Improvement and effectiveness of polymers through reinforced materials coupled with environmental nuisance of the Cissus populnea fiber remains an area of concern. Tensile responses of chemically treated C. populnea fibers were investigated. Gravimetric analysis was used to determine the composition of C. populnea fibers. Sodium hydroxide (NaOH), acetic anhydride (AC) and ethylene diaminetetra-acetic acid (EDTA), respectively, were used for fiber treatment and optimized with variable parameters (concentration and time) using response surface methodology (RSM) with central composite design. Scanning electron microscopy (SEM) with energy dispersive spectroscopy (EDS) were studied. At optimum treatment conditions, NaOH, AC and EDTA, respectively, increased the tensile strength of C. populnea fiber by 33.49, 274 and 194.52% as well as tensile modulus by 793.43, 20799.43 and 855%. Hence acetic anhydride treatment gave the best tensile properties of C. populnea fibers as corroborated by SEM with EDS. Thus, the effective use of C. populnea fiber in composite applications can be improved by chemical surface modifications.