Combining STMAS and CRAMPS NMR spectroscopy: High-resolution HETCOR NMR spectra of quadrupolar and H-1 nuclei in solids

abstract

High-resolution two-dimensional (2D) heteronuclear correlation spectra between half-integer quadrupolar and H-1 nuclei have been obtained combining Satellite Transition Magic-Angle Spinning (STMAS) and wPMLG3 CRAMPS methods. The experiments use split-t(1) versions of DQ/DQF-STMAS adapted to 3/2 and 5/2 spins to obtain a Na-23 and Al-27 isotropic dimension, respectively. Transfer of magnetization from quadrupolar nuclei to protons has been achieved by cross-polarization, and high-resolution H-1 spectra have been recorded using the wPMLG3 decoupling during the t(2) evolution period. The performance of the pulse sequences have been tested on the templated microporous aluminophosphate IST-1 and trisodium citrate employing a B-0 field of 9.4 T. (C) 2009 Elsevier B. V. All rights reserved.

keywords

QUANTUM CROSS-POLARIZATION; ANGLE-SPINNING NMR; STATE NMR; MQMAS NMR; HETERONUCLEAR CORRELATION; MAS NMR; SENSITIVITY ENHANCEMENT; AMPLITUDE-MODULATION; MAGNETIC-RESONANCE; IST-1

subject category

Chemistry; Physics

authors

Siegel, R; Rocha, J; Mafra, L

our authors

acknowledgements

We acknowledge CICECO and University of Aveiro. We also thank Fundacao para a Ciencia e Tecnologia (FCT) for their general financial support and for Post-Doc Grant SFRH/BPD/44355/2008 (to R. S.).

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