A method was developed to access the interior of light-guiding structures in order to exploit the enhanced sensing potential of the highly confined electromagnetic field distributions, located within the core of a waveguide. The work presented in this thesis explores therefore the possibilities of optical waveguide spectroscopy utilising transparent mesoporous thin-film waveguides deposited on top of athin gold layer. These multi-layer assemblies are employed in a prism-coupling attenuated total internal reflection (ATR) configuration. The angular read-out of the reflected light intensity allows label-free detection schemes with high sensitivity to changes of the dielectric environment in the case of the presence of analyte molecules within the probing region. This optical waveguide spectroscopy technique has been used to study the real-timediffusion of Ruthenium 535-bisTBA (N-719) dye into mesoporous nanocrystalline titaniumdioxide films. The porous films were prepared on top of gold substrates and prism coupling was used to create a guided wave in the nanocrystalline film. Dying was carried out by bring the film into contact with a 3 x 10-4 moldm-3 dye solution and using optical waveguide spectroscopy to monitor the change in both the refractive index and theextinction coefficient of the nanoporous layer as dye diffused into the porous network. Dyeuptake in a 1.27 μm film was slow with the refractive index of the film still increasing after 22 hours.

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