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In this paper, we report on the synthesis of styrofoam/cellulose acetate composite nanofibers using electrospinning. Styrofoam was dissolved in DMF (dimethylformamide) with a concentration of 25 wt% and cellulose acetate at a concentration of 5 wt% with DMF solvent as well. Both solutions were blended and stirred until homogeneous. The precursor solution was varied by the mass ratio of styrofoam solution and cellulose acetate solution 80:20, 60:40, 50:50, 40:60, and 20:80. The solution characteristics were the viscosity, surface tension, and conductivity measured for each precursor solution. All solutions have been spun on the same parameters. The nanofibers morphology was characterized by a scanning electron microscope (SEM). The produced nanofibers have a straight, smooth, without bead morphology, and have a diameter of 500 nm to 2.5 µm. Each variation of the spinning solution produces a different diameter of the nanofiber. Addition of the content of styrofoam solution has produced a larger nanofiber diameter. The increase in fiber diameter was related to the characteristics of the viscosity solution, surface tension, and conductivity. Mixing cellulose acetate and styrofoam is expected to reduce the hydrophobicity of styrofoam. So that styrofoam nanofibers can have wider applications.