Toward CO Electroreduction Under Controlled Mass Flow Conditions: A Combined Inverted RDE and Gas Chromatography Approach

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 CO, accompanied by parasitic hydrogen evolution, on a silver electrode.