Currently applied methods for measurement of solubility and supersaturation based on viscometry, refractometry, interferometry and density require the separation of phases prior to measurement. ATR (attenuated total reflection) infrared spectroscopy provides a unique configuration in which the infrared spectrum of a liquid phase can be obtained in a slurry without phase separation. The applicability of the technique was investigated using a micro Circle® open boat cell equipped with a ZnSe (zinc selenide) ATR rod. Experiments conducted with aqueous citric acid proved that ATR infrared spectroscopy can be successfully employed to determine solubility and supersaturation.