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This paper is concerned with the demonstration of a methodology for chemically characterizing diesel particulate organic matter (POM) emissions. The procedure begins with a Soxhlet extraction of the POM with dichloromethane to obtain a soluble organic fraction (SOF). The acidic and basic portions of the SOF are isolated by liquid-liquid extraction techniques with aqueous base and aqueous acid, respectively. The neutral portion of the extract is separated into paraffin, aromatic, transitional and oxygenated fractions by column chromatography on silica gel. Two additional fractions, the ether insoluble and hexane insoluble fractions, are also separated by the procedure. Quantitative mass data are presented on the extraction and fractionation of twelve particulate samples from the exhaust of a medium-duty diesel engine collected in a dilution tunnel at a volume dilution ratio of 8 to 1.