Electrospraying (electrohydrodynamic spraying) is a method of liquid atomization by electrical forces. Spraying solutions or suspensions allow production of fine particles, down to nanometer size. These particles are interesting for a wide variety of applications, thanks to their unprecedented chemical and physical behaviour in comparison to their bulk form. Knowledge of the particle size in powders is important in many studies employing nanoparticles. In this paper, the effect of some process parameters on the size of electrosprayed polyacrylonitrile particles is presented in the form of response surface model. The model is achieved by employing a factorial design to evaluate the influence of parameters on the polyacrylonitrile nanoparticle size and response surface methodology. Four electrospraying parameters, namely, applied voltage, electrospraying solution concentration, flow rate, and syringe needle diameter were considered.