Charge neutralisation plays a major role in heavy metal and humic substance removal in water treatment. Humic substances have no readily identifiable structure and they consist of anionic macromolecules of low to moderate molecular weight. Humic substances are easily coagulated using cationic metals and polyelectrolytes. Different concentrations of humic substances have been coagulated with different concentrations of heavy metals and/or polyelectrolytes. The charge neutralisation was determined using U.V. spectrophotometer. Humic substance removal increased with increasing salinity level until reaching a point where HS destabilization is considered complete and salinity no longer play a role in HS removal. Humic substance removal increased with increasing heavy metals concentration and precipitation was experienced at high concentrations of heavy metals (15-20 mg/L) and low concentration of humic substances (10 mg/L). In addition, HS removal also increased with increasing polyelectrolyte concentration. Diallydimethylammonium chloride (PDADMAC) polyelectrolyte was more effective in humic substance coagulation compared to copolymer of dimethyl aminoethyl acrylate (CoAA). The addition of heavy metals in polyelectrolyte coagulation increased humic substance removal due to the combined charge neutralization of the metals and polyelectrolytes.