Regional geochemical mapping was carried out in Bilaspur and Korba Districts of Chhattisgarh, and stream sediments/slope wash, soil, and water samples were analyzed for concentration of heavy metals. The study contributes to understanding heavy metals contamination of sediments, soils, and water due to anthropogenic activity, mainly in agriculture-based rural areas. The study reveals that high geochemical anomalies observed for heavy metals like Ni, Cr, As, and Zn in sediments and soil samples are due to the extensive uses of phosphatic fertilizer and soil amendments in the form of poultry and swine manure. Water quality assessment of major streams in the study areas shows that the water is suitable for domestic and agricultural uses. Correlation analysis reveals that the chemical weathering of rock-forming minerals doesn’t control the surface water chemistry of the study area and is also an anthropogenic source of sodium in water. This study also shows the importance of the country’s geochemical mapping database, which will have much broader applications than conventional mineral exploration and geological mapping.