The Mayak Production Association (Mayak PA) was established in the late 1940's to produce plutonium for the Soviet Nuclear Weapons Programme. In total, seven reactors and two reprocessing plants have been in operation. Today, the area comprises both military and civilian reactors as well as reprocessing and metallurgical plants. Authorized and accidental releases of radioactive waste have caused severe contamination to the surrounding areas. In the present study, [alpha]-spectrometry and inductively coupled plasma-mass spectrometry (ICP-MS) have been used to determine plutonium activities and isotope ratios in soil and sediment samples collected from reservoirs of the Techa River at the Mayak area and downstream Techa River. The objective of the study was to determine the total inventory of plutonium in the reservoirs and to identify the different sources contributing to the plutonium contamination. Results based on [alpha]-spectrometry and ICP-MS measurements show the presence of different sources and confirmed recent reports of civilian reprocessing at Mayak. Determination of activity levels and isotope ratios in soil and sediment samples from the Techa River support the hypothesis that most of the plutonium, like other radionuclides in the Techa River, originated from the very early waste discharges to the Techa River between 1949 and 1951. Analysis of reservoir sediment samples suggest that about 75% of the plutonium isotopes could have been released to Reservoir 10 during the early weapons production operation of the plant, and that the majority of plutonium in Reservoir 10 originates from discharges from power production or reprocessing. Enhanced 240Pu/239Pu atom ratios in river sediment upper layers (0-2 cm) between 50 and 250 km downstream from the plant indicate a contribution from other, non-fallout sources.