Rotating disk voltametry

For the in situ characterization of modified electrodes, the method of choice is electrochemical analysis by cyclic voltammetry, ac voltammetry, chronoamperometry or chronocoulometry, or rotating disk voltametry. Cyclic voltammograms are easy to interpret from a qualitative point of view (Fig, 1). The other methods are less direct but they can yield quantitative data more readily. 

It is our belief that a full and detailed understanding of the electron-transfer properties of organometallic complexes can be achieved only by a combination of chemical and electrochemical studies the use of one alone can lead to erroneous conclusions. Because we have insufficient space to provide a discussion of the theory and practice of elementary electrochemical techniques we refer the reader to several excellent treatments which also include an explanation of commonly used terminology (25-30). The synthetic chemist should not be deterred from routinely using techniques such as cyclic voltametry (CV),1 voltametry at rotating metal disk electrodes, or controlled potential electrolysis (CPE), coulometry, and chronoamperometry. The proper employment of such techniques, for which instrumentation is readily available, should prove sufficient for all but the most detailed studies. 

Figure 29.6 shows a polarization curve where the current is plotted against the voltage.The data can be obtained from a potentiostat setup, shown in Fig. 29.7. Here, we have three electrodes in the plating solution. The first is a counter electrode and is usually made of copper or platinum the second is the working electrode and is a rotating platinum disk and the third is the reference electrode, like a double-junction calomel. Voltage is applied between the working and the reference electrodes, and the ensuing current is measured between the working and the counter electrodes. This is the principle upon which cyclic voltametrie stripping (CVS)...

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