Prenzler, Paul DBramley, RichardDowning, StephenHeath, Graham2015-12-131388-2481http://hdl.handle.net/1885/90110This report summarizes the design and performance of the first practicable in situ electrogenerative high-field solution-NMR cell, designed for simultaneous NMR spectroelectrochemistry in a conventional 10- or 16-mm 300 MHz probe. The axially symmetric three-electrode assembly is stationary and self-aligning. It dips into a standard spinning 10-mm sample tube and is adapted for convenient operation in any commercial high-field, multi-nuclear, variable-temperature FT NMR spectrometer. The tubular, rf-transparent working electrode (presently consisting of a gold film, coated on glass) completely spans the detection region; the recommended coating thickness is ≤ 0.01 δ where δ is the rf-absorbing conductor skin depth. With careful shimming, very narrow1H signals (~ 1 Hz) can be obtained. The performance of the in situ NMR-electrochemical cell is illustrated by monitoring the progressive reduction of 'p-quinone' (1,4-benzoquinone) to its dihydro-form by controlled-potential electrolysis in an acidic medium. (C) 2000 Elsevier Science S.A.Keywords: 1,4 benzoquinone; analytic method; article; compartment model; electrochemical analysis; electrode; electrolysis; nuclear magnetic resonance spectroscopy Electrolysis; In situ detection; NMR-electrochemical cell; Nuclear magnetic resonance; Quinone/hydroquinone; Spectroelectrochemistry200010.1016/S1388-2481(00)00042-42015-12-12