Polyacrylonitrile (PAN) is a hard, rigid, thermoplastic substance with various applications, including carbon fiber production for the aerospace and automotive sectors, textile manufacturing, and water and air filtration. Its usage as a synthetic resin is particularly notable in its stabilized form. Stabilization ensures thermal stability during graphitization by transforming the structure from linear to lateral, resulting in an aromatic ladder. In this study, an 8% w/w polyacrylonitrile solution in N,N-dimethylformamide is electrospun and subsequently stabilized by heating up to 280 °C. The electrospun sample (pristine material) and its stabilized form at 280 °C in air were analyzed using x-ray photoelectron spectroscopy (XPS) at room temperature with a nonmonochromatic Mg Kα x-ray source.