Scanning Electrochemical Microscopy with Forced Convection Introduced by High-Precision Stirring.

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Title: Scanning Electrochemical Microscopy with Forced Convection Introduced by High-Precision Stirring.
Authors: Iffelsberger, Christian1, Vatsyayan, Preety1, Matysik, Frank-Michael1 frank-michael.matysik@ur.de
Source: Analytical Chemistry. 2/7/2017, Vol. 89 Issue 3, p1658-1664. 7p.
Subjects: Electrolyte analysis, Forced convection, Solution (Chemistry), Electrochemical analysis, Scanning electron microscopy, Analytical chemistry
Abstract: In the present report the well-known advantages of hydrodynamic mass transport in electrochemical systems are used in combination with scanning electrochemical microscopy (SECM). The hydrodynamic SECM system integrates a high-precision stirring device into the experimental setup. The well-defined stirring of the SECM electrolyte results in steady state diffusion layer characteristics in the vicinity of large substrate electrodes operated in chronoamperometric measuring mode. For a range of rotation frequencies of a rotating cylinder the thickness and the stability of the diffusion layer was studied by hydrodynamic SECM in the substrate generation/tip collection (SG/TC) as well as in the competition mode using ferrocene methanol as redox mediator. Different UME probe dimensions ranging from Pt diameters of 20 μm down to 0.6 μm were used. The smallest probe with dPt = 0.6 μm was found most suitable for these studies due to the almost convection-independent amperometric response associated with subμm electrodes. Additionally, preliminary studies of hydrodynamic SECM imaging of a 2 mm Pt disk electrode surface in the SG/TC mode based on in situ produced hydrogen as a mediator are presented. Comparative images measured in the conventional positive feedback mode in quiescent solution show that hydrodynamic SECM offers attractive complementary information. [ABSTRACT FROM AUTHOR]
Copyright of Analytical Chemistry is the property of American Chemical Society and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)
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  Label: Title
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  Data: Scanning Electrochemical Microscopy with Forced Convection Introduced by High-Precision Stirring.
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  Data: <searchLink fieldCode="AR" term="%22Iffelsberger%2C+Christian%22">Iffelsberger, Christian</searchLink><relatesTo>1</relatesTo><br /><searchLink fieldCode="AR" term="%22Vatsyayan%2C+Preety%22">Vatsyayan, Preety</searchLink><relatesTo>1</relatesTo><br /><searchLink fieldCode="AR" term="%22Matysik%2C+Frank-Michael%22">Matysik, Frank-Michael</searchLink><relatesTo>1</relatesTo><i> frank-michael.matysik@ur.de</i>
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  Data: <searchLink fieldCode="JN" term="%22Analytical+Chemistry%22">Analytical Chemistry</searchLink>. 2/7/2017, Vol. 89 Issue 3, p1658-1664. 7p.
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  Data: <searchLink fieldCode="DE" term="%22Electrolyte+analysis%22">Electrolyte analysis</searchLink><br /><searchLink fieldCode="DE" term="%22Forced+convection%22">Forced convection</searchLink><br /><searchLink fieldCode="DE" term="%22Solution+%28Chemistry%29%22">Solution (Chemistry)</searchLink><br /><searchLink fieldCode="DE" term="%22Electrochemical+analysis%22">Electrochemical analysis</searchLink><br /><searchLink fieldCode="DE" term="%22Scanning+electron+microscopy%22">Scanning electron microscopy</searchLink><br /><searchLink fieldCode="DE" term="%22Analytical+chemistry%22">Analytical chemistry</searchLink>
– Name: Abstract
  Label: Abstract
  Group: Ab
  Data: In the present report the well-known advantages of hydrodynamic mass transport in electrochemical systems are used in combination with scanning electrochemical microscopy (SECM). The hydrodynamic SECM system integrates a high-precision stirring device into the experimental setup. The well-defined stirring of the SECM electrolyte results in steady state diffusion layer characteristics in the vicinity of large substrate electrodes operated in chronoamperometric measuring mode. For a range of rotation frequencies of a rotating cylinder the thickness and the stability of the diffusion layer was studied by hydrodynamic SECM in the substrate generation/tip collection (SG/TC) as well as in the competition mode using ferrocene methanol as redox mediator. Different UME probe dimensions ranging from Pt diameters of 20 μm down to 0.6 μm were used. The smallest probe with dPt = 0.6 μm was found most suitable for these studies due to the almost convection-independent amperometric response associated with subμm electrodes. Additionally, preliminary studies of hydrodynamic SECM imaging of a 2 mm Pt disk electrode surface in the SG/TC mode based on in situ produced hydrogen as a mediator are presented. Comparative images measured in the conventional positive feedback mode in quiescent solution show that hydrodynamic SECM offers attractive complementary information. [ABSTRACT FROM AUTHOR]
– Name: AbstractSuppliedCopyright
  Label:
  Group: Ab
  Data: <i>Copyright of Analytical Chemistry is the property of American Chemical Society and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract.</i> (Copyright applies to all Abstracts.)
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RecordInfo BibRecord:
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    Identifiers:
      – Type: doi
        Value: 10.1021/acs.analchem.6b03764
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      – Code: eng
        Text: English
    PhysicalDescription:
      Pagination:
        PageCount: 7
        StartPage: 1658
    Subjects:
      – SubjectFull: Electrolyte analysis
        Type: general
      – SubjectFull: Forced convection
        Type: general
      – SubjectFull: Solution (Chemistry)
        Type: general
      – SubjectFull: Electrochemical analysis
        Type: general
      – SubjectFull: Scanning electron microscopy
        Type: general
      – SubjectFull: Analytical chemistry
        Type: general
    Titles:
      – TitleFull: Scanning Electrochemical Microscopy with Forced Convection Introduced by High-Precision Stirring.
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            NameFull: Iffelsberger, Christian
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            NameFull: Vatsyayan, Preety
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            NameFull: Matysik, Frank-Michael
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            – D: 07
              M: 02
              Text: 2/7/2017
              Type: published
              Y: 2017
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              Value: 89
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            – TitleFull: Analytical Chemistry
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