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Issue 27, 2021
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Mass spectrometric detection of fleeting neutral intermediates generated in electrochemical reactions

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Abstract

Towards the goal of on-line monitoring of transient neutral intermediates during electrochemical reactions, an electrochemistry-neutral reionization-mass spectrometry (EC-NR-MS) technique was developed in this work. The EC-NR setup consisted of a customized EC flow cell, a sonic spray ionization source, a heating tube, an ion deflector and an electrospray ionization source, which were respectively used for the precise control of the electrochemical reaction, solution nebulization, droplet desolvation, ion deflection and neutral intermediate ionization. Based on the EC-NR-MS approach, some long-sought neutral radicals including TPrA˙, DBAE˙ and TEOA˙, which belong to important reductive intermediates in electrochemiluminescence (ECL) reactions, were successfully identified which helps to clarify the previously unproven ECL reaction mechanism. These findings were also supported by spin-trapping experiments and the tandem MS technique. Accordingly, the EC-NR-MS method provides a direct solution for studying complicated electrochemical reactions, especially for detecting short-lived neutral radicals as well as ionic intermediates.

Graphical abstract: Mass spectrometric detection of fleeting neutral intermediates generated in electrochemical reactions

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Supplementary files

Article information


Submitted
09 Mar 2021
Accepted
09 Jun 2021
First published
12 Jun 2021

This article is Open Access
All publication charges for this article have been paid for by the Royal Society of Chemistry

Chem. Sci., 2021,12, 9494-9499
Article type
Edge Article

Mass spectrometric detection of fleeting neutral intermediates generated in electrochemical reactions

J. Liu, K. Yu, H. Zhang, J. He, J. Jiang and H. Luo, Chem. Sci., 2021, 12, 9494 DOI: 10.1039/D1SC01385H

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