Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25K

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Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25K

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12-15-2012, 09:51 AM

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Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25K

Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25K

January 2013
Publication year: 2013
Source:Journal of Magnetic Resonance, Volume 226

We describe an apparatus for solid state nuclear magnetic resonance (NMR) with dynamic nuclear polarization (DNP) and magic-angle spinning (MAS) at 20–25K and 9.4Tesla. The MAS NMR probe uses helium to cool the sample space and nitrogen gas for MAS drive and bearings, as described earlier [1], but also includes a corrugated waveguide for transmission of microwaves from below the probe to the sample. With a 30mW circularly polarized microwave source at 264GHz, MAS at 6.8kHz, and 21K sample temperature, greater than 25-fold enhancements of cross-polarized 13C NMR signals are observed in spectra of frozen glycerol/water solutions containing the triradical dopant DOTOPA-TEMPO when microwaves are applied. As demonstrations, we present DNP-enhanced one-dimensional and two-dimensional 13C MAS NMR spectra of frozen solutions of uniformly 13C-labeled l-alanine and melittin, a 26-residue helical peptide that we have synthesized with four uniformly 13C-labeled amino acids.
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? Probe for solid state NMR with dynamic nuclear polarization (DNP) and magic-angle spinning (MAS) at 20K and 9.4Tesla. ? Signal enhancement greater than 25-fold (microwaves on versus microwaves off) using 30mW of microwaves. ? 2D 13C–13C spectra for 160nmol of the 26 residue peptide melittin in frozen solution, taken in ~2½h.

Source: Journal of Magnetic Resonance

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