The thermophysical properties of liquid mixtures are very important as fundamental data in process design and are also helpful in understanding characteristics of solutions.Comparing thermophysical properties with spectroscopic measurements, different contributions to the non-ideal behavior of liquid mixture can be evaluated. The proposed research work is a detailed thermophysical and spectroscopic studies of structural and interactional behavior of mixtures of alkanediols in non-aqueous media. The aim of the present work is twofold: first is to enlarge the thermodynamic database for mixtures needed by the industry for design purpose. Secondly, the estimation of several related parameters in order to attain a deeper insight into various interactions operating in the mixtures. The emphasis is to report excess volumes, ultrasonic velocities, viscosity and spectroscopic (IR, 1H and 13C NMR) data in order to obtain information about structural and interactional parameters for the mixtures of alkanediols in non-aqueous media. The present study seems to have the most promising chance to be used successfully in different fields of chemistry and chemical engineering.