The present work describes an attractive and economically viablenovel separation techniqueusing superabsorbing hydrophilic polymer gel for dewatering anindustrial o-toluidine-wateremulsion. It is demonstrated that the initial water content of30% in the emulsion is reducedto 3% within 10 min by using a semicontinuous separation strategy,which can have significantenergy savings over the conventional distillation process. Themechanism of water removaland the effect of the presence of interfacial agents on the rate ofwater removal are also studied.