Synchrotron Infrared Radiation for Electrochemical External Reflection Spectroscopy: A Case Study Using Ferrocyanide

Synchrotron infrared radiation has been successfully coupled through an infrared (IR) microscope to a thin-cavity external reflectance cell to study the diffusion controlled redox of a ferrocyanide solution. Excellent signal-to-noise ratios were achieved even at aperture settings close to the diffra...

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Published inAnalytical chemistry (Washington) Vol. 83; no. 10; pp. 3632 - 3639
Main Authors Rosendahl, Scott M, Borondics, Ferenc, May, Tim E, Pedersen, Tor M, Burgess, Ian J
Format Journal Article
LanguageEnglish
Published Washington, DC American Chemical Society 15.05.2011
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Abstract Synchrotron infrared radiation has been successfully coupled through an infrared (IR) microscope to a thin-cavity external reflectance cell to study the diffusion controlled redox of a ferrocyanide solution. Excellent signal-to-noise ratios were achieved even at aperture settings close to the diffraction limit. Comparisons of noise levels as a function of aperture size demonstrate that this can be attributed to the high brilliance of synchrotron radiation relative to a conventional thermal source. Time resolved spectroscopic studies of diffusion controlled redox behavior have been measured and compared to purely electrochemical responses of the thin-cavity cell. Marked differences between the two measurements have been explained by analyzing diffusion in both the axial (linear) and radial dimensions. Whereas both terms contribute to the measured current and charge, only species that originate in the volume element above the electrode and diffuse in the direction perpendicular to the electrode surface are interrogated by IR radiation. Implications for the use of ultramicroelectrodes and synchrotron IR (SIR) to study electrochemical processes in the submillisecond time domain are discussed.
AbstractList Synchrotron infrared radiation has been successfully coupled through an infrared (IR) microscope to a thin-cavity external reflectance cell to study the diffusion controlled redox of a ferrocyanide solution. Excellent signal-to-noise ratios were achieved even at aperture settings close to the diffraction limit. Comparisons of noise levels as a function of aperture size demonstrate that this can be attributed to the high brilliance of synchrotron radiation relative to a conventional thermal source. Time resolved spectroscopic studies of diffusion controlled redox behavior have been measured and compared to purely electrochemical responses of the thin-cavity cell. Marked differences between the two measurements have been explained by analyzing diffusion in both the axial (linear) and radial dimensions. Whereas both terms contribute to the measured current and charge, only species that originate in the volume element above the electrode and diffuse in the direction perpendicular to the electrode surface are interrogated by IR radiation. Implications for the use of ultramicroelectrodes and synchrotron IR (SIR) to study electrochemical processes in the submillisecond time domain are discussed.
Synchrotron infrared radiation has been successfully coupled through an infrared (IR) microscope to a thin-cavity external reflectance cell to study the diffusion controlled redox of a ferrocyanide solution. Excellent signal-to-noise ratios were achieved even at aperture settings close to the diffraction limit. Comparisons of noise levels as a function of aperture size demonstrate that this can be attributed to the high brilliance of synchrotron radiation relative to a conventional thermal source. Time resolved spectroscopic studies of diffusion controlled redox behavior have been measured and compared to purely electrochemical responses of the thin-cavity cell. Marked differences between the two measurements have been explained by analyzing diffusion in both the axial (linear) and radial dimensions. Whereas both terms contribute to the measured current and charge, only species that originate in the volume element above the electrode and diffuse in the direction perpendicular to the electrode surface are interrogated by IR radiation. Implications for the use of ultramicroelectrodes and synchrotron IR (SIR) to study electrochemical processes in the submillisecond time domain are discussed. [PUBLICATION ABSTRACT]
Author Rosendahl, Scott M
Burgess, Ian J
Borondics, Ferenc
May, Tim E
Pedersen, Tor M
AuthorAffiliation University of Saskatchewan
Canadian Light Source
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Issue 10
Keywords Microscope
Noise
Electrochemical method
Size
Use
Time
Ultramicroelectrode
Case study
Reflection spectrometry
Time resolution
Volume
Infrared radiation
Hexacyanoferrates II
Limit
Diffusion
Comparative study
Synchrotron radiation
Reflectance
Signal to noise ratio
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Snippet Synchrotron infrared radiation has been successfully coupled through an infrared (IR) microscope to a thin-cavity external reflectance cell to study the...
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SubjectTerms Analytical chemistry
Chemistry
Diffusion
Electrocatalysis
Electrochemical methods
Electrochemical Techniques - methods
Electrodes
Exact sciences and technology
Ferrocyanides - chemistry
Infrared radiation
Oxidation-Reduction
Spectrometric and optical methods
Spectrophotometry, Infrared - instrumentation
Spectrophotometry, Infrared - methods
Spectrum analysis
Synchrotrons
Title Synchrotron Infrared Radiation for Electrochemical External Reflection Spectroscopy: A Case Study Using Ferrocyanide
URI http://dx.doi.org/10.1021/ac200250s
https://www.ncbi.nlm.nih.gov/pubmed/21486090
https://www.proquest.com/docview/870690589
https://search.proquest.com/docview/866532893
Volume 83
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