Experiments have been performed to demonstrate and quantify cross‐relaxation between water and methylene resonances in a simple model system. Inversion recovery experiments on aqueous solutions of polyethylene glycol produce a transient nuclear Overhauser effect that alters the recovery of the methylene resonance. The relevant equations and parameters that describe this effect are identified and their values are explicitly quantified by analyzing the experimental results. It is shown that cross‐relaxation is measurable and significant in this system even though there are no strong hydrophilic interactions available to immobilize water. In studies of dog bile, the water and lipid resonances behave in a qualitatively similar fashion, lending support to the contention that cross‐relaxation cannot be neglected in solutions of biological macromolecules. © 1989 Academic Press, Inc.