The responsive nature of polyaniline (PANI) to gaseous pollutants is highly dependent on processing conditions, film composition, and morphology. Hybrid systems of leucoemeraldine-based polyaniline (LEB-PANI) have shown to aid in the stability of the material yielding an active matrix for gas sensing. The electrospinning technique was employed for preparation of PANI-Polyvinyl Pyrrolidone (PVP) hybrid structures for room temperature NO2 detection.