Accelerating Electrochemical Reactions in a Voltage‐Controlled Interfacial Microreactor

Cheng, Heyong; Tang, Shuli; Yang, Tingyuan; Xu, Shiqing; Yan, Xingru

doi:10.1002/anie.202007736

Cited by 48 publications

(50 citation statements)

References 75 publications

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“…Yan et al to develop an interfacial microreactor to enhance the rates of electrochemical reactions in nanoESI, which are otherwise slow in bulk. [46] They reported a voltage-controlled interfacial microreactor formed at the Taylor cone in a nanoESI emitter ( Figure 2c). The novel interfacial microreactor was found to accelerate electrochemical reactions in dripping and spindle, and most microdripping spray modes by applying relatively low voltages and in the ESI emitter with a much larger orifice (> 50 μm) than regular ones.…”

Section: Electrochemistry In Nanoesimentioning

confidence: 99%

“…[42] with permission from Wiley-VCH, Ref. [46] with permission from Wiley-VCH, and Ref. [61] with permission from the Royal Society of Chemistry.…”

Section: Electrochemistry In Nanoesimentioning

confidence: 99%

“…Double-barrel nanoESI is typically achieved by using a thetashaped capillary (two independent channels physically isolated by a glass septum). [43][44][45][46][47] Theta capillary based-nanoESI is capable of rapid small-volume mixing for studying complex reactions, [56,57] protein folding and unfolding, [58,59] and hydrogendeuterium exchange. [60] The rapid mixing feature of the theta capillary is also beneficial to electrochemical reactions followed by MS detection of intermediates.…”

Section: Electrochemistry In Double-barrel Nanoesimentioning

confidence: 99%

“…Double‐barrel nanoESI is typically achieved by using a theta‐shaped capillary (two independent channels physically isolated by a glass septum) [43–47] . Theta capillary based‐nanoESI is capable of rapid small‐volume mixing for studying complex reactions, [56,57] protein folding and unfolding, [58,59] and hydrogen‐deuterium exchange [60] .…”

Section: Electrochemistry In Ms Ion Sourcesmentioning

confidence: 99%

“…This motivated Yan et al. to develop an interfacial microreactor to enhance the rates of electrochemical reactions in nanoESI, which are otherwise slow in bulk [46] . They reported a voltage‐controlled interfacial microreactor formed at the Taylor cone in a nanoESI emitter (Figure 2c).…”

Section: Electrochemistry In Ms Ion Sourcesmentioning

confidence: 99%

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Recent Advances of In‐Source Electrochemical Mass Spectrometry

et al. 2021

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Hyphenation of electrochemistry (EC) and mass spectrometry has become a powerful tool to study redox processes. Approaches that can achieve this hyphenation include integrating chromatography/electrophoresis between electroinduced redox reactions and detection of products, coupling an EC flow cell to a mass spectrometer, and performing electrochemical reactions inside the ion source of a mass spectrometer. The first two approaches have been well reviewed elsewhere. This Minireview highlights the inherent electrochemical properties of many mass spectrometry ion sources and their roles in the coupling of electrochemistry and mass spectrometric analysis. Development of modified ion sources that allow the compatibility of electrochemistry with ionization processes is also surveyed. Applications of different in-source electrochemical devices are provided including intermediate capturing, bioanalytical studies, nanoparticle formation, electrosynthesis, and electrode imaging.

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Section: Electrochemistry In Nanoesimentioning

confidence: 99%

“…[42] with permission from Wiley-VCH, Ref. [46] with permission from Wiley-VCH, and Ref. [61] with permission from the Royal Society of Chemistry.…”

Section: Electrochemistry In Nanoesimentioning

confidence: 99%

Section: Electrochemistry In Double-barrel Nanoesimentioning

confidence: 99%

Section: Electrochemistry In Ms Ion Sourcesmentioning

confidence: 99%

Section: Electrochemistry In Ms Ion Sourcesmentioning

confidence: 99%

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Recent Advances of In‐Source Electrochemical Mass Spectrometry

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Dissecting the Flash Chemistry of Electrogenerated Reactive Intermediates by Microdroplet Fusion Mass Spectrometry

Wang

Zhang

et al. 2021

Angewandte Chemie

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A novel mass spectrometric method for probing the flash chemistry of electrogenerated reactive intermediates was developed based on rapid collision mixing of electrosprayed microdroplets by using a theta‐glass capillary. The two individual microchannels of the theta‐glass capillary are asymmetrically or symmetrically fabricated with a carbon bipolar electrode to produce intermediates in situ. Microdroplets containing the newly formed intermediates collide with those of the invoked reactants at sub‐10 microsecond level, making it a powerful tool for exploring their ultrafast initial transformations. As a proof‐of‐concept, we present the identification of the key radical cation intermediate in the oxidative dimerization of 8‐methyl‐1,2,3,4‐tetrahydroquinoline and also the first disclosure of previously hidden nitrenium ion involved reaction pathway in the C−H/N−H cross‐coupling between N,N′‐dimethylaniline and phenothiazine.

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In Situ Probing and Identification of Electrochemical Reaction Intermediates by Floating Electrolytic Electrospray Mass Spectrometry

et al. 2023

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The in-depth study of electrochemical (EC) synthesis can require a powerful mass spectrometry (MS) analytical platform which can discover and identify fleeting intermediates in EC reactions. Here we report a floating electrolytic electrospray ionization (FE-ESI) strategy that can perform EC processes in a floating electrolytic cell and monitor intermediates by highresolution MS. Compared with previous EC-MS methods, a significant advantage of FE-ESI-MS is that it allows one to modulate the electrolytic and electrospray process individually, ensuring its high sensitivity in discovering intermediates and universality to investigate redox reactions in different scenarios. This powerful platform has been successfully used to investigate the EC reductive coupling of p-tolylboronic acid and pnitrotoluene. A series of nitrene intermediates were discovered and identified by FE-ESI-MS, indicating that a hidden mechanism involving nitrene formation might play a key role in EC reductive coupling process.

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Accelerating Electrochemical Reactions in a Voltage‐Controlled Interfacial Microreactor

Cited by 48 publications

References 75 publications

Recent Advances of In‐Source Electrochemical Mass Spectrometry

Recent Advances of In‐Source Electrochemical Mass Spectrometry

Dissecting the Flash Chemistry of Electrogenerated Reactive Intermediates by Microdroplet Fusion Mass Spectrometry

In Situ Probing and Identification of Electrochemical Reaction Intermediates by Floating Electrolytic Electrospray Mass Spectrometry

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