Film coating fluids commonly contain a pigment suspension. The sedimentation of insoluble particles in the coating suspension is one of the main problems during the formulation of the coating fluid. The aims of this work were to investigate the suitability of an energy-dispersive X-ray fluorescence analyser for rapid measurement of the sedimentation of titanium dioxide in aqueous suspensions. The suspensions were produced with a high-speed Ultra-Turrax. The process factors evaluated were the stirring rate, time and volume, and the process of sedimentation of the pigment. The enrichment of the pigment at the bottom of the sample holder was followed by means of the very rapid method of energy-dispersive X-ray fluorescence analysis. It can be concluded that the sedimentation of the particles is described by the Weibull equation. With an appropriate combination of the factors, a threefold increase in the sedimentation time was achieved. The mathematically based information (sedimentation time, kinetics of sedimentation, etc.) is essential for an exact evaluation of the preparation of the coating fluid. The understanding of the process through use of this test method leads to the ability to identify the critical control points of film coating.