Double and zero quantum filtered H-2 NMR spectroscopy is used to study the structure and dynamics of D2O in sulfonated poly(ether ether ketone) membranes as a function of membrane hydration. Both residual quadrupolar coupling constants and T-2 relaxation values are obtained as a function of hydration. The residual couplings vary from 160 Hz at low hydration to 30 Hz at high hydration. The T-2 relaxation times range from 3 to 14 ms, with the high hydration values having longer T-2. Results from this study are compared to results obtained for Nafion membranes, revealing similarities and differences in the water environments of the two membranes that result from the structure of the polymers and can be related to properties such as water diffusion.