A new method for extraction kinetics studying in a biphasic system using time-lapse recording of IR absorption spectra in the attenuated total internal reflection (ATR IR) geometry is developed. The method is examined by studying the extraction process of europium, yttrium and cesium ions with various extractants both from acidic and carbonate media. The mechanism of step-wise coordination with functional groups of the ligand is proposed. The extraction kinetics constants are calculated for the extraction systems with europium. The main advantages of the new method are miniaturization and rapidity, compared to classical methods.