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Water mobility within the porous network of dense clay sediments was investigated over a broad dynamical range by using 2 H nuclear magnetic resonance spectroscopy. Multi-quanta 2 H NMR spectroscopy and relaxation measurements were first performed to identify the contributions of the various relaxation mechanisms monitoring the time evolution of the nuclear magnetisation of the confined heavy water. Secondly, multi-quanta spin-locking NMR relaxation measurements were then performed over a broad frequency domain, probing the mobility of the confined water molecules on a time-scale varying between microseconds and milliseconds. Thirdly, 1 H NMR pulsed-gradient spin-echo attenuation experiments were performed to quantify water mobility on a time-scale limited by the NMR transverse relaxation time of the confined NMR probe, typically a few milliseconds. Fourthly, the long living quantum state of the magnetisation of quadrupolar nuclei was exploited to probe a two-time correlation function at a time-scale reaching one second. Finally, magnetic resonance imaging measurements allow probing the same dynamical process on time-scales varying between seconds and several hours. In that context, multi-scale modelling is required to interpret these NMR measurements and extract information on the influences of the structural properties of the porous network on the apparent mobility of the diffusing water molecules. That dual experimental and numerical approach appears generalizable to a large variety of porous networks, including zeolites, micelles and synthetic or biological membranes.

international journal of molecular sciences

A Multi-Scale Study of Water Dynamics under Confinement, Exploiting Numerical Simulations in Relation to NMR Relaxometry, PGSE and NMR Micro-Imaging Experiments: An Application to the Clay/Water Interface