biostudies-literatureZhang GEngineering and Physical Sciences Research Council (EPSRC)National Natural Science Foundation of ChinaState Key Laboratory of CatalysisDalian Institute of Chemical Physics, Chinese Academy of SciencesEngineering and Physical Sciences Research CouncilNational Natural Science Foundation of China-China Academy of General Technology Joint Fund for Basic Researche202312607https://www.ebi.ac.uk/biostudies/studies/S-EPMC10952920biostudies-literatureUnknown62(48)The mechanistic understanding of electrochemical CO₂ reduction reaction (CO₂ RR) requires a rapid and accurate characterisation of product distribution to unravel the activity and selectivity, which is yet hampered by the lack of advanced correlative approaches. Here, we present the time-resolved identification of CO₂ RR products by using the synchronised electrochemistry-mass spectrometry (sEC-MS). Transients in product formation can be readily captured in relation to electrochemical conditions. Moreover, a soft ionisation (SI) strategy is developed in MS for the direct observation of CO, immune to the interference of CO₂ fragments. With the sEC-MS-SI, the kinetic information, such as Tafel slopes and onset potentials, for a myriad of CO<sub>2</Angewandte Chemie (International ed. in English)Time-Resolved Product Observation for CO₂ Electroreduction Using Synchronised Electrochemistry-Mass Spectrometry with Soft Ionisation (sEC-MS-SI).PMC10952920EP/P024807/1DICP I20212522202194Zhang GKucernak AfalseTime-Resolved Product Observation for CO₂ Electroreduction Using Synchronised Electrochemistry-Mass Spectrometry with Soft Ionisation (sEC-MS-SI).The mechanistic understanding of electrochemical CO₂ reduction reaction (CO₂ RR) requires a rapid and accurate characterisation of product distribution to unravel the activity and selectivity, which is yet hampered by the lack of advanced correlative approaches. Here, we present the time-resolved identification of CO₂ RR products by using the synchronised electrochemistry-mass spectrometry (sEC-MS). Transients in product formation can be readily captured in relation to electrochemical conditions. Moreover, a soft ionisation (SI) strategy is developed in MS for the direct observation of CO, immune to the interference of CO₂ fragments. With the sEC-MS-SI, the kinetic information, such as Tafel slopes and onset potentials, for a myriad of CO<sub>2</2023-01-01T00:00:00Z2023 Nov2026-07-14T21:18:07.941Z2024-11-20T03:26:46.465ZS-EPMC109529203780161210.1002/anie.202312607