The present work is devoted to the analysis of results of investigations carried out in the Russian sector of the Sea of Azov and in the lower part of the Don River during the period from 2006 to 2010. In several scientific expeditions for the first time in the Sea of Azov investigation history 48 sediment cores from 20 to 100 cm thick were taken and studied layer-by-layer in order to determine the distribution of oil components and radioisotopes Cs-137 and Pb-210. The radioisotopes’ specific activities were measured by gamma-spectrometry in order to assess the sedimentation rates and to date different sediment core layers. The concentrations of oil components were obtained with the use of thin layer and column chromatography, optical and gravimetric methods making possible to determine separately the sum of aliphatic, naphthenic, mono- and di-aromatic hydrocarbons, the sum of polycyclic aromatic hydrocarbons and the asphaltic components as well as the presence of hydrocarbons of contemporary biological origin. According to the results of radiological analysis, the highest sedimentation rates are obtained for the delta and the near-delta part of the Don Rive (5 to 14 mm of wet matter per year). The lowest rates are characteristic for the shallow eastern part of the Gulf of Taganrog (1 to 2 mm of wet matter per year) in spite of considerable sediment runoff of the Don River. That’s because of low depths (2 to 5 m) and high hydrodynamic activity of water column favoring regular stirring-up and carrying out of sediments. In the deeper central and southern parts of the Sea of Azov the sedimentation rates rise up to 4 mm per year. The study of oil components distribution in the sediment cores shows that the most of them are concentrated in the upper layer formed in the last 50 to 70 years, i.e. in the period of the most important anthropogenic pressure.