Polychlorinated biphenyl compounds (PCBs) were included to the Stockholm Convention's list of typical persistent organic pollutants on May 22, 2001. (POPs). Humans have produced PCBs, which are pervasive in the environment. They are a concern for people all around the world because of their toxic, bioaccumulative, long-lasting, hydrophobic, and transboundary characteristics. The study's goals included describing how PCBs are distributed in surface water and evaluating how certain physiochemical factors affect PCB concentrations. Five separate Okitipupa locations—OAUSTECH, Igodan, Okunmo, Idepe, and Lebi/Ofe River—had their water samples taken. The overall average concentration of PCBs discovered in the samples taken from five (5) distinct places was determined to be as follows: OAUSTECH (5.720.13), Igodan (5.520.00), Okunmo (3.480.03), Idepe (21.830.02), and Lebi/Ofe (0.160.00), with their combined probability being determined to be 0.001. Twenty-five (25) PCB congeners were examined using a gas chromatography-electron capture detector (GC-ECD). The majority of congeners were below the detection threshold at every site. Total PCB values varied from 0.16 g/L to 21.83 g/L. The correlation between the overall level of polychlorinated biphenyls and the total organic carbon was positive (0.214), but it was weak (PCBs) and pH, positive (0.096) but poor correlation between the electrical conductivity, and a positive (0.220). The levels found in this investigation, with the exception of one area, were obviously lower than the 0.5μg/l level advised by the WHO. The water's concentration of polychlorinated biphenyls (PCBs) is not significantly impacted by the physicochemical characteristics, and the water is safe to use for household purposes.