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Reduction of spin diffusion artifacts from 2D zfr-INADEQUATE MAS NMR spectra

Authors
Journal
Journal of Magnetic Resonance
1090-7807
Publisher
Elsevier
Volume
208
Issue
1
Identifiers
DOI: 10.1016/j.jmr.2010.10.006
Keywords
  • Solid-State Nmr
  • Zero-Quantum Coherences
  • Z-Filter
  • Inadequate
  • Magic-Angle Spinning
  • Scalar Coupling
  • Frequency-Switched Lee–Goldberg
  • Homonuclear Decoupling
Disciplines
  • Physics

Abstract

Abstract The primary shortcoming of the z-filtered refocused INADEQUATE MAS NMR pulse sequence is the possibility of artifacts introduced during the z-filter due to spin diffusion where by extra peaks in the single-quantum dimension (from other sites in the molecule) appear correlated with a given double-quantum frequency. This is a problem when the spinning speeds are too slow (less than 15kHz) to sufficiently average the proton–proton homonuclear dipolar couplings. This would be especially important when working with large volume rotors that are difficult to spin fast enough to completely average the homonuclear couplings. In our experiments we used the frequency-switched Lee–Goldberg (FSLG) method of homonuclear decoupling during the z-filter to remove the artifact peaks. This method has the advantage of being quite easy to setup and implement on most modern NMR spectrometers.

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