The interaction of semiconductor surfaces with aqueous acid solutions is important in chemical cleaning and etching. Wet chemical treatments are advantageous because they cause little damage to the surface and do not usually require high temperatures. The surface chemistry of GaAs after treatment with phosphoric acid was studied using multiple internal reflection infrared spectroscopy. The treatment left behind a thin film containing several types of PxOy bonds. The chemical nature of the film was observed to change with time as new species would form on the surface.