The objective of this project was to explore and more fully develop capillary supercritical fluid chromatography (SFC) as a high resolution separation technique. The developed SFC techniques were then to be applied to the separation and structural evaluation of various asphaltene fractions. This report covers the following work performed: (1) development of bonded stationary phases; (2) optimization of fluorescence detection; (3) ultraviolet absorption detection; (4) evaluation of different mobile phases; and (5) analysis of asphaltenes. 14 references, 40 figures, 9 tables.