Multiple-pulse and magic-angle spinning aided double-quantum proton solid-state NMR spectroscopy

We here report on a high-resolution pulse scheme for double-quantum (DQ) proton NMR spectroscopy in the solid-state. The pulse scheme employs a combination of multiple-pulses and magic-angle spinning (MAS) for both the excitation and conversion of DQ coherences and their evolution under homonuclear dipolar decoupling. This is made possible in this two-dimensional experiment by an effective combination of homonuclear dipolar decoupling method of phase modulated Lee-Goldburg and symmetry adapted sequence for homonuclear dipolar recoupling under MAS. DQ spectra of monoethyl fumaric acid, glycine, and histidine are presented to highlight the utility of the pulse scheme together with some of the existing drawbacks. (C) 2004 Published by Elsevier B.V.