The combination of H-1 magic angle spinning (MAS) n.m.r. and two-dimen
sional nuclear Overhauser enhancement spectroscopy (NOESY) is shown to
be readily applicable to hydrogels. This is demonstrated in the super
absorbing polymer, hydrolysed starch-g-poly(acrylonitrile), which read
ily responds to hydration. Enhanced molecular mobility of the polymer
is directly revealed by polymer-polymer NOESY connectivities. The two-
dimensional experiment also reveals the presence of an efficient cross
-relaxation mechanism between the water of hydration and the polymer.