TY - JOUR
T1 - High-field NMR spectroelectrochemistry of spinning solutions
T2 - Simultaneous in situ detection of electrogenerated species in a standard probe under potentiostatic control
AU - Prenzler, Paul D.
AU - Bramley, Richard
AU - Downing, Stephen R.
AU - Heath, Graham A.
PY - 2000
Y1 - 2000
N2 - This 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 narrow 1H 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.
AB - This 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 narrow 1H 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.
KW - Electrolysis
KW - In situ detection
KW - NMR-electrochemical cell
KW - Nuclear magnetic resonance
KW - Quinone/hydroquinone
KW - Spectroelectrochemistry
UR - http://www.scopus.com/inward/record.url?scp=0033826291&partnerID=8YFLogxK
U2 - 10.1016/S1388-2481(00)00042-4
DO - 10.1016/S1388-2481(00)00042-4
M3 - Article
SN - 1388-2481
VL - 2
SP - 516
EP - 521
JO - Electrochemistry Communications
JF - Electrochemistry Communications
IS - 7
ER -