The effect of phase inversion during semibatch aromatic nitrations is experimentally characterized and analysed. The influence of various parameters, i.e. interfacial area, effective heat-transfer coefficient and overall mass-transfer coefficient, is studied. The implications for optimizing nitrations are discussed from performance and safety points of view. The accumulation of unreacted nitric acid can be dangerous if accompanied by a phase inversion, owing to the fact that the rate may increase suddenly.