Carbon fiber brush electrode as a novel substrate for atmospheric solids analysis probe (ASAP) mass spectrometry: Electrochemical oxidation of brominated phenols

A carbon fiber brush electrode (CFBE) was newly designed and used as a substrate for both controlled potential electrolysis and atmospheric solids analysis probe (ASAP) mass spectrometry. Electropolymerized and strongly adsorbed products of electrolysis were directly desorbed and ionized from the el...

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Veröffentlicht in:Analytica chimica acta 2018-01, Vol.999, p.60-68
Hauptverfasser: Skopalová, Jana, Barták, Petr, Bednář, Petr, Tomková, Hana, Ingr, Tomáš, Lorencová, Iveta, Kučerová, Pavla, Papoušek, Roman, Borovcová, Lucie, Lemr, Karel
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container_title Analytica chimica acta
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creator Skopalová, Jana
Barták, Petr
Bednář, Petr
Tomková, Hana
Ingr, Tomáš
Lorencová, Iveta
Kučerová, Pavla
Papoušek, Roman
Borovcová, Lucie
Lemr, Karel
description A carbon fiber brush electrode (CFBE) was newly designed and used as a substrate for both controlled potential electrolysis and atmospheric solids analysis probe (ASAP) mass spectrometry. Electropolymerized and strongly adsorbed products of electrolysis were directly desorbed and ionized from the electrode surface. Electrochemical properties of the electrode investigated by cyclic voltammetry revealed large electroactive surface area (23 ± 3 cm2) at 1.3 cm long array of carbon fibers with diameter 6–9 μm. Some products of electrochemical oxidation of pentabromophenol and 2,4,6-tribromophenol formed a compact layer on the carbon fibers and were analyzed using ASAP. Eleven new oligomeric products were identified including quinones and biphenoquinones. These compounds were not observed previously in electrolyzed solutions by liquid or gas chromatography/mass spectrometry. The thickness around 58 nm and 45 nm of the oxidation products layers deposited on carbon fibers during electrolysis of pentabromophenol and 2,4,6-tribromophenol, respectively, was estimated from atomic force microscopy analysis and confirmed by scanning electron microscopy with energy-dispersive X-ray spectroscopy measurements. [Display omitted] •New mode of coupling of electrochemistry and mass spectrometry is presented.•Large surface carbon fiber brush electrode was designed for atmospheric solids analysis probe.•Electrochemically generated species were directly desorbed and ionized from electrode.•Insoluble oligomeric and strongly adsorbed bromophenol oxidation products were identified.
doi_str_mv 10.1016/j.aca.2017.11.024
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Electropolymerized and strongly adsorbed products of electrolysis were directly desorbed and ionized from the electrode surface. Electrochemical properties of the electrode investigated by cyclic voltammetry revealed large electroactive surface area (23 ± 3 cm2) at 1.3 cm long array of carbon fibers with diameter 6–9 μm. Some products of electrochemical oxidation of pentabromophenol and 2,4,6-tribromophenol formed a compact layer on the carbon fibers and were analyzed using ASAP. Eleven new oligomeric products were identified including quinones and biphenoquinones. These compounds were not observed previously in electrolyzed solutions by liquid or gas chromatography/mass spectrometry. 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[Display omitted] •New mode of coupling of electrochemistry and mass spectrometry is presented.•Large surface carbon fiber brush electrode was designed for atmospheric solids analysis probe.•Electrochemically generated species were directly desorbed and ionized from electrode.•Insoluble oligomeric and strongly adsorbed bromophenol oxidation products were identified.</description><identifier>ISSN: 0003-2670</identifier><identifier>EISSN: 1873-4324</identifier><identifier>DOI: 10.1016/j.aca.2017.11.024</identifier><identifier>PMID: 29254575</identifier><language>eng</language><publisher>Netherlands: Elsevier B.V</publisher><subject>Ambient ionization ; Atmospheric solids analysis probe mass spectrometry ; Atomic force microscopy ; Bromination ; Bromophenols ; Carbon ; Carbon fiber brush electrode ; Carbon fibers ; Electrochemical analysis ; Electrochemical oxidation ; Electrochemistry ; Electrodes ; Electrolysis ; Electron microscopy ; Electropolymerization ; Energy dispersive X ray spectroscopy ; Fibers ; Gas chromatography ; Mass spectrometry ; Mass spectroscopy ; Oxidation ; Oxidation products ; Phenols ; Quinones ; Scanning electron microscopy ; Solids ; Substrates ; Tribromophenol ; X-ray spectroscopy</subject><ispartof>Analytica chimica acta, 2018-01, Vol.999, p.60-68</ispartof><rights>2017 Elsevier B.V.</rights><rights>Copyright © 2017 Elsevier B.V. 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Electropolymerized and strongly adsorbed products of electrolysis were directly desorbed and ionized from the electrode surface. Electrochemical properties of the electrode investigated by cyclic voltammetry revealed large electroactive surface area (23 ± 3 cm2) at 1.3 cm long array of carbon fibers with diameter 6–9 μm. Some products of electrochemical oxidation of pentabromophenol and 2,4,6-tribromophenol formed a compact layer on the carbon fibers and were analyzed using ASAP. Eleven new oligomeric products were identified including quinones and biphenoquinones. These compounds were not observed previously in electrolyzed solutions by liquid or gas chromatography/mass spectrometry. The thickness around 58 nm and 45 nm of the oxidation products layers deposited on carbon fibers during electrolysis of pentabromophenol and 2,4,6-tribromophenol, respectively, was estimated from atomic force microscopy analysis and confirmed by scanning electron microscopy with energy-dispersive X-ray spectroscopy measurements. 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Electropolymerized and strongly adsorbed products of electrolysis were directly desorbed and ionized from the electrode surface. Electrochemical properties of the electrode investigated by cyclic voltammetry revealed large electroactive surface area (23 ± 3 cm2) at 1.3 cm long array of carbon fibers with diameter 6–9 μm. Some products of electrochemical oxidation of pentabromophenol and 2,4,6-tribromophenol formed a compact layer on the carbon fibers and were analyzed using ASAP. Eleven new oligomeric products were identified including quinones and biphenoquinones. These compounds were not observed previously in electrolyzed solutions by liquid or gas chromatography/mass spectrometry. 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subjects Ambient ionization
Atmospheric solids analysis probe mass spectrometry
Atomic force microscopy
Bromination
Bromophenols
Carbon
Carbon fiber brush electrode
Carbon fibers
Electrochemical analysis
Electrochemical oxidation
Electrochemistry
Electrodes
Electrolysis
Electron microscopy
Electropolymerization
Energy dispersive X ray spectroscopy
Fibers
Gas chromatography
Mass spectrometry
Mass spectroscopy
Oxidation
Oxidation products
Phenols
Quinones
Scanning electron microscopy
Solids
Substrates
Tribromophenol
X-ray spectroscopy
title Carbon fiber brush electrode as a novel substrate for atmospheric solids analysis probe (ASAP) mass spectrometry: Electrochemical oxidation of brominated phenols
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