Pulsed field gradient NMR measurements are made of the proton diffusion coefficient in proton uranyl periodates. The conductivity and the diffusion coefficient are sensitive to relative humidity, and the measurements are made under carefully controlled relative humidity conditions. It is found that the activation energy for diffusion is consistently smaller than that required for conductivity, perhaps due to the necessity in the conduction process of forming carriers, whereas diffusion is sensitive only to carrier mobilities. The activation energy decreases with increasing humidity, perhaps reflecting the extent of completeness of hydrogen bonded networks. Copyright © 1990 WILEY‐VCH Verlag GmbH & Co. KGaA