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Refocusing CSA during magic angle spinning rotating-frame relaxation experiments.

Eric G Keeler1, Keith J Fritzsching1, Ann E McDermott1

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Journal of Magnetic Resonance (San Diego, Calif. : 1997)
|September 26, 2018
PubMed
Summary
This summary is machine-generated.

Coherent spin-locked magnetization evolution in magic-angle spinning (MAS) affects relaxation measurements. A new pulse sequence, RECRR, minimizes these effects for accurate dynamic information.

Keywords:
CSA refocusingChemical kineticsRotary echo

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Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy.
  • Chemical dynamics and molecular motion analysis.

Background:

  • Magic-angle spinning (MAS) NMR is crucial for studying molecular dynamics.
  • Rotating-frame relaxation (R1ρ) experiments probe chemical exchange.
  • Coherent evolution of spin-locked magnetization can complicate R1ρ measurements.

Purpose of the Study:

  • To investigate coherent spin-locked magnetization evolution during MAS relaxation experiments.
  • To assess the impact of chemical shielding anisotropy (CSA) on this coherent evolution.
  • To develop a pulse sequence for more accurate R1ρ measurements.

Main Methods:

  • Numerical simulations of spin dynamics under MAS conditions.
  • Experimental validation using solid-state NMR.
  • Development and testing of a novel pulse sequence (RECRR).

Main Results:

  • Coherent evolution of spin-locked magnetization is significant even when standard matching conditions are avoided.
  • This coherent evolution interferes with the analysis of relaxation decay curves.
  • The proposed RECRR pulse sequence effectively refocuses CSA contributions.

Conclusions:

  • Coherent evolution poses challenges for extracting dynamic information from R1ρ experiments.
  • The RECRR pulse sequence enhances sensitivity and reduces interference from coherent evolution.
  • RECRR is robust to experimental imperfections like field inhomogeneity and miscalibrations.