In this study, simultaneous removal of Cr(VI) and phenol from binary solution was carried out using Fetreated tea waste biomass. The effect of process parameters such as adsorbent dose, pH, initial concentration of Cr(VI) (mg/L), and initial concentration of phenol (mg/L) was optimized. The analysis of variance of the quadratic model demonstrates that the experimental results are in good agreement with the predicted values. Based on experimental design at an initial concentration of 55 mg/L of Cr(VI), 27.50 mg/L of phenol, pH 2.0, 15 g/L adsorbent dose, 99.99% removal of Cr(VI), and phenol was achieved.