In this thesis attempts were made to investigate dissolved organic carbon (DOC) and coexisting heavy metals in an area highly polluted with organic waste from municipal sewage and heavy metals from acid mine drainage. DOC was sampled and prefiltrated to < 0.45 µm. Prefiltrated samples were enriched by nanofiltration. Organic heavy metals with organic ligands were isolated by Size Exclusion Chromatography with online UV detection (SEC-UV). Isolated fractions were freeze dried and further characterized by Pyrolyzis-Gas Chromatograpy-Mass Spectrometry and-Isotopic Ratio Mass Spectrometry (Py-GC-MS/IRMS). These characterizations yield in the identification of anthropogenic and biogenic organic ligands for heavy metals.