A controlled Tetrachloroethylene (PCE) spill experiment was conducted in a multi-layer formation consisting of sand and clayey-sand layers. The purpose of the work was to determine the detection limits and capability of various geophysical methods. Measurements were made with ten different geophysical techniques before, during, and after the PCE injection. This experiment provided a clear identification of any geophysical anomalies associated with the presence of the PCE. During the injection period all the techniques indicated anamolies associated with the PCE. In order to quantify the results and provide an indication of the PCE detection limits of the various geophysical methods, the tank was subsequently excavated and samples of the various layers were analyzed for residual PCE concentration with gas chromatography (GC). This paper presents some of the results of five of the techniques: cross borehole complex resistivity (CR) also referred to as spectral induced polarization (SIP), cross borehole high resolution seismic (HRS), borehole self potential (SP), surface ground penetration radar (GPR), and borehole video (BV).