Raman spectroscopy is a vibrational and non-destructive technique that requires minimal sample quantity as well as sample preparation. The thesis includes the use of conventional Raman spectroscopy in aiding the synthesis of heterogeneous catalytic system. Near infrared scanning angle (SA) Raman spectroscopy, a variant of total internal reflection Raman spectroscopy, allows Raman spectra collection simultaneously with incident angle change. The technique is capable of obtaining chemical information, measuring submicron thickness, and detecting buried thin polymer layer from bilayer thin films.