Solid-state Dynamic Nuclear Polarization at 263 GHz: Spectrometer Design and Experimental Results

Overview

Journal Phys Chem Chem Phys

Publisher Royal Society of Chemistry

Specialties Biophysics
Chemistry

Date 2010 May 8

PMID 20449524

Citations 92

Authors

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

Affiliations

Soon will be listed here.

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 (1)H 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.

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