This study investigated the effect of moisture on a model silane coupling agent modified adhesive bond. Fourier transform infrared-attenuated total reflectance (FTIR-ATR) spectroscopy was used to characterize the transport of moisture to a polypropylene-silane interphase and monitor the resulting chemical changes. The FTIR-ATR method offers the advantage of in-situ examination of the diffusion process, as well as the ability to characterize chemical changes that occur due to the presence of moisture. Experiments were conducted at ambient and elevated temperatures. The results of the real-time measurements demonstrated that moisture will migrate through the polypropylene to the silane interphase. The diffusion behavior was described well by a Fickian model. The apparent diffusion coefficients for water in the polypropylene-silane bilayer were on the order of the diffusion coefficients for water in polypropylene at both test temperatures. Furthermore, changes in the spectra were observed during the diffusion experiments. These changes were indicative of hydrolysis of the siloxane backbone in the silane layer while buried beneath the polypropylene film. This finding is significant as it presents direct evidence of a degradation mechanism in silane-modified adhesive bonds.