Abstract
The use of rotating disk electrodes (RDEs) is probably the most convenient way of studying simple electrode reactions under well-defined transport conditions. Standard RDEs become, however, less expedient when the studied electrode process is a complex one, leading to the formation of various reaction products. In these cases, the accurate detection and quantification of the formed products are desirable. If the formed products are gaseous, then the usual way of quantifying them is the use of online gas chromatography (GC), a method that is not compatible with open RDE cells. In order to overcome these difficulties, we present here a sophisticated inverted RDE (iRDE) cell design. The design combines various advantages: it is amenable to the same mathematical treatment as standard (downward-facing) RDEs; it can be operated airtight and coupled to online GC; and due to its upward-facing design, the electrode surface is less prone to blockage by any formed gas bubbles. The iRDE&GC design is tested using simple model reactions and is demonstratively used for studying the electrochemical reduction of CO2, accompanied by parasitic hydrogen evolution, on a silver electrode.
Highlights
The use of rotating disk electrodes (RDEs) is probably the most convenient way of studying simple electrode reactions under well-defined transport conditions
In order to check the hydrodynamic performance of the inverted RDE (iRDE) design, we measured linear sweep voltammograms (LSVs, sweep rate 20 mV s−1) on a glassy carbon iRDE in a 1 mol dm−3 KCl electrolyte solution containing the ferro-/
We presented the design of a custom-made, hermetically sealed inverted rotating disk electrode coupled to a gas chromatographic detection system
Summary
We presented the design of a custom-made, hermetically sealed inverted rotating disk electrode coupled to a gas chromatographic detection system. Special care must be taken in this situation so that the purging gas flow does not interfere with the convective transport of the rotating disk Another important point that deserves emphasis is related to the transport conditions of the iRDE cell. It is usually assumed that on rotating electrodes stationary current/potential characteristics can be attained, this condition may not hold for long-lasting experiments during which the electrolysis becomes at least partially exhaustive. This second limitation may, be overcome if the electrolyte solution is replaced from time to time or when a continuous flow of electrolyte guarantees that no permanent bulk concentration changes can be caused by the electrolysis. Scanning electron micrographs and energy-dispersive Xray spectra of alumina and diamond-polished silver RDE surfaces (PDF)
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