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Fig. 5.45 Single-sweep voltammogram of oxidation of methanol in 0.5 M H2SO4, with the same electrode and the same conditions of methanol adsorption as in Fig. 5.43. Concentrations of methanol (mol dm"3): (1) 0, (2) 10"4, (3) 10-*, (4) 10~2, (5) HT1. (By courtesy of J. Weber)
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366 or is the result of some other type of inhibition. The steric effect where the sufficiently close approach of the electroactive substance to the electrode is inhibited is typical for large surface-active molecules. The adsorbed layer of surfactant replacing the layer of water molecules covering the surface of the electrode prevents the reacting species and their solvation shells from forming a configuration suitable for the electrode reaction (see Section 5.3). This leads to a decrease in the value of the rate constant of the electrode reaction. For example, in the case of an irreversible electrode reaction with a rate constant kc and adsorption of an uncharged surfactant, we have fcc = fc0(l-O) + fc1 (5.7.18)
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where k0 and kY are the rate constants for the electrode reaction at unoccupied and occupied sites of the electrode surface, respectively. For the adsorption of surface-active ions, these quantities are also a function of the surface coverage 0. It is very simple to determine the value of 0 = F/F m for a strongly adsorbed substance in electrolysis with a dropping mercury electrode. If a much smaller amount of substance is sufficient for complete electrode coverage than available in the test solution, then the surface concentration of the surface-active substance F is determined by its diffusion to the electrode. The total amount M adsorbed on the electrode in time t (A is the surface of the electrode according to Eq. (4.4.4) and F is the surface excess in moles per square centimetre) is given as
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M = 0.85Fm2/V/3 =
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p Jo \dx/x=0 where Dp(dcp/dx)x=0 is the material flux of the surface-active substance to the electrode, corresponding to the limiting current density and given according to Eq. (2.7.17) by the relationship
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where cp is the concentration of the surface-active substance, Dp is its diffusion coefficient and c is its concentration in the bulk of the solution. The surface concentration at time t is given by the equation deduced by J. Koryta: F = 0.74c (Dp01/2 (5.7.21) If complete coverage of the electrode Fm is practically attained at time 0, then
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Fig. 5.46 The dependence on time of the instantaneous current / at a dropping mercury electrode in a solution of
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0 . 0 8 M C O ( N H 3 ) 6 C 1 3 + 0 . 1 M H 2 S O 4 + 0 . 5 M K2SO4 at the
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electrode potential where - / / d (i.e. the influence of diffusion of the electroactive substance is negligible): (1) in the absence of surfactant; (2) after addition of 0.08% polyvinyl alcohol. The dashed curve has been calculated according to Eq. (5.7.23). (According to J. Kuta and I. Smoler)
The value of Fm can be calculated from Eq. (5.7.21) where F approaches Fm at time t = 6. The instantaneous polarographic current /ads controlled by the rate of the irreversible electrode reaction of substance A is as follows:
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(see Eq. 5.7.18), assuming that kx = 0 and that the current is so small that diffusion of the electroactive substance can be neglected; / is the current in the absence of the surface-active substance. Figure 5.46 shows the time dependence of the instantaneous current in the absence and presence of the surface-active substance. References
Anson, F. C , Patterns of ionic and molecular adsorption at electrodes, Ace. Chem. Res., 8,400(1975). Breiter, M. W., Electrochemical Processes in Fuel Cells, Springer-Verlag, New York, 1969.
368 Kinetics and mechanisms of electrode processes, CTE, 7 (1983) Frumkin, A. N., Hydrogen overvoltage and adsorption phenomena, Part I, Mercury, AE, 1, 65 (1961); Part II, Solid metals, AE, 3, 267 (1963). Gilman, S., The anodic film on platinum electrode, in Electroanalytical Chemistry (Ed. A. J. Bard), Vol. 2, p. I l l , M. Dekker, New York, 1967. Heyrovsky, J., and J. Kuta, see page 343. Hoare, J., The Electrochemistry of Oxygen, Interscience, New York, 1968. Krishtalik, L. I., Hydrogen overvoltage and adsorption phenomena, Part III, Effect of the adsorption energy of hydrogen on overvoltage and the mechanism of the cathodic process, AE, 7, 283 (1970). Krishtalik, L. I., The mechanism of the elementary act of proton transfer in homogeneous and electrode reactions, /. Electroanal. Chem.y 100, 547 (1979). Lamy, C , Electrocatalytic oxidation of organic compounds on noble metals in aqueous solutions, Electrochim. Acta, 29, 1581 (1984). Marcus, R. A., Similarities and differences between electron and proton transfers at electrodes and in solution, Theory of hydrogen evolution reaction, Proc. Electrochem. Soc, 80-3, 1 (1979). Schulze, J. W., and M. A. Habib, Principles of electrocatalysis and inhibition by electroadsorbates and protective layer, /. Appl. Electrochem., 9, 255 (1979). Vielstich, W., Fuel Cells, John Wiley & Sons, New York, 1970. 5.8 Deposition and Oxidation of Metals
Sections 5.6.2 and 5.6.3 dealt with the deposition of metals from complexes; these processes follow the simple laws dealt with in Sections 5.2 and 5.3, particularly if they take place at mercury electrodes. The deposition of metals at solid electrodes (electrocrystallization) and their oxidation is connected with the kinetics of transformation of the solid phase, which has a specific character. A total of five different cases can be distinguished in these processes: 1. The deposition occurs at an electrode of a different metal or other conductive material (e.g. graphite). 2. The deposition occurs at an electrode of the same metal. 3. The metal is ionized in the anodic process to produce soluble ions. 4. The metal is anodically oxidized to ions that react with the components of the solution to yield an insoluble compound forming a surface film on the electrode. 5. A component of the solution participates in the anodic oxidation of the metal, so that the metal is converted directly into a surface film. These processes either lead to the formation of a new solid phase or the original solid phase grows or disappears. In addition to the electrochemical laws discussed earlier, this group of phenomena must be explained on the basis of the theory of new phase formation (crystallization, condensation, etc.). The basic properties of electrocrystallization can best be illustrated by the example of the deposition of a metal on an electrode of a different material (case 1).