Analytical Chemistry

Thin-Layer Electroanalysis Microchip Reveals More about Electrochemical Reactions of Organic Compounds



It is important but challenging to elucidate the electrochemical reaction mechanisms of organic compounds using electroanalytical methods. In this work, we exploited the advantages of classic thin-layer electrochemistry to develop a thin-layer electroanalysis microchip (TEAM). The TEAM provided better resolved voltammetric peaks than measurements under semi-infinite diffusion conditions. Importantly, because the analyte solution was mechanically isolated using a polyelectrolyte gel, rapid small-volume electrolysis allowed the accurate determination of the number of electrons transferred, n. The performance of the TEAM was validated using both voltammetry and coulometry of standard redox couples. Moreover, a spectroelectrochemical analysis of FM 1-43, an organic dye widely used in neuroscience, was successfully performed. Harnessing the analytical power of the TEAM, the electrochemical oxidation mechanisms of pivanilides and alkyltrifluoroborate salts were studied. Thus, the TEAM has the potential to provide invaluable mechanistic information and promote the rational design of electrosynthetic strategies.


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Supplementary material

Thumbnail image of Supplementary (Commun)_TLC_210721.pdf
Supplementary Information
Experimental details; additional simulation data and explanation; cross-sectional diagram of TEAM; synthetic scheme of pLA-TFPB, peak-to-peak separation of ferrocyanide CVs; n–t plot without polyelectrolyte gel; CVs of Fc, FM1-43, and 4-MePhNHPiv with semi-infinite diffusion; summary of oxidation potential and n.
Thumbnail image of 01 20um concentration profile E1 0.5 E2 0.6 15hz dE 2mV tiime step.gif
Video S1
Video of simulated concentration profile change in thin-layer cell.