Abstract: The study was conducted to assess and ascertain the physico-chemical properties of Mahanadi river water from five different locations of (Binakhandi, 500 m upstream of Binakhandi, 500 m downstream of Binakhandi, PC bridge and Dhanupali) Sambalpur city of Odisha during the month of March and August, 2014. The analysis was carried out by taking certain important parameters like pH, dissolved oxygen (DO), biological oxygen demand (BOD), chemical oxygen demand (COD), Chloride, total dissolved oxygen (TDS), Nitrate, Sulphates, total hardness (TH), electrical conductivity (EC) and Fluoride. Analyzed parameters like pH, DO, TH, Chloride, Sulphate, and TDS were found within permissible limit prescribed by IS 10500 except Nitrate and Fluoride content which exceeds at some sites. COD values were invariably higher than BOD indicating the presence of considerable amount of chemically oxidizable matter which were non-biodegradable.