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A novel Fast Response Chemiluminescence Detector and a Fast Flame Ionization detector have been used to examine the instantaneous NO and unburnt hydrocarbon concentration in the cylinder and exhaust port of a DI Diesel engine. The in-cylinder results indicate very high levels of NO in the premixed phase of combustion, followed by generally lower levels during the diffusion burning phase. Hydrocarbon signals also indicate significant detail. The in-cylinder uHC signal is consistent with the probe location being between two of the fuel sprays. Both in-cylinder and exhaust results indicate rather high cyclic variability in the NO levels at steady conditions. Variations in the timing and structure of the exhaust uHC signal during the valve open period with load may give insight into the fuel spray/air motion.