Anin situelectrochemical cell for Q- and W-band EPR spectroscopy
Publication year: 2011
Source: Journal of Magnetic Resonance, Available online 22 September 2011
Paul R.*Murray, David*Collison, Simon*Daff, Nicola*Austin, Ruth*Edge, ...
A simple design for anin 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 thein situgeneration 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.
Graphical abstract
Highlights
? In situ EPR/ESR spectroelectrochemistry at high frequency. ? 3-electrode cells in standard Q- and W-band silica tubes. ? Variable temperature operation, including frozen solutions. ? Example operation on ubiquinone, bpipyridines and their platinum complexes, and a flavin protein.
Source:
Journal of Magnetic Resonance