Proving the Formation of Carbonic Acid Hemiesters Using Self-Assembled Monolayers and Electrochemistry

This study demonstrates, for the first time, the formation of a hemiester of carbonic acid on self-assembled monolayers using voltammetric techniques and redox probes. A gold electrode (GE) was modified with 2-mercaptoethanol (ME) through self-assembly. With this modified electrode (GE-ME), a well-d...

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Main Authors: Berlane G. Santos, Fernanda P. Carli, Claudimir L. do Lago, Ivano G. R. Gutz, Lúcio Angnes
Format: Article
Language:English
Published: MDPI AG 2025-03-01
Series:Chemosensors
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Online Access:https://www.mdpi.com/2227-9040/13/3/93
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author Berlane G. Santos
Fernanda P. Carli
Claudimir L. do Lago
Ivano G. R. Gutz
Lúcio Angnes
author_facet Berlane G. Santos
Fernanda P. Carli
Claudimir L. do Lago
Ivano G. R. Gutz
Lúcio Angnes
author_sort Berlane G. Santos
collection DOAJ
description This study demonstrates, for the first time, the formation of a hemiester of carbonic acid on self-assembled monolayers using voltammetric techniques and redox probes. A gold electrode (GE) was modified with 2-mercaptoethanol (ME) through self-assembly. With this modified electrode (GE-ME), a well-defined peak was observed by differential pulse voltammetry (DPV) for the negatively charged redox probe, ferricyanide/ferrocyanide, [Fe(CN)<sub>6</sub>]<sup>3−</sup>/<sup>4−</sup>, in sodium acetate as an electrolyte adjusted to pH 8.2. In the presence of dissolved CO<sub>2</sub> in equilibrium with bicarbonate, there is a decrease in the ferrocyanide peak current with time (~30% in 60 min), attributed to the formation of hemiester 2-mercapto ethyl carbonate at the GE-ME/solution interface. Similarly, dissolved CO<sub>2</sub> and bicarbonate also affect the electrochemical impedance measurements by increasing resistance to the charge transfer process with time (elevation of Rct values), compatible with the formation of the hemiester. The addition of barium salt led to the displacement of the equilibrium towards BaCO<sub>3</sub> precipitation and consequent dissociation of the hemiester, attested by the recovery of the initial ferricyanide DPV signal. With the positively charged redox probe [Ru(NH<sub>3</sub>)<sub>6</sub>]<sup>2+</sup>, no decrease in the DPV peak was observed during the formation of the hemiester by reaction with bicarbonate. The repulsion of [Fe(CN)<sub>6</sub>]<sup>3−</sup>, but not of [Ru(NH3)<sub>6</sub>]<sup>2+</sup>, suggests that the formed species is the negatively charged 2-mercapto-ethyl carbonate, i.e., the hemiester with a dissociated proton. Due to the lack of a voltammetric signal from the hemiester itself, the formation of a self-assembled layer of thio-alcohol followed by the gradual formation of the corresponding carbonic acid hemiester allowed us to reach an elegant way of electrochemically demonstrating the formation of these species.
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spelling doaj-art-edff148ca2ac434d8d00a6fa068c6ec02025-08-20T02:42:46ZengMDPI AGChemosensors2227-90402025-03-011339310.3390/chemosensors13030093Proving the Formation of Carbonic Acid Hemiesters Using Self-Assembled Monolayers and ElectrochemistryBerlane G. Santos0Fernanda P. Carli1Claudimir L. do Lago2Ivano G. R. Gutz3Lúcio Angnes4Department of Fundamental Chemistry, Institute of Chemistry, University of São Paulo, Av. Prof. Lineu Prestes, 748, São Paulo 05508-000, SP, BrazilDepartment of Fundamental Chemistry, Institute of Chemistry, University of São Paulo, Av. Prof. Lineu Prestes, 748, São Paulo 05508-000, SP, BrazilDepartment of Fundamental Chemistry, Institute of Chemistry, University of São Paulo, Av. Prof. Lineu Prestes, 748, São Paulo 05508-000, SP, BrazilDepartment of Fundamental Chemistry, Institute of Chemistry, University of São Paulo, Av. Prof. Lineu Prestes, 748, São Paulo 05508-000, SP, BrazilDepartment of Fundamental Chemistry, Institute of Chemistry, University of São Paulo, Av. Prof. Lineu Prestes, 748, São Paulo 05508-000, SP, BrazilThis study demonstrates, for the first time, the formation of a hemiester of carbonic acid on self-assembled monolayers using voltammetric techniques and redox probes. A gold electrode (GE) was modified with 2-mercaptoethanol (ME) through self-assembly. With this modified electrode (GE-ME), a well-defined peak was observed by differential pulse voltammetry (DPV) for the negatively charged redox probe, ferricyanide/ferrocyanide, [Fe(CN)<sub>6</sub>]<sup>3−</sup>/<sup>4−</sup>, in sodium acetate as an electrolyte adjusted to pH 8.2. In the presence of dissolved CO<sub>2</sub> in equilibrium with bicarbonate, there is a decrease in the ferrocyanide peak current with time (~30% in 60 min), attributed to the formation of hemiester 2-mercapto ethyl carbonate at the GE-ME/solution interface. Similarly, dissolved CO<sub>2</sub> and bicarbonate also affect the electrochemical impedance measurements by increasing resistance to the charge transfer process with time (elevation of Rct values), compatible with the formation of the hemiester. The addition of barium salt led to the displacement of the equilibrium towards BaCO<sub>3</sub> precipitation and consequent dissociation of the hemiester, attested by the recovery of the initial ferricyanide DPV signal. With the positively charged redox probe [Ru(NH<sub>3</sub>)<sub>6</sub>]<sup>2+</sup>, no decrease in the DPV peak was observed during the formation of the hemiester by reaction with bicarbonate. The repulsion of [Fe(CN)<sub>6</sub>]<sup>3−</sup>, but not of [Ru(NH3)<sub>6</sub>]<sup>2+</sup>, suggests that the formed species is the negatively charged 2-mercapto-ethyl carbonate, i.e., the hemiester with a dissociated proton. Due to the lack of a voltammetric signal from the hemiester itself, the formation of a self-assembled layer of thio-alcohol followed by the gradual formation of the corresponding carbonic acid hemiester allowed us to reach an elegant way of electrochemically demonstrating the formation of these species.https://www.mdpi.com/2227-9040/13/3/93hemiesterCO<sub>2</sub>alcoholcarbonic acidself-assembled monolayer
spellingShingle Berlane G. Santos
Fernanda P. Carli
Claudimir L. do Lago
Ivano G. R. Gutz
Lúcio Angnes
Proving the Formation of Carbonic Acid Hemiesters Using Self-Assembled Monolayers and Electrochemistry
Chemosensors
hemiester
CO<sub>2</sub>
alcohol
carbonic acid
self-assembled monolayer
title Proving the Formation of Carbonic Acid Hemiesters Using Self-Assembled Monolayers and Electrochemistry
title_full Proving the Formation of Carbonic Acid Hemiesters Using Self-Assembled Monolayers and Electrochemistry
title_fullStr Proving the Formation of Carbonic Acid Hemiesters Using Self-Assembled Monolayers and Electrochemistry
title_full_unstemmed Proving the Formation of Carbonic Acid Hemiesters Using Self-Assembled Monolayers and Electrochemistry
title_short Proving the Formation of Carbonic Acid Hemiesters Using Self-Assembled Monolayers and Electrochemistry
title_sort proving the formation of carbonic acid hemiesters using self assembled monolayers and electrochemistry
topic hemiester
CO<sub>2</sub>
alcohol
carbonic acid
self-assembled monolayer
url https://www.mdpi.com/2227-9040/13/3/93
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AT claudimirldolago provingtheformationofcarbonicacidhemiestersusingselfassembledmonolayersandelectrochemistry
AT ivanogrgutz provingtheformationofcarbonicacidhemiestersusingselfassembledmonolayersandelectrochemistry
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