Recent advances and applications of electrochemical mass spectrometry for real-time monitoring of electrochemical reactions

Abstract

Real-time monitoring of electrochemical reactions is crucial for advancing energy conversion and storage, electrocatalysis, organic electrosynthesis, and electroanalysis. Despite progress in in situ spectroscopic and electrochemical techniques, these methods fail to directly resolve and track multiple electrogenerated species simultaneously during electrochemical processes. Electrochemical mass spectrometry (EC-MS) bridges this gap by providing direct molecular-level compositional and structural information while simultaneously monitoring the evolution of newborn species at the electrode–electrolyte interfaces (EEIs). Propelled by the ongoing improvements in ionization sources and electrochemical cells, EC-MS methods have broadened the functional scope from online detection of reaction products to the rapid capture of fleeting intermediates and, most recently, to simultaneous real-time tracking of the dynamics of multiple intermediates. This progressive advancement establishes EC-MS as a robust methodology for mechanistic investigation of electrochemical reactions. This review focuses on the recent advances in EC-MS methods and their applications in exploring organic electrosynthesis, electrocatalysis, lithium-ion batteries (LIBs) and electrochemiluminescence (ECL). Finally, we outline the current limitations and future directions for EC-MS technology, forecasting its expanding utility in electrochemical reaction monitoring.