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In 1992, a Round Robin was sponsored by the CRC's Emissions Analysis Round Robin Subcommittee, to provide an opportunity for automotive emissions laboratories to compare their analytical methodologies with those used in other laboratories. Compressed gas samples were provided to participants to test hydrocarbon methodologies, while liquid samples were used for alcohol and carbonyl analyses. The results of this study were published in SAE 950780 and SAE 941944. A second Round Robin study was conducted in 1995, using the same basic structure as the first study. The results of the carbonyl analyses have been published separately (SAE 971609). The purpose of this paper is to compare methods used for hydrocarbon speciation of emissions by gas chromatography. As in the 1992 study, cylinders of a synthetic exhaust were prepared by using a fuel base, and adding components that would be expected as typical combustion products.