Heavy metals contamination especially in the aquatic environment poses severe environmental pollution concerns worldwide. Sources of heavy metals especially in textile industries has been discharging toxic heavy metals through the release of dyes into the environment during fibre dyeing and finishing processes. Individual wastewater treatment through physical, biological, or chemical method is often very costly and results in large amount of sludge. Thus, there is a need for alternative treatment processes that covers from pre to post wastewater treatment stage. Magnetic chitosan cellulose nanofiber (Mag-Chi-CNF) nanocomposite was synthesized from the isolated cellulose nanofiber by sol-gel technique. Several characterization methods were utilized to characterize the physicochemical, morphological, and thermal properties of the isolated Mag-Chi-CNF. Subsequently, the isolated Mag-Chi-CNF was utilized for single and simultaneous adsorption of heavy metals ions such as Cu(II), Cr(VI), and Pb(II) from synthetic aqueous solution. The adsorption was conducted by varying adsorption parameters such as pH, bio- sorbent doses, treatment time, and temperature. The surface morphologies of Mag- Chi-CNF revealed the porous structure that may enhance heavy metal adsorption, with average particle length of 500 ± 20 nm and width of 380 ± 12 nm, respectively. Thermal stability analysis shows the Mag-Chi-CNF have high thermal stability properties with thermal degradation temperature of 312 °C
