Nanostructured Pd hydride microelectrodes: In situ monitoring of pH variations in a porous medium

Mara Serrapede, G L Pesce, R J Ball, Guy Denuault

Research output: Contribution to journalArticle

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Abstract

In this study we report the exceptional potentiometric properties of pH microprobes made with nanostructured palladium hydride microelectrodes and demonstrate their application by monitoring pH variations resulting from a reaction confined in a porous medium.

Their potentiometric response was found to be reproducible and stable over several hours but primarily Nernstian over a remarkably wide pH range, including alkaline conditions up to pH 14. Continuous operation was demonstrated by reloading hydrogen at regular intervals to maintain the correct hydride
composition thereby alleviating the need for calibration. These properties were validated by detecting pH transients during the carbonation of Ca(OH)2 within a fibrous mesh. Experimental pHs recorded in situ were in excellent agreement with theoretical calculations for the Co2 partial pressures considered. Results also showed that the electrodes were sufficiently sensitive to differentiate between the formation of vaterite and calcite, two polymorphs of CaCO3. These nanostructured microelectrodes are uniquely suited to the determination of pH in highly alkaline solutions, particularly those arising from interfacial reactions at solid and porous surfaces and are thus highly appropriate as pH sensing tips in scanning electrochemical microscopy.

LanguageEnglish
Pages5758-5765
Number of pages8
JournalAnalytical Chemistry
Volume86
Issue number12
Early online date12 May 2014
DOIs
StatusPublished - 17 Jun 2014

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Calcium Carbonate
Microelectrodes
Hydrides
Porous materials
Carbonation
Monitoring
Surface chemistry
Polymorphism
Partial pressure
Hydrogen
Microscopic examination
Calibration
Scanning
Electrodes
Chemical analysis
palladium hydride

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Nanostructured Pd hydride microelectrodes : In situ monitoring of pH variations in a porous medium. / Serrapede, Mara; Pesce, G L; Ball, R J; Denuault, Guy.

In: Analytical Chemistry, Vol. 86, No. 12, 17.06.2014, p. 5758-5765.

Research output: Contribution to journalArticle

Serrapede, Mara ; Pesce, G L ; Ball, R J ; Denuault, Guy. / Nanostructured Pd hydride microelectrodes : In situ monitoring of pH variations in a porous medium. In: Analytical Chemistry. 2014 ; Vol. 86, No. 12. pp. 5758-5765
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