Chemical disinfection of surface waters has been proven effective in minimizing the risk of contamination by water-borne pathogens. However, surface waters contain natural organic matter (NOM) which, upon chemical disinfection, is readily converted into hazardous disinfection-by-products. Hence, NOM removal from these waters is critical. Chemical coagulation is a readily implementable technology to minimize these undesired side-effects by NOM removal. Herein, capabilities of ferric chloride (FeCl₃) and polyaluminum chloride (PACl) as pre-treatment for NOM abatement from natural raw surface water have been benchmarked. Excitation-emission fluorescence matrix (EEM) spectroscopy characterization of NOM fractions demonstrated high removal efficiency. A two-level full factorial design was employed to analyze the effects of coagulant dosage and initial pH on the removal of turbidity, humic acid-like substances and fulvic acid-like substances from the raw water. Higher removal of ~77% NOM was attained with PACl than with FeCl₃ (~72%). Optimization through response surface methodology showed that the initial pH—coagulant dosage interaction was significant in removing NOM and turbidity for both PACl and FeCl₃. These results identify the opportunity for coagulation technologies to prevent and minimize disinfection-by-products formation through NOM removal.