Many groundwater contamination incidents begin with the release of an essentially immiscible fluid into the subsurface environment. Once in the subsurface, an immiscible fluid participates in a complex pattern of transport processes. For immiscible fluids that are commonly found in contaminated groundwater environments the interphase mass transfer between the nonaqueous phase liquids (NAPLs) phase and the aqueous phase is an important process. An experimental apparatus and procedure were used to isolate and measure mass transfer between toluene and water in glass bead media systems. The rate of interphase mass transfer was investigated in two-fluid systems as a function of aqueous phase velocity, aqueous- and nonaqueous-phase fluid saturations, and porous media characteristics. The rate of interphase mass transfer is found to be directly related to aqueous phase velocity and nonaqueous phase fluid saturation level, but no significant relation to mean particle size is found. Correlation expressions for the rate of interphase mass transfer are developed using relevant dimensionless parameters and are compared to literature values. Equilibrium between the two fluid phases investigated is shown to be achieved rapidly, over wide ranges of nonaqueous phase fluid saturations and aqueous phase velocities. The derived correlations provide a means for estimating the appropriateness of the local equilibrium assumption for a nonaqueous phase liquid-aqueous phase couple in multiphase groundwater systems.