Because of the increased amount of cobalt and Congo red dye effluents attributable to the industrial operations, the capacity of Enteromorpha intestinalis biomass as a sustainable source to achieve significant biosorption percent for both pollutants from dual solution was assessed. A fifty batch FCCCD experiments for biosorption of cobalt ions and Congo red dye were performed. The complete removal of Congo red dye was obtained at 36th run using an initial pH value of 10, 1.0 g/L of Enteromorpha intestinalis biomass, 100 and 200 mg/L of Congo red and cobalt for a 20-min incubation time. Meanwhile, a cobalt removal percent of 85.22 was obtained at 35th run using a neutral pH of 7.0, 3.0 g/L of algal biomass, 150 and 120 mg/L of Congo red, and cobalt for a 60-min incubation time. For further illustration and to interpret how the biosorption mechanism was performed, FTIR analysis was conducted to inspect the role of each active group in the biosorption process, it can be inferred that –OH, C–H, C=O, O–SO₃^- and C–O–C groups were mainly responsible for Co²⁺ adsorption of from aqueous dual solution. Also, scan electron microscope revealed the appearance of new shiny particles biosorbed on E. intestinalis surface after the biosorption process. EDS analysis proved the presence of Co²⁺ on the algal surface after the biosorption process.