Correlating Fast and Slow Chemical Shift Spinning Sideband Patterns in Solid-State NMR

Robin Orr, Melinda J Duer, Sharon Elizabeth Ashbrook

Research output: Contribution to journalArticlepeer-review

32 Citations (Scopus)

Abstract

An experiment is presented that enables the measurement of small chemical shift anisotropy tensors under fast magic-angle spinning (MAS). The two-dimensional spectra obtained give a fast MAS sideband pattern in the directly observed dimension with the spinning sideband intensities equivalent to the chemical shift anisotropy scaled by a factor of N, or equivalently the sample spinning frequency scaled by 1/N, in the indirectly observed dimension. The scaling factor may be arbitrarily varied by changing the number and timings of the rotor synchronized π-pulses used. Desirable features of the experiment include a fixed length pulse sequence and efficient sampling of the indirectly observed dimension. In addition, neither quadrature detection in the indirect dimension nor storage periods are required, consequently no signal intensity is discarded by the pulse sequence. The experiment is demonstrated using P-31 NMR of sodium phosphate and C-13 NMR of fumaric acid monoethyl ester for which a scaling factor of N = 10.2 was employed. © 2005 Elsevier Inc. All rights reserved.

Original languageEnglish
Pages (from-to)301-309
Number of pages9
JournalJournal of Magnetic Resonance
Volume174
DOIs
Publication statusPublished - Jun 2005

Keywords

  • solid-state NMR
  • magic-angle spinning
  • chemical shift anisotropy
  • recoupling
  • NUCLEAR-MAGNETIC-RESONANCE
  • MAGIC-ANGLE
  • ROTATING SOLIDS
  • 2-DIMENSIONAL SEPARATION
  • SPECTRA
  • PHASE
  • MAS
  • SPECTROSCOPY
  • MANIPULATION
  • RESOLUTION

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