As the control of real driving emissions continues to increase in importance, the importance of understanding emission formation mechanisms during engine transients similarly increases. Knowledge of the NO2/NOx ratio emitted from a diesel engine is necessary, particularly for ensuring optimum performance of NOx aftertreatment systems. In this work, cycle-to-cycle NO and NOx emissions have been measured using a Cambustion CLD500, and the cyclic NO2/NOx ratio calculated as a high-speed light-duty diesel engine undergoes transient steps in load, while all other engine parameters are held constant across a wide range of operating conditions with and without exhaust gas recirculation. The results show that changes in NO and NOx, and hence NO2/NOx ratio, are instantaneous upon a step change in engine load. NO2/NOx ratios have been observed in line with previously reported results, although at the lightest engine loads and at high levels of exhaust gas recirculation, higher levels of NO2 than have been previously reported in the literature are observed.