Confocal microprobe Raman spectroscopy has been applied to the study of liquid/gas and solid/liquid interfaces. With the help of the resonance Raman effect, the aggregation process of TSPP has been monitored at the liquid/gas interface using Raman spectroscopy, which is shown to have very different behavior compared with that in the bulk. The solution layer analysis has been performed in the interfacial region above a Pt electrode under reaction, and the solution composition is monitored in situ during the electrochemecial reaction. Taking the advantage of high spatial resolution of the confocal microscope, the surface enhanced Raman imaging has been performed on the electrodeposited gold surface.