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T G Ajithkumar

Publications and source records attributed to T G Ajithkumar.

4 recordsLinked to original sources

New opportunities for double rotation NMR of half-integer quadrupolar nuclei.

A combined approach is presented which expands the applicability of double rotation (DOR) by overcoming its most prominent disadvantages: spinning stability and sensitivity. A new design using air-bearings for the inner rotor and a computer-assisted start-up procedure allows DOR operation over in principle unlimited time at outer rotor speeds of up to 2000Hz. Sensitivity enhancement of the DOR experiment is achieved by applying amplitude-modulated adiabatic pulses such as the double frequency sweep (DFS) before pulse excitation. Repeating the DFS enhancement and signal readout several times without allowing for spin-lattice relaxation leads to sensitivity enhancements of a factor 3 for (27)Al in various minerals. As a result, it becomes possible to study low sensitivity quadrupolar nuclei and various long duration 2D measurements can be performed routinely. Spinning is adequate to suppress residual homonuclear dipolar couplings in the spectral dimension of typical quadrupolar spin systems. In 2D-exchange spectroscopy, however, homonuclear correlation can still be established through dipolar-quadrupolar cross-terms.

Journal Article↗

Homonuclear correlation experiments of half-integer quadrupolar nuclei using multiple-quantum techniques spinning at a P(4) magic angle.

A new approach for obtaining structural information in half-integer quadrupolar nuclei is proposed and demonstrated. In this method, the two-dimensional multiple-quantum experiment is performed, spinning at one of the angles at which the fourth order Legendre polynomial vanishes (P4 magic angle). In such an experiment, the dipolar interaction is retained, whereas the second-order quadrupolar broadening is refocused by the MQ-1Q correlation scheme. By adding an exchange period to this pulse scheme, we performed efficient homonuclear correlation experiments in a regular magic angle spinning probe with minor modifications. The experiment is demonstrated on a model compound, and the results are briefly discussed.

Journal Article↗

Off-resonance effects in two-dimensional NQR spectroscopy using a single crystal.

Two-dimensional nutation pure NQR experiments on 35Cl have been carried out on a single crystal of NaClO3. The 2D nutation experiment separates out different orientations of each chemically equivalent site in a unit cell as a separate frequency in the omega1 domain. The squares of the observed frequencies lie on a straight line with respect to the squares of the offsets, confirming the expected offset dependence quantitatively. The intercepts at zero offset yield the relative orientations of the efg tensors with respect to the axis of the radiofrequency coil.

Crystallization↗

Homonuclear correlation experiments for quadrupolar nuclei, spinning away from the magic angle.

We present a set of homonuclear correlation experiments for half-integer quadrupolar spins in solids. In all these exchange-type experiments, the dipolar interaction is retained during the mixing time by spinning the sample at angles other than the "regular magic angle" (54.7 degrees celsius). The second-order quadrupolar interaction is averaged by different strategies for the different experiments. The multiple-quantum off magic angle spinning (MQOMAS) exchange experiment is essentially a regular MQMAS experiment where the quadrupolar interaction is averaged by combining magic angle spinning with a multiple- to single-quantum correlation scheme. The sample is spun at the magic angle at all times except during the mixing time which is added to establish homonuclear correlation. In the multiple-quantum P4 magic angle spinning (MQP4MAS) exchange experiment, the sample is spun at one of the angles at which the fourth-order Legendre polynomial vanishes (P4 magic angle), the remaining second-order quadrupolar interaction now governed by a second-rank tensor is refocussed by the multiple to single-quantum correlation scheme. In the dynamic angle spinning (DAS) exchange experiment, the second-order quadrupolar interaction is averaged by correlating the evolution from two complementary angles. These experiments are demonstrated and compared, in view of their specific advantages and disadvantages, for 23Na in the model compound Na2SO3.

Journal Article↗