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1. 2 DEMS Instrument Overview 31 Fig. 1 A diagram presenting an overview of the various components contributing to the whole DEMS instrument setup. The instrument consists of the key DEMS components, namely the electrochemical cell, membrane interface and vacuum system including QMS. The operation of the DEMS components of course relies on additional instrumental control and data acquisition hardware and software Although in DEMS we are essentially combining an electrochemical half-cell with mass spectrometry, they are nonetheless operated and controlled as discrete entities that happen to be (albeit intentionally) interfaced by a membrane.

3 Study of the Electro-oxidation of Small Organic Compounds One of the first ever DEMS studies focused its attention towards the study of the methanol oxidation reaction (MOR) which is of fundamental research interest for direct methanol fuel cell (DMFC) development [37]. Since then, the MOR [7, 21, 31, 50, 51] and other potential organic fuels that are oxidised to carbon dioxide, such as ethanol [32, 52–54] have been quite extensively studied using DEMS on a number of electrode systems. The overall MOR may be described by the following reaction formula: E CH3 OH þ H2 O !

1) in terms of potential control and stability. This necessitates the modification of the standard threeelectrode electrochemical setup, employing a stabilising resistor and NID, later described in detail in Sect. 1. 1 Details of the specifications of the two DEMS cell flow regimes Cyclone Linear WE comp. Sampling comp. 2 (-membrane) *9 The compartmental volumes are determined by the size and shape of the punctured holes in the cell PTFE gaskets To summarise, the modular DEMS electrochemical flow cell design presented here allows controlled electrochemistry at the WE of interest and incorporates a PTFE membrane that interfaces the cell electrolyte with the vacuum of a QMS.

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