Rotor-Synchronised Acquisition of Quadrupolar Satellite Transition NMR Spectra: Practical Aspects and Double-Quantum Filtration

The very broad resonances of quadrupolar (spin I > 1/2) nuclei are resolved by magic angle spinning (MAS) into a large number of spinning sidebands, each of which often remains anisotropically broadened. The quadrupolar interaction can be removed to a first-order approximation if the MAS NMR spectrum is acquired in a rotor-synchronized fashion, aliasing the spinning sidebands onto a centreband and thereby increasing the signal-to-noise ratio in the resulting, possibly second-order broadened, spectrum. We discuss the practical aspects of this rotor-synchronization in the direct (t(2)) time domain, demonstrating that the audiofrequency filters in the receiver section of the spectrometer have a significant impact on the precise timings needed in the experiment. We also introduce a novel double-quantum filtered rotor-synchronized experiment for half-integer spin quadrupolar (spin I = 3/2, 5/2, etc.) nuclei that makes use of central-transition-selective inversion pulses to both excite and reconvert double-quantum coherences and yields a simplified spectrum containing only the ST1 (m(1) = +/- 1/2 <-> +/- 3/2) satellite-transition lineshapes. For spin I = 5/2 nuclei, such as O-17 and Al-27, this spectrum may exhibit a significant resolution increase over the conventional central-transition spectrum. (c) 2005 Elsevier Inc. All rights reserved.