As a result of a gasoline spill in an urban area, Electrical Resistivity Tomography (ERT), Electromagnetic Profiling (EMP) and Volatile Organic Compounds (VOC) methods were used in order to define the contamination plume and to optimize the drilling and soil sampling activities. The VOC anomalies (recent contamination) indicated that a gas station located at the study site is an active contamination source. The mature contaminated zones defined by ERT and EMP methods corresponded with low resistivity anomalies due to degradation process of the hydrocarbons contaminants. The ERT, EMP and VOC results were integrated on a map, allowing the final configuration of contamination plumes and the optimization of drilling and soil/freeproduct sampling. Laboratory analyses of free-product samples suggest the existence of more than one contamination event in the site, with the presence of recent and degraded-hydrocarbon contaminants classified in the gasoline range. This study shows the advantages of joint application of ERT, EMP and VOC methods in sites with active contamination source, where the existence of recent and mature contaminants in subsoil is assumed.