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composition of surfactant, silica, water, acid, and solvent. After surfactant removal by calcination or solvent extraction, mesoporous silica materials are formed (Fig. 13.6). EISA provides a highly controllable approach to fabricate nanoporous lms and particles. The fast process, easy integration of nanoporous lms into devices, and controllable properties (pore sizes, pore surface chemistries, pore arrangements, and porosity) are especially suitable for the application of nanotechnology in industry.

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Thus a plot of the dependence of Eqh on the pH (Fig. 3.11) will yield a curve with three linear regions (the second of which is poorly defined), with slopes of 0.0591, 0.0295 and 0 (at 25 C). The intersections of each two neighbouring extrapolated linear portions yield the pK[ and pA^ values, as follows from comparison of Eqs (3.2.34) to (3.2.36). Figure 3.12 gives examples of the dependence of the apparent formal potential on the pH for other organic systems (see also p. 465).

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Concept of Stimuli-Responsive Nanocomposite Materials. To expand the range of applications as well as create new properties, various organic functional groups have been covalently incorporated onto the pore surfaces of mesoporous materials, including phenyl, octyl, aminoalkyl, cyanoalkyl, thioloalkyl, epoxyl, and vinyl groups (Nicole et al., 2005). However, these modi cations have provided mainly passive functionalities, such as controlled wetting properties, reduced dielectric constants, or enhanced adsorption of metal ions. By comparison, materials with stimuli-responsive functionalities would enable properties to be dynamically controlled by external stimuli, such as pH, temperature, or light. The concept of stimuli-responsive nanocomposite materials was proposed by Brinker and coworkers (Liu et al., 2003a; Fig. 13.7). Incorporation of covalently bonded, switchable ligands as pendant groups (as opposed to bridging groups) within a porous (rather than a layered) framework is expected to result in nanocomposites in which the pore size, surface area, and adsorptive properties are externally controllable. In such synergistic nanocomposites, the 3-D organization of the responsive ligands allows transduction of photo, chemical, or thermal energy into a useful mechanical response of interest for molecular valves or gates. In addition, the rigid framework could serve to enhance the mechanical, chemical, and thermal stability of the responsive moieties, fostering their integration into devices. As described earlier, switchable azobenzene derivatives are promising candidate molecules for the synthesis of photoresponsive nanocomposite materials. To best utilize photoisomerization to accurately control pore size, azobenzene ligands need to be anchored to the pore surfaces of a uniform mesostructure with monosized pores. This allows the rigid inorganic framework to precisely position azobenzene ligands in 3-D con gurations where switching results in a well-de ned change in pore size.

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Two synthetic methods have been exploited to incorporate azobenzene moieties into mesoporous silica frameworks. The postgrafting method involves functionalizing mesoporous sol gel materials with reactive azobenzene derivatives to tether azobenzene moieties to sol gel matrices. The one-pot synthesis method requires

Fig. 3.11 The dependence of the potential of the quinhydrone electrode qh(V) on pH. The straight line (1) corresponds to Eq. (3.2.34), (2) to (3.2.35) and (3) to (3.2.36)

14

Figure 13.7. Concept of responsive nanocomposites. Organization of stimuli responsive ligands within a 3-D porous framework imparts new molecular-level functionality, useful for opening and closing a nanoscale valve. Source: From Liu et al., 2003a. Reprinted with permission.

In cases where the potential of an inert electrode, in the presence of the redox system of interest, is established slowly, another redox system may then be added as a 'mediator'. The latter system should react rapidly with the former and quickly establish an equilibrium at the electrode. As a very small amount of the mediator is added, concentration changes in the measured system compared to the original state can be neglected. Suitable mediators are Ce 4+ -Ce 3+ , methylene blue-leucoform, etc. Standard redox potentials can be determined approximately from the titration curves for suitably selected pairs of redox systems. However, these curves always yield only the difference between the standard potentials and a term containing the activity coefficients, i.e. the formal potential. The large values of the terms containing the activity coefficients lead to a considerable difference between the formal potential and the standard potential (of the order of tens of millivolts). 3.2.6 Electrode potentials in non -aqueous media While the laws governing electrode potentials in non-aqueous media are basically the same as for potentials in aqueous solutions, the standardization in this case is not so simple. Two approaches can be adopted: either a suitable standard electrode can be selected for each medium (e.g. the hydrogen electrode for the protic medium, the bis-diphenyl chromium(II)/ bis-diphenyl chromium(I) redox electrode for a wide range of organic

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