Solid-State Dynamic Nuclear Polarization at 263 GHz: Spectrometer Design and Experimental Results
Name
PCCP-MMR-100224_ref.pdf
Size
1.16 MB
Format
Adobe PDF
Checksum (MD5)
b97e6817442494ca515a4e462e775e95
Author(s)
Rosay, Melanie
Tometich, Leo
Pawsey, Shane
Bater, Reto
Schauwecker, Robert
Blank, Monica
Borchard, Philipp M.
Cauffman, Stephen R.
Felch, Kevin L.
Weber, Ralph T.
Date Issued
May 2010
Journal
Physical Chemistry Chemical Physics
Publisher
Royal Society of Chemistry
Citation
Rosay, Melanie et al. “Solid-state Dynamic Nuclear Polarization at 263 GHz: Spectrometer Design and Experimental Results.” Physical Chemistry Chemical Physics 12.22 (2010): 5850. Web.
Version
Author's final manuscript
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 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.
MIT Department
Massachusetts Institute of Technology. Department of Chemistry
Massachusetts Institute of Technology. Department of Physics
Francis Bitter Magnet Laboratory (Massachusetts Institute of Technology)
Terms of Use
Creative Commons Attribution-Noncommercial-Share Alike 3.0
Persistent DSpace Link
DOI of Published Version
https://doi.org/10.1039/c003685b
