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This study was conducted to analyze the effect of alkali treatment against bonding between natural fiber and polyester matrix. The Sisal fiber used by reinforced polyester matrix. Alkalization treatment by NaOH concentration 5 wt.% within 0, 2, 4 and 6 hours, soaking time. Sisal fiber cut 1 cm to used reinforced unsaturated polyester resin (UPR) with weight fraction volume ratio of 30:70 (w/w). The composite product uses press mold method with 1 bar compression to produce the Sisal Polyester Composite (SPC). Mechanical test such as tensile, bending, impact, and of SPC according to ASTM D-638, D-790 and D-5942. Tensile test shows soaking time for 4 hours increases the tensile, flexural, toughness by 29%, 8% and 38%. SEM image shows phenomena fracture the SPC untreatment would be more dominated by fiber pullout. Alkaline soaking time for 4 hours causes the SPC more toughness and ductile than untreated. It occurs because the surfaces of cellulose of sisal fibers bonded the matrix perfectly. The long soaking time for 6 hours caused the damage of cellulose crystalline region and it causes fibrillation on the surfaces.