ISSN:
1433-0768
Keywords:
Key wordsSpectroelectrochemistry
;
Diffuse reflectance spectrometry
;
Solid state electrochemistry
;
Voltammetry
;
Microscopy
Source:
Springer Online Journal Archives 1860-2000
Topics:
Chemistry and Pharmacology
Notes:
Abstract An instrumental setup is described which allows electrochemical measurements to be performed with solid particles immobilized on the surface of a graphite electrode with in situ recording of diffuse reflectance spectra under an incident light microscope. The instrument used includes a special electrochemical cell and a microscope which is interfaced by a light␣guide to a transputer-integrated photodiode-array spectrometer allowing measurements ranging from 320 to 950 nm with a resolution of 3.2 nm/pixel and a PC-interfaced potentiostat. The 0R0 geometry of the optical arrangement and the use of crossed polarization filters for blocking specular reflectance makes it possible to use the Kubelka-Munk function for quantifying the optical measurements. The above instrument has been used for the study of the electrochromic system of solid silver octacyanomolybdate(IV/V) adjacent to a silver nitrate solution. The in situ diffuse reflec tance spectroelectrochemical measurements prove that the electrochemical reaction starts at the graphite/sample interface and then advances into the bulk of the sample towards the sample/electrolyte interface. The ratios Red:Ox determined by spectrometry and chronocoulometry as a function of electrode potentials are identical.
Type of Medium:
Electronic Resource
URL:
http://dx.doi.org/10.1007/s100080050023
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