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Issue 22, 2010
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Solid-state dynamic nuclear polarization at 263 GHz: spectrometer design and experimental results

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Abstract

Dynamic Nuclear Polarization (DNP) experiments transfer polarization from electron spins to nuclear spins with microwave irradiation of the electron spins for enhanced sensitivity in nuclear magnetic resonance (NMR) spectroscopy. Design and testing of a spectrometer for magic angle spinning (MAS) DNP experiments at 263 GHz microwave frequency, 400 MHz 1H frequency is described. Microwaves are generated by a novel continuous-wave gyrotron, transmitted to the NMR probe via a transmission line, and irradiated on a 3.2 mm rotor for MAS DNP experiments. DNP signal enhancements of up to 80 have been measured at 95 K on urea and proline in waterglycerol with the biradical polarizing agent TOTAPOL. We characterize the experimental parameters affecting the DNP efficiency: the magnetic field dependence, temperature dependence and polarization build-up times, microwave power dependence, sample heating effects, and spinning frequency dependence of the DNP signal enhancement. Stable system operation, including DNP performance, is also demonstrated over a 36 h period.

Graphical abstract: Solid-state dynamic nuclear polarization at 263 GHz: spectrometer design and experimental results

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Article information


Submitted
26 Feb 2010
Accepted
20 Apr 2010
First published
07 May 2010

Phys. Chem. Chem. Phys., 2010,12, 5850-5860
Article type
Paper

Solid-state dynamic nuclear polarization at 263 GHz: spectrometer design and experimental results

M. Rosay, L. Tometich, S. Pawsey, R. Bader, R. Schauwecker, M. Blank, P. M. Borchard, S. R. Cauffman, K. L. Felch, R. T. Weber, R. J. Temkin, R. G. Griffin and W. E. Maas, Phys. Chem. Chem. Phys., 2010, 12, 5850
DOI: 10.1039/C003685B

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