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Sensitivity Enhancement in Structural Measurements by Solid State NMR through Pulsed Spin Locking

โœ Scribed by Aneta T. Petkova; Robert Tycko


Publisher
Elsevier Science
Year
2002
Tongue
English
Weight
161 KB
Volume
155
Category
Article
ISSN
1090-7807

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โœฆ Synopsis


Free induction decay (FID) signals in solid state NMR measurements performed with magic angle spinning can often be extended in time by factors on the order of 10 by a simple pulsed spin locking technique. The sensitivity of a structural measurement in which the structural information is contained in the dependence of the integrated FID amplitude on a preceding evolution period can therefore be enhanced substantially by pulsed spin locking in the signal detection period. We demonstrate sensitivity enhancements in a variety of solid state NMR techniques that are applicable to selectively isotopically labeled samples, including 13 C-15 N rotational echo double resonance (REDOR), 13 C-13 C dipolar recoupling measurements using the constant-time finite-pulse radio-frequency-driven recoupling (fpRFDR-CT) and constant-time double-quantum-filtered dipolar recoupling (CTDQFD) techniques, and torsion angle measurements using the double quantum chemical shift anisotropy (DQCSA) technique. Further, we demonstrate that the structural information in the solid state NMR data is not distorted by pulsed spin locking in the detection period.


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