In Situ Electrochemical-NMR Spectroscopy.
Reduction of Aromatic Halides
Richard D. Webster
10.1021/ac0351724.s001
https://acs.figshare.com/articles/journal_contribution/In_Situ_Electrochemical_NMR_Spectroscopy_Reduction_of_Aromatic_Halides/3346534
A three-electrode, two-compartment cylindrical electrochemical cell has been constructed for in situ operation
in a 500 MHz <sup>1</sup>H NMR spectrometer. The cell was
designed around a standard 10-mm sample tube holder
and is lowered into position within the magnet by height-adjustable aluminum rods that support the wires connecting the potentiostat to the working, auxiliary and
reference electrodes. The electrochemical cell functions
under diffusion-controlled conditions in nonspinning
mode and is able to operate under variable temperature
and oxygen-free regimes. The working electrode consists
of a 10-nm-thick gold film deposited onto the surface of
a 7.49-mm-o.d. glass NMR tube that is located directly
within the radio frequency coils of the NMR probe. The
NMR spectra were collected simultaneously to the current
flowing during the electrolysis with typical NMR line
widths being approximately 2 Hz. The highly symmetrical
nature of the cell design meant that probe tuning and
gradient shimming changed minimally between experiments, which allowed standard shim sets to be saved and
recalled for later use, thereby greatly reducing the time
taken for tuning processes. Insertion and removal of the
cell from within the magnet is achieved within a few
seconds, which combined with the rapid shimming process makes the cell suitable for routine operation. The
cell was used to study the in situ reduction of 9-bromoanthracene, 9-chloroanthracene, and 4-bromobenzophenone in deuterated acetonitrile with tetrabutylammonium
hexafluorophosphate as the supporting electrolyte.
2004-03-15 00:00:00
gradient shimming
NMR probe
nonspinning mode
tetrabutylammonium hexafluorophosphate
electrochemical cell
cell design
reference electrodes
glass NMR tube
NMR line widths
NMR spectra
2 Hz
radio frequency coils
electrochemical cell functions
Aromatic Halides
500 MHz 1 H NMR spectrometer
shimming process