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@ARTICLE{Jovanovic:894232,
      author       = {Jovanovic, Sven and Schleker, P. Philipp M. and Streun,
                      Matthias and Merz, Steffen and Jakes, Peter and Schatz,
                      Michael and Eichel, Rüdiger-A. and Granwehr, Josef},
      title        = {{A}n electrochemical cell for in operando
                      $\<sup\>13\</sup\>{C}$ nuclear magnetic resonance
                      investigations of carbon dioxide/carbonate processes in
                      aqueous solution},
      journal      = {Magnetic resonance},
      volume       = {2},
      number       = {1},
      issn         = {2699-0016},
      address      = {Göttingen},
      publisher    = {Copernicus Publications},
      reportid     = {FZJ-2021-03112},
      pages        = {265 - 280},
      year         = {2021},
      abstract     = {In operando nuclear magnetic resonance (NMR) spectroscopy
                      is one method for the online investigation of
                      electrochemical systems and reactions. It allows for
                      real-time observations of the formation of products and
                      intermediates, and it grants insights into the interactions
                      of substrates and catalysts. An in operando NMR setup for
                      the investigation of the electrolytic reduction of CO2 at
                      silver electrodes has been developed. The electrolysis cell
                      consists of a three-electrode setup using a working
                      electrode of pristine silver, a chlorinated silver wire as
                      the reference electrode, and a graphite counter electrode.
                      The setup can be adjusted for the use of different electrode
                      materials and fits inside a 5 mm NMR tube. Additionally, a
                      shielding setup was employed to minimize noise caused by
                      interference of external radio frequency (RF) waves with the
                      conductive components of the setup. The electrochemical
                      performance of the in operando electrolysis setup is
                      compared with a standard CO2 electrolysis cell. The small
                      cell geometry impedes the release of gaseous products, and
                      thus it is primarily suited for current densities below
                      1 mA cm−2. The effect of conductive components on 13C
                      NMR experiments was studied using a CO2-saturated solution
                      of aqueous bicarbonate electrolyte. Despite the B0 field
                      distortions caused by the electrodes, a proper shimming
                      could be attained, and line widths of ca. 1 Hz were
                      achieved. This enables investigations in the sub-Hertz range
                      by NMR spectroscopy. High-resolution 13C NMR and relaxation
                      time measurements proved to be sensitive to changes in the
                      sample. It was found that the dynamics of the bicarbonate
                      electrolyte varies not only due to interactions with the
                      silver electrode, which leads to the formation of an
                      electrical double layer and catalyzes the exchange reaction
                      between CO2 and HCO−3, but also due to interactions with
                      the electrochemical setup. This highlights the necessity of
                      a step-by-step experiment design for a mechanistic
                      understanding of processes occurring during electrochemical
                      CO2 reduction.},
      cin          = {IEK-9},
      ddc          = {530},
      cid          = {I:(DE-Juel1)IEK-9-20110218},
      pnm          = {1223 - Batteries in Application (POF4-122)},
      pid          = {G:(DE-HGF)POF4-1223},
      typ          = {PUB:(DE-HGF)16},
      doi          = {10.5194/mr-2-265-2021},
      url          = {https://juser.fz-juelich.de/record/894232},
}