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Observación directa de C₂O₄ y CO₂ mediante la oxidación de oxalato dentro del nanoespacio del microscopio

Tianhan Kai¹, Min Zhou¹, Sarah Johnson¹

¹Center for Electrochemistry, Department of Chemistry , The University of Texas at Austin , Austin , Texas 78712 , United States.

Journal of the American Chemical Society

|November 3, 2018

Resumen

La oxidación del oxalato involucra a los aniones radicales intermedios. Este estudio utilizó microscopía electroquímica de barrido a nanoescala para demostrar un mecanismo escalonado, determinando que la vida media del anión radical oxalato (C2O4•−) es de 1,3 μs.

Área de la Ciencia:

La electroquímica
Química analítica
La fotoquímica

Sus antecedentes:

La oxidación de oxalato es crucial para los sistemas de quimioluminiscencia electrogenerada (ECL).
El mecanismo propuesto implica el anión radical de oxalato (C2O4•) y el anión radical de dióxido de carbono (CO2•).
La evidencia experimental de este mecanismo ha sido limitada debido a la complejidad del sistema y los intermedios de corta duración.

Objetivo del estudio:

Demostrar experimentalmente el mecanismo propuesto de oxidación del oxalato.
Para determinar el tiempo de vida de los radicales intermedios clave.
Aclarar el papel del oxalato como coreactivo en la ECL.

Principales métodos:

Se utilizó microscopía electroquímica de barrido a nanoescala (SECM) en modo de generación de punta/colección de sustrato (TG/SC).
Se utilizan microelectrodos de platino (UMEs) en N,N-dimetilformamida (DMF) anhidro.
Se investigó la influencia de la distancia entre la punta y el sustrato en los productos intermedios capturados.

Principales resultados:

Anión radical de dióxido de carbono identificado (CO2•−) como el intermediario primario a distancias de hueco >73 nm.
Se identificó el anión radical oxalato (C2O4•−) como el intermediario predominante a distancias de hueco <73 nm.
Se determinó una vida media de 1,3 μs para el anión radical oxalato (C2O4•−).

Conclusiones:

Proporcionó pruebas experimentales de un mecanismo de oxidación gradual del oxalato.
Se confirmó la formación y las funciones distintas de los intermedios C2O4•− y CO2•−.
Ofreció información sobre la optimización de los sistemas de ECL basados en oxalato.

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