This researchdescribe wastewater pre-treatment that contaminated with Methylene Blue dye (MB) and Ni(II) ion by Athelia Bombacina fungus dead biomass (ABFDB). Researches finding on ABFDB characterization by SEM, XRD, CHNS and FT-IR analysis show that ABFDB can be used as efficient sorbent, because ABFDB cellular wall consist of Chitin, β-Glucan and Cellulose biopolymers, generally. Results show that removal of MB and Ni(II) ion by ABFDB sorbent is more than 86.41 and 66.2%, respectively. So, after parameters investigation of MB and Ni(II) ion sorption process by ABFDB, the response surface method was employed for optimization and study the interaction of operational parameters on the sorption of pollutants. This low-cost and natural environmental friendly biosorbent can be utilized for pretreatment process in the first step of wastewater treatment project.