A silver halide infrared fiber-optic evanescent wave spectroscopic technique for in-situ monitoring of chemical processes and surface analysis is described. Samples are spread onto a fiber contained in a teflon-lined cell. Attenuated total internal reflectance (AIR) measurement with a Fourier transform infrared (FTIR) spectrometer yields spectra at various stages of a process (for example, the monitoring of adhesive curing and coupling agent polymerization). Changes in known spectroscopic features may be recognized in films as thin as a monolayer. The advantages and limitations of this surface analysis technique are discussed.