounds are evaluated. In addition, particle size distributions have been determined using a scanning mobility particle sizer (SMPS). Results show that the chemical composition of the particulate matter is highly dependent on the engine operating conditions.