The agitation of immiscible liquids or solid suspensions is a frequent operation in chemical and metallurgical industries. The product quality yield and economy of the processes are significantly affected by mixing conditions. Prediction of mean drop size distribution (DSD) during agitation is fundamental for processes in many branches of industry where the mass transfer is crucial. This contribution aims to analyze the homogeneity of a dispersed system in a vessel agitated by a high-shear sawtooth impeller. The homogeneity of liquid−liquid dispersion is determined by comparison of Sauter mean diameters and drop size distribution (DSD) from different measured regions and for various dispersion times. The experiments were carried out in a baffled vessel for various impeller speeds. The sizes of droplets were obtained by the in-situ measurement technique and by the image analysis (IA) method.