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

作者：Hung Ivan; Edwards Trenton; Sen Sabyasachi; Gan Zhehong^*

来源：Journal of Magnetic Resonance, 2012, 221: 103-109.

DOI：10.1016/j.jmr.2012.05.013

• Chemical shift anisotropy (CSA)
• Magic-angle turning (MAT)
• Phase-adjusted spinning sidebands (PASS)
• CPMG
• Magic-angle spinning (MAS)
• GeSe4 glass
• Se-77

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 f(1) shearing during data processing to arrive at the PASS representation. Such a protocol has root 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 Se-77 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.

• 出版日期2012-8