doi:10.1016/j.cplett.2004.08.050
Copyright © 2004 Elsevier B.V. All rights reserved.
A continuously recirculating optical pumping apparatus for high xenon polarization and surface NMR studies
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Kevin Knagge, Jonathan Prange and Daniel Raftery
, 
Department of Chemistry, Purdue University, 560 Oval Drive, West Lafayette, IN 47907, USA
Received 10 May 2004;
revised 16 August 2004.
Available online 11 September 2004.
Abstract
A continuously recirculating xenon optical pumping apparatus was constructed and coupled to a 200 MHz NMR spectrometer. Steady-state 129Xe polarizations as high as 69% were achieved approximately 5 min after circulation was begun, and this polarization is >3.5 times larger than observed for single pass operation. Using this apparatus, spin polarization induced nuclear Overhauser effect (SPINOE) experiments were performed on porous silicon samples and on 13CD3OD adsorbed on TiO2-coated optical fibers to evaluate the capabilities of the system for studying low surface areas samples. The 13C enhancement achieved was approximately 14. The recirculating optical pumping system provides high xenon polarization at moderate laser powers for a variety of NMR studies.
Fig. 1. Schematic design of continuous recirculation optical pumping apparatus.
Fig. 2. 129Xe polarization versus laser cell temperature for different flow rates. Non-recirculating (single pass) conditions with a flow rate of 150 mL/min: diamond. Recirculating conditions with a flow rate of: 250 mL/min, filled box; 200 mL/min, triangle; 150 mL/min, cross; 100 mL/min, open box. Polarization was calculated by comparing the hyperpolarized xenon signals to a standard of 14 μmol of Xe gas.
Fig. 3. (a) 29Si spectrum of porous silicon using hyperpolarized xenon flowing at 200 mL/min taken at 143 K. Spectrum was obtained after 16 transients with a delay of 100 s. (b) 29Si spectrum of porous silicon without hyperpolarized xenon taken at 143 K. Spectrum was obtained after 128 transients with a delay of 100 s. TMS was used as the 29Si reference.
Fig. 4. Dotted line is 13C spectrum of 13CD3OD adsorbed on titanium coated optical fibers. Spectrum was taken with continuous re-circulating hyperpolarized xenon at a flow rate of 100 mL/min and at 143 K. Solid line is simulated powder pattern with chemical shift anisotropy parameters of δ = 2800 Hz and η = 0.5.

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