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As vehicle tailpipe emission levels decrease with improvements in emission control technology and reformulation of gasolines, exhaust hydrocarbon levels begin to approach the levels in ambient air. Hydrocarbon speciation at these low levels requires high sensitivity capillary gas chromatography methods. In this study, a mixture of “synthetic” exhaust was prepared at two concentration levels (approximately 5 ppm C and 10 ppm C), and was analyzed by the widely-used Auto/Oil Air Quality Improvement Research Program (AQIRP) Phase II (gas chromatography) speciation method with a sensitivity of 0.005 ppm C for individual species. The mixture at each concentration level, along with a sample of ambient air, was analyzed a total of 20 times on 10 separate days over a 2½ week period. Concentrations of total hydrocarbons (HCs) and individual species (using the AQIRP library) were measured; averages and standard deviations were calculated.