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

Melanie Rosay; Leo Tometich; Shane Pawsey; Reto Bader; Robert Schauwecker; Monica Blank; Philipp M. Borchard; Stephen R. Cauffman; Kevin L. Felch; Ralph T. Weber; Richard J. Temkin; Robert G. Griffin; Werner E. Maas

doi:10.1039/C003685B

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Physical Chemistry Chemical Physics

Issue 22, 2010

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

Melanie Rosay , Leo Tometich , Shane Pawsey , Reto Bader , Robert Schauwecker , Monica Blank , Philipp M. Borchard , Stephen R. Cauffman , Kevin L. Felch , Ralph T. Weber , Richard J. Temkin , Robert G. Griffin and Werner E. Maas

Phys. Chem. Chem. Phys., 2010,12, 5850-5860

DOI: 10.1039/C003685B
Received 26 Feb 2010, Accepted 20 Apr 2010
First published on the web 07 May 2010
This article is part of the collection: High field dynamic nuclear polarization – The renaissance

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Abstract
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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 water–glycerol 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.