Synthesis, characterization, and interfacial properties of hydroxy-substituted alkyl benzenesulfonates, sodium 2-hydroxy-3-decyl-5-octylbenzenesulfonate (C10C8OHphSO3Na) and 2-hydroxy-3-octyl-5-decylbenzenesulfonate (C8C10OHphSO3Na), are reported. The dynamic dilational properties of the surfactants are expounded by means of oscillating the bubble/drop method at both water-air and water-decane interfaces. The distinct maxima appear in dilational modulus vs time curves in some cases, which is believed to be attributed to the change of surfactant conformation and the arrangement of surface layer. Our results show that the measurement of dynamic interfacial dilational properties is a powerful tool to probe the structure of the surfactant adsorption film.