MATPASS/CPMG: A sensitivity enhanced magic-angle spinning sideband separation experiment for disordered solids

Abstract

A Carr–Purcell Meiboom–Gill (CPMG) sensitivity-enhanced spinning sideband separation experiment is presented. The experiment combines the idea of magic-angle turning and phase-adjusted sideband separation (MATPASS), allowing for isotropic/anisotropic chemical shift separation of disordered solids with line widths far greater than the magic-angle spinning frequency. The use of CPMG enhances the sensitivity of the wide-line spectra by an order of magnitude via multiple-echo acquisition. The MATPASS/CPMG protocol involves acquisition of time-domain data using a MAT/CPMG pulse sequence followed by f1 shearing during data processing to arrive at the PASS representation. Such a protocol has √2 higher sensitivity than the conventional PASS method because all CPMG echo signals are used for the final PASS spectrum. Application of this method is demonstrated using a GeSe4 glass sample with both 77Se isotropic line widths and chemical shift anisotropy that far exceed the spinning frequency. The sideband separation allows for the measurement of chemical shift anisotropy of the disordered solids.