Since wastewater treatment is of great interest to society, it is important to develop techniques that perform this treatment by removing pollutants such as dyes, pesticides, and metals. In this context, adsorption stands out as a promising method in the treatment of effluents, allied to this, as polymeric membranes considerably improve the ability to remove pollutants. Carbon-based additives, such as graphene oxide, have been used in the area of adsorption because they are an adsorbent capable of removing metallic ions and dyes. Thus, it is interesting to carry out studies of the polystyrene polymer with graphene oxide, aiming at the production of adsorbent membranes. To this end, the production of polystyrene was first analyzed, with graphene oxide added to the polymer matrix in the future. Thus, polystyrene microfibers were produced using the electrospinning technique and analyzed morphologically using optical microscopy and scanning electron microscopy (SEM). With the help of ImageJ and OriginPro 8.5 software, a histogram of the frequency distribution of microfiber diameters and the normal curve was created. Through the results obtained, it was observed that there was the production of microfibers with considerable morphology, as fibers with beads and agglomerates were not observed.. From the histogram, it was noted that the microfibers had an average diameter of 5.73 µm.