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Although much has been learned in recent years about the atmospheric reactivity of the hydrocarbon (HC) emissions from gasoline-fueled vehicles, there is only a limited database of corresponding information for exhaust emissions from diesel-fueled vehicles. An assessment of exhaust reactivity requires “speciation”, or measurement of the individual species of the HC fraction. The HC exhaust emissions are a complex mixture of unburned and partially burned fuel components. Because diesel fuel contains a much higher molecular weight range (typically C9-C26) than gasoline (typically C5-C12), new methodology was required to accommodate the collection and analysis of the >C12 fraction of the HC exhaust. As part of a study of the effects of fuel and other factors on the chemical nature of diesel emissions, we have developed a method for the collection and analysis of the semivolatile or heavy HC (>C12) fraction of the exhaust.