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This paper investigates the relationship between NOx and ion current measured inside the combustion chamber of a heavy duty diesel engine under different operating conditions. Nevertheless, ion current is a local signal, thus it is important to measure NOx concentrations at the same exact location of the ion current probe. A novel technique is developed to simultaneously sample in-cylinder NOx and measure the ion current signal by adapting gas sampling probes for ion sensing. The cycle-resolved traces for the rate of heat release, NO mole fraction and ion current were analyzed to determine the contribution of the premixed combustion and the mixing-diffusion controlled combustion on NO formation and ionization in diesel engines.