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50 mM KCl in a cubic cell. Fig. 13.12c shows the UV/visible spectra data of a Brij 56 templated TSUA-modi ed, nanocomposite lm coated on an ITO/glass substrate. The lm exhibits an excellent reversible photoisomerization phenomenon. UV irradiation causes gradual decreases in the p p* transition band (355 nm) and increases in the n p* transition band (456 nm). The reverse cistrans isomerization can be achieved by a visible light exposure (l = 435 nm). A comparison between the absorbance in air (Fig. 13.12a) and absorbance in buffer solution (Fig. 13.12c) shows the aqueous environment causing a decrease in the absorbance in the n p* transition band. This indicates weaker hydrogen-bonding interactions between the azo and silanol groups on the silica wall than those present in air. Brinker and coworkers also monitored the absorbance (A) at 355 nm (p p* transition) in situ to calculate the kinetics of the cis-trans isomerization of the azobenzene ligands contained in the nanocomposite lm deposited on the ITO/ glass substrate in buffer solution (Liu, 2004). The rst-order plot of ln((AN A0)/ (AN At)) vs. t was not perfectly linear in the entire region. The slope (rate constant, k) gradually decreases (to250 min) and remains constant (tW250 min). The deviation from rst-order kinetics is common for azobenzene ligands con ned in sol gel matrices or polymers (Bohm et al., 1996; Ueda et al., 1992). These data imply that the kinetics is composed of two parts, a fast one (k1) and a slow one (k2). When t is small, the fast process is predominant. On the contrary, the slow process becomes predominant as time (t) increases. A double exponential equation was used to t the data and evaluate k1 and k2. A t A 1 a1 e

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Here At and AN are the absorbance at time t and in nite time. k1 and k2 are the rate constants of the fast and the slow processes. a1 and a2 represent the relative contributions of the fast and slow processes to the kinetics of the cistrans isomerization. The rate constants of the fast (k1) and the slow (k2) processes at 201C are 1.7 10 4 s 1 and 1.7 10 5 s 1, respectively. The rate constant of the thermal cis-trans isomerization of azobenzene derivatives in solution is usually on the order of 10 5 s 1. Compared with this value, the rate of cis-trans isomerization of azobenzene ligands incorporated into the nanocomposite lms is faster for k1 and is in the same order for k2, which is good for applications requiring fast switching between the two isomerization states. For P123-templated nanocomposite lms, a similar analysis was performed to evaluate the rate constants of the fast and the slow processes. The rate constants of the fast (k1) and the slow (k2) processes are 5.7 10 4 s 1 and 6.5 10 5 s 1, respectively. Similar to those of Brij 56 templated nanocomposite lms, the cistrans isomerization of P123-templated lms is faster for k1 and is in the same order for k2. Brinker and coworkers proposed a physical explanation to the foregoing experimental results (Liu, 2004). In the photoresponsive nanocomposites, a portion of the azobenzene ligands positioned on the mesopore surfaces has

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Fig. 3.14 An extrapolation graph for determination of the thermodynamic dissociation constant of acetic acid using Eq. (3.3.14)

suf cient free volume to isomerize (cis-trans) via a rotation mechanism at a rate (k1) comparable to that in solution, whereas a second portion of azobenzene ligands anchored at the constrictions between the mesopores (inherent to the cubic symmetry) is constrained and isomerizes (cis-trans) faster via an inversion mechanism (k2). This is reasonable because the activation energy and extra volume needed for isomerization via the inversion mechanism are less than those needed for the rotation mechanism. The fast isomerization fractions (a1/(a1+a2)) of Brij 56 and P123-templated nanocomposite lms are 38% and 29%, respectively, and both are larger than that of the azobenzene ligands contained in hybrid polymers (14%) (Bohm et al., 1996; Ueda et al., 1992). 13.3.2.2. Photoisomerization of Azobenzene-Containing Dendrons in Nanostructured Silica. Zink and coworkers studied the photoisomerization of azobenzene-containing dendrons in 2-D hexagonal mesoporous silica materials (Sierocki et al., 2006). Figure 13.13 shows a representative absorption spectra evolution of AzoG1 (see Fig. 13.9) in dichloromethane in the dark after

197 constant using Eq. (3.3.13). A series of measurements of E is carried out for a single mxlm2 ratio and varying sodium chloride concentrations ra3. Then the expression on the left-hand side of Eq. (3.3.14) is plotted against V7 and the dependence is extrapolated to / 0. The intercept on the ordinate axis yields the value of log KA (see Fig. 3.14). However, the value of E AgCl/Ag must be the same as that employed for standard pH measurements. References

Fibre Channel, iSCSI ( 07)

York, 1973. Covington, A. K., R. G. Bates and R. A. Durst, Definition of pH scales, standard reference values, measurement of pH and related terminology, Pure AppL Chern., 57, 531 (1985). Glasoe, P. K., and F. A. Long, Use of glass electrode to measure acidities in deuterium oxide, /. Phys. Chem., 64, 188 (1960).

0.0 0 0.2 100,000 Time (s) 200,000

Harned, H. S., and B. B. Owen, The Physical Chemistry of Electrolytic Solutions,

Fibre Channel, iSCSI ( 07)

0.0 300 400 500 Wavelength (nm) 600 700

Reinhold, New York, 1950. Robinson, R. A., and R. H. Stokes, Electrolyte Solutions, Butterworths, London, 1959.

Figure 13.13. Absorbance evolution of AzoG1 as a function of time after irradiation with 344-nm light to reach the photostationary state. Inset is the plot of the rst-order kinetics. Source: Sierocki et al., 2006. Reprinted with permission.

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Serjeant, E. P., Potentiometry and Potentiometric Titrations, John Wiley & Sons, New York, 1984. Wawzonek, S., see page 190.