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In this research, the effect of polyethylene glycol (PEG) molecular weight on permeability and selectivity of polysulfone/polyethylene glycol (PSF/PEG) composite membrane is investigated. Polyethylene glycol with molecular weights of 4000, 6000, and 10,000 is applied. It is shown from the results that PEG applied in composite membranes with molecular weight of 1000 had the best diffusivity in comparison with the other composite membranes containing PEG with lower molecular weights. In addition, it is perceived that the permeability of CO 2 from PSF/PEG10000 composite membranes has increased with enhancing weight percent. CO 2 permeability into PSF/PEG composite membranes containing 20 wt% PEG10000 is calculated 7.64 barrer (1 barrer = 10 −10 cm 3 (STP) cm/cm 2 s cmHg). The ideal selectivity for CO 2 /N 2 gas pair in PSF pure membrane and composite membranes containing 10 wt% and 20 wt% PEG10000 are calculated 26.57, 30.61, and 32.12, respectively. Finally, the morphology and membrane structure of the membrane were evaluated with infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), and tensile strength test.