Full quadrupolar tensor determination by NMR using a micro-crystal spinning at the magic angle

An implementation of rotor-synchronised Magic Angle Spinning (MAS) NMR is presented to determine the quadrupolar coupling tensor values from a single crystal study for half-integer quadrupolar nuclei. Using a microcoil based probehead for studying micro crystals with superior sensitivity, we successfully determine the full quadrupolar tensor of 23Na using a micro crystal of dimensions 210 × 210 × 700 μm of NaNO3 as a model system. A two step simulation procedure is used to obtain the orientation of the quadrupolar tensor information from the experimental spectra and is verified by XRD analysis.