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School of Energy and Chemical Engineering (Chemical Engineering)Glycerol, a major by-product in biodiesel production, can be selectively electrooxidized to the value-added derivatives such as dihydroxyacetone and glyceric acid. In particular, dihydroxyacetone is a monomer that is difficult to synthesize and has a high market price, so it is a promising monomer. Highly conductive two-dimensional titanium carbide (Ti3C2) was chosen as a support for platinum to obtain dihydroxyacetone, and the results were confirmed according to the number of Ti3C2 layers by comparison with Pt/C. It was demonstrated that the presence of bismuth can selectively change the mechanism of glycerol oxidation. In the absence of bismuth, glycerol oxidation progressed both primary and secondary alcohol oxidation, but primary oxidation was dominant. The onset potential was shifted and the primary oxidation pathway was blocked in the presence of bismuth, so secondary oxidation proceeded dominantly. Also, at a specific potential, the selectivity of dihydroxyacetone was obtained about 100 %. Furthermore, a small-scale flow cell for an online product analysis was designed. By reducing the dead volume as much as possible, an internal volume of 100 ??L were obtained, and the electrode surface area to the volume of electrolyte was increased. The flow cell is combined with linear sweep voltammetry technique to establish a system for direct product analysis by HPLC. It was suitable for analyzing concentrated products in a range of the potential, and Faraday efficiency was calculated by potential. From the CVs of the Pt/C and Pt/Ti3C2 catalysts in 0.5 M H2SO4 with 2 M glycerol, the synthesized Pt/Ti3C2 catalysts showed a current density more than 2 times higher than commercial Pt/C. From the results of LSVs, Pt/22L showed the best electrocatalytic performance in the concentration of the products (dihydroxyacetone: 0.09 mM) and the Faraday efficiency (99.5 %), and the current density (3.4 mA cm-2). Therefore, the edge-dominancy of the Ti3C2 support showed higher glycerol electrooxidation activity. A quantitative and qualitative standard for glycerol electrooxidation is successfully established by a system of designed flow cell combined with voltammetry.clos