Water samples from environmental waters, namely the Mammoth Cave in Kentucky and the Harpeth and Cumberland Rivers in Tennessee were analyzed to determine the extent of organic pollutants. Tap water and deionized water samples were also collected and used as controls. Acid/base liquid/liquid extractions were performed on the water samples including the controls. The aqueous layers were discarded and the collected organic layers were stored temporarily at -20 ºC before analysis. The dried organic layers were analyzed using a Varian Saturn Gas Chromatograph - Mass Spectrometer (GC-MS). Chromatograms of sample peaks were analyzed according to retention time using the GC-MS’s embedded library to determine some of the perspective compounds present. Detected compounds were classified as either nontoxic, mildly toxic or toxic to humans based on the available information from the literature. The results indicate the presence of several emerging organic pollutants which may compromise the quality of drinking water for populations who largely depend on them.