The analysis of hydrocarbon-contaminated soils from abandoned refinery sites in Alberta, Canada is used to illustrate a tiered analytical approach to the characterization of complex hydrocarbon wastes. Soil extracts isolated from heavy oil- and creosote-contaminated sites were characterized by thin layer chromatography with flame ionization detection (TLC-FID), ultraviolet fluorescence, simulated distillation (GC-SIMDIS) and chemical ionization GC-MS analysis. The combined screening and detailed analytical methods provided information essential to remedial technology selection including the extent of contamination, the class composition of soil extracts, the distillation profile of component classes and the distribution of individual class components within various waste fractions. Residual contamination was characteristic of heavy, degraded oils, consistent with documented site operations and length of hydrocarbon exposure at the soil surface.