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An in situ electrochemical cell for Q- and W-band EPR spectroscopy
Authors:Murray Paul R  Collison David  Daff Simon  Austin Nicola  Edge Ruth  Flynn Brian W  Jack Lorna  Leroux Fanny  McInnes Eric J L  Murray Alan F  Sells Daniel  Stevenson Tom  Wolowska Joanna  Yellowlees Lesley J
Institution:School of Chemistry, University of Edinburgh, Joseph Black Building, King's Buildings, West Mains Road, Edinburgh EH9 3JJ, UK.
Abstract:A simple design for an in situ, three-electrode spectroelectrochemical cell is reported that can be used in commercial Q- and W-band (ca. 34 and 94 GHz, respectively) electron paramagnetic resonance (EPR) spectrometers, using standard sample tubing (1.0 and 0.5 mm inner diameter, respectively) and within variable temperature cryostat systems. The use of the cell is demonstrated by the in situ generation of organic free radicals (quinones and diimines) in fluid and frozen media, transition metal ion radical anions, and on the enzyme nitric oxide synthase reductase domain (NOSrd), in which a pair of flavin radicals are generated.
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