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Techniques have been developed to sample and speciate dilute heavy duty diesel exhaust to determine the specific reactivities and the ozone forming potential. While the Auto/Oil Air Quality Improvement Research Program (AQIRP) has conducted a comprehensive investigation to develop data on potential improvements in vehicle emissions and air quality from reformulated gasoline and various other alternative fuels. However, the development of sampling protocols and speciation of heavy duty diesel exhaust is still in its infancy [1, 2, 3, 4, 5 and 6]. This paper focuses on the first phase of the heavy duty diesel speciation program, that involves the development of a unique set of sampling protocols for the gas phase, semi-volatile and particulate matter from the exhaust of engines operating on different types of diesel fuel. Effects of sampling trains, sampling temperatures, semi-volatile adsorbents and driving cycles are being investigated.