Warnes, Gavin Michael (1991) New developments in applied Raman spectroscopy. University of Southampton, Doctoral Thesis.
Abstract
Work has been carried out on the development of new applications of Fourier Transform Raman Spectroscopy. This has centred on the characterisation of oxide heterogeneous catalysts, and the measurement of very small band shifts. Raman spectra have been obtained of pyridine adsorbed to silica, alumina and a variety of T type zeolites. These show the existence physisorbed, hydrogen bonded and Lewis coordinated species. The detection of Bronsted sites is complicated by the presence of hydrogen bonded pyridine. The surface areas of the materials studied were measured using nitrogen isotherm experiments and BET theory. Significant fluorescence and sample heating are still observed with near infrared excitation and this is likely to prevent wide scale use of the technique in this field. By using curve fitting procedures it has been possible to measure small shifts in the position of Raman bands using data from both multichannel and FT Raman spectrometers. Mixtures of acetone H6/D6 and polyethylene/perdeuteropolyethylene were used as trial systems. Band shifts measured were found to be a linear function of mole fraction. Cuvette cells were found to be the best for liquid phase studies with shifts as small as 0.1cm-1 being reliably detected. The method was extended to solids by using plasma emissions from the laser line as an internal frequency standard. A considerable range of applications of this method are envisaged.
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