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A potential correlation between OH* chemiluminescence and exhaust NO concentration is investigated to pursue a simple diagnostic technique for measurements of NO cycle-to-cycle fluctuations. Previous investigations of NO formation in a direct-injection gasoline engine have indicated that there may be a correlation between the concentration of NO and OH* chemiluminescence. Shortcomings of this work, namely phase-locked measurements, were overcome in the present study by using highspeed imaging capability to obtain chemiluminescence within the entire engine cycle and from entire engine cylinder volume. Cycle-resolved NO exhaust gas detection were performed synchronously with the chemiluminescence measurements on an optical spark-ignited engine with spray-guided direct-injection. A quartz cylinder liner, head and piston windows provide optical access for a highspeed CMOS camera and image intensifier to capture OH* images.