Pure Isotropic Proton Solid State NMR.

Resolution in proton solid state magic angle sample spinning (MAS) NMR is limited by the intrinsically imperfect nature of coherent averaging induced by either MAS or multiple pulse sequence methods. Here, we suggest that instead of optimizing and perfecting a coherent averaging scheme, we could approach the problem by parametrically mapping the error terms due to imperfect averaging in a -space representation, in such a way that they can be removed in a multidimensional correlation leaving only the desired pure isotropic signal. We illustrate the approach here by determining pure isotropic H spectra from a series of MAS spectra acquired at different spinning rates. For six different organic solids, the approach is shown to produce pure isotropic H spectra that are significantly narrower than the MAS spectrum acquired at the fastest possible rate, with linewidths down to as little as 48 Hz. On average, we observe a 7-fold increase in resolution, and up to a factor of 20, as compared with spectra acquired at 100 kHz MAS. The approach is directly applicable to a range of solids, and we anticipate that the same underlying principle for removing errors introduced here can be applied to other problems in NMR spectroscopy.