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Fig. 5.43 Influence of methanol adsorption on the hydrogen adsorption at a bright platinum electrode in 0.5 M H 2 SO 4 . This is the same electrode as in Fig. 5.40 polarized by a single potential sweep (dE/df = 30 V s 1 ) from E = 0.5V to E = 0.1V. Concentration of methanol (in mol dm~3 from bottom to top): 0, 10~4, 10~\ 10~2, 10~\ 5. Methanol was adsorbed at " = 0.5 V during 2min (the equilibrium coverage was achieved), t = 20 C. (By courtesy of J. Weber) the adsorbed substance is 0 =
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The dependence of the relative coverage of the platinum electrode with methanol on its concentration in solution indicates that the adsorption of methanol obeys the Temkin isotherm (4.3.46). The anodic oxidation of molecular hydrogen dissolved in the electrolyte at a Pt electrode consists of several steps: the transport of hydrogen
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molecules to the electrode, their dissociation with simultaneous adsorption of atomic hydrogen on the electrode (reversed Tafel reaction (5.7.2)) and its subsequent oxidation. The shape of the polarization curve depends on which of these processes is slowest. The adsorption of hydrogen is affected by the adsorption of anions, occurring at positive potentials. The adsorbed anions, especially iodide, decrease both the adsorption energy and the maximal amount of hydrogen adsorbed. The effect of iodide is analogous to that of substances termed cathodic poisons, such as mercury ions, trivalent arsenic or cyanide ions. The retarding effect of adsorbed anions is especially apparent for the anodic ionization of hydrogen dissolved in solution at a platinum electrode. Figure 5.44 shows the voltammograms for this process at a rotating disk electrode. In the vicinity of the equilibrium potential, this process is controlled by convective diffusion (see Eqs 5.4.20 and 5.4.23); at slightly more positive potentials a limiting current appears that is then independent of the potential. At much more positive potentials, the surface process is retarded by the adsorption of sulphate anions and becomes the
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Fig. 5.44 The voltammogram of molecular hydrogen at a rotating bright platinum disk electrode in 0.5 M H2SO4, pHl = 105 Pa, 25 C. The rotation speed ^ ( s 1 ) is indicated at each curve. (According to E. A. Aykazyan and A. I. Fedorova)
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364 rate-controlling step in place of diffusion. The higher the rotation rate of the electrode, the sooner the transition occurs between the transport-controlled process and the surface-controlled process. The current increase at 1.6 V corresponds to platinum 'surface oxide' formation. The electrocatalytic oxidation of lower aliphatic compounds such as alcohols, aldehydes, hydrocarbons and formic and oxalic acid at platinumgroup electrodes has a number of typical features. The chemisorption process usually involves the dissociation of several hydrogen atoms from the original molecule and a so-far not completely identified intermediate (often termed 'reduced carbon dioxide' for the reactions of methanol, formaldehyde and formic acid) remains adsorbed on the electrode. At electrode potentials higher than 0.35 V (versus a hydrogen electrode located in the same solution and saturated with hydrogen at standard pressure) all the hydrogen atoms formed during chemisorption are oxidized anodically. The adsorbed intermediate can be oxidized at potentials higher than +0.4 V; the larger the coverage by the adsorbed intermediate, the higher the threshold potential of the anodic oxidation. This phenomenon can be explained by the 'pair mechanism' of the anodic process, proposed by S. Gilman. Water molecules in the vicinity of the adsorbed intermediate are highly polarized, facilitating their oxidation. The OH radicals formed then immediately attack this intermediate in a surface reaction. At a constant potential, the rate of this process decreases because the number of sites available for oxidation of water gradually diminishes. However, if a pulse of increasing positive potential is applied to the electrode, then the oxidation of water resulting in OH radical formation is accelerated by increasing the potential and the rate of the overall electrode process is enhanced, as shown for methanol in Fig. 5.45. Clearly, the rate of the process at low potentials decreases with increasing concentration of methanol owing to the retarding effect of electrode coverage with the intermediate. In contrast, at higher potentials, the rate of the process increases with increasing concentration (the oxidation of water is so fast that the overall rate increases with increasing surface coverage). So far, several examples have been given of the inhibition of electrocatalytic processes. This retardation is a result of occupation of the catalytically more active sites by electroinactive components of the electrolyte, preventing interaction of the electroactive substances with these sites. The electrode process can also be inhibited by the formation of oxide layers on the surface and by the adsorption of less active intermediates and also of the products of the electrode process. The inhibition of electrode processes as a result of the adsorption of electroinactive surfactants has been studied in detail at catalytically inactive mercury electrodes. In contrast to solid metal electrodes where knowledge of the structure of the electrical double layer is small, it is often possible to determine whether the effect of adsorption on the electrode process at mercury electrodes is solely due to electrostatics (a change in potential 02)
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