Multiphase flow and contaminant transport in porous media are strongly influenced by the presence of fluid-fluid interfaces. Recent theoretical work based on conservation laws and the second law of thermodynamics has demonstrated the need for quantitative interfacial area information to be incorporated into multiphase flow models. We have used synchrotron based X-ray microtomography to investigate unsaturated flow through a glass bead column. Fully three-dimensional images were collected at points on the primary drainage curve and on the secondary imbibition and drainage loops. Analysis of the high-resolution images (17 micron voxels) allows for computation of interfacial areas and saturation. Corresponding pressure measurements are made during the course of the experiments. Results show the fluid-fluid interfacial area increasing as saturation decreases, reaching a maximum at saturations ranging from 20 to 35% and then decreasing as the saturation continues to zero. The findings support results of numerical studies reported in the literature.