X-Ray Photoelectron Spectroscopy (XPS) and Auger Electron Spectroscopy (AES) have been used to investigate the elemental composition, chemical and electronic state of elements that exist within the Herastrau Lake (Bucharest, Romania) sediments. XPS spectra were obtained by irradiating the sediment samples with an Al source of X-rays (1486.6 eV). A very broad peak at 165-180 eV corresponds to sulfur oxides, sulfate and sulfite ions and sulfur hexafluoride. The measurements indicate metal oxides: (Al2O3, Fe2O3) at 528-531 eV, SiO2 at 533 eV, phosphates, nitrates at 531-533 eV, silicates at 532-533 eV, CaO, CaCO3 and CaS at 346-347 eV, CaSO4 at 348 eV, Ca(NO3)2 at 349 eV and slight traces of NH3. A very intense peak at 784 eV also appears due to CoSO4. The analysis of Electron Spin Resonance (ESR) spectra revealed an additional free radical peak in the center of Mn2+ sextet, at a g = 2.0038, attributed to SO3- species as well a very intense and broad signal due to Fe3+ ions.