The performance of chemical protective materials is an important and sensitive issue as it is associated with human safety and therefore, the development of highly efficient chemical protective materials is always a continuous process. The emergences of nanotechnology opened up so many research areas and electrospun nanocompositefiber is a potential candidate that could be used as a self detoxifying material. In this study, nanocrystalline magnesium oxide-polyethylene oxide nanofibers have been produced in the laboratory and this composite can be used against the nerve agents (Sarin, Soman and VX agents) and the organophosphorous compounds efficiently. Nanocrystalline magnesium oxide has been reported as the most reactive metal oxides and it can work as a destructive adsorbent by breaking the P-O and P-F bondings. It also immobilizes the resultant fragments. On the other hand, polyethylene oxide has been chosen for its solubility in water and it is cheap as well. Nanofibers have high surface area to volume ratio and they are porous in nature and incorporation of nanocrystalline metal oxide onto the nanofiber matrix actually boosts the performance of nanofiber composites. The nanofibers were characterized by using scanning electron microscopy (SEM), transmission electron microscopy (TEM), Electron dispersion spectroscopy (EDS) and X-ray diffraction (XRD) technique. In addition to this, thermogravimetric analyzer (TGA) was used to study the adsorption performance of the nanocompositefibers. Nanofibers in the range of 50 to 250 nm have been developed and promising results were achieved in producing self detoxifying nanofiber materials. The adsorption studies were compared with that of activated carbon fiber alone and it has been found that the initial adsorption rate and percent weight gain have been increased for the nanocompositefibers.