High-Resolution 1H NMR of Powdered Solids by Homonuclear Dipolar Decoupling

Abstract The development of homonuclear dipolar decoupling sequences to obtain high-resolution 1H NMR spectra from solids has recently celebrated its 50th birthday. Over the years, a series of different decoupling schemes have been developed, starting with the pioneering Lee-Goldburg and WAHUHA sequences up to the most recent generations of experimentally optimized phase-modulated schemes such as eDUMBO-122 and LG4. These schemes can all yield over an order of magnitude reduction in 1H NMR linewidths in solids. Here we provide an overview and a broad experimental comparison of the performance of the main sequences, which has so far been absent in the literature, especially between the newest and the oldest decoupling schemes. We compare experimental results obtained using eight different decoupling schemes (LG, WHH-4, MREV-8, BR-24, FSLG/PMLG, DUMBO-1, eDUMBO-122 and LG4) on three different microcrystalline powdered samples (alanine, glycine and β-AspAla) and at three different MAS rates (3.0, 12.5 and 22.0 kHz). Finally, since these sequences can be technically demanding, we describe the experimental protocol we have used to optimize these schemes with the aim to provide simple guidelines for the optimization of CRAMPS experiments for all NMR users.