In this thesis, the exposure extent of MgO and Al 2 O 3 nanoparticles embedded in polyacrylonitrile (PAN) nanofibers to 2-chloroethyl ethyl sulfide (2-CEES) was enhanced through activation processes. The diameter reduction of MgO and Al 2 O 3 -embedded PAN nanofibers through electrospinning depends on the amount, type, and specific surface area of the nanoparticles. The results showed that high specific surface area of nanoparticles brings about higher reduction of PAN nanofibers during activation process. Furthermore, raising the amount and specific surface area of MgO and Al 2 O 3 nanoparticles increased the weight loss and diameter reduction of PAN nanofibers considerably during activation process. Type of metal oxide nanoparticles also affects the weight loss and diameter reduction of PAN nanofibers in activation process. In this work, it was clarified that the type, amount, and specific surface area of metal oxide nanoparticles have great effects on destructive adsorption of 2-CEES by MgO and Al 2 O 3 -embedded activated carbon nanofibers (ACNFs). The order of reactivity of the MgO and Al 2 O 3 -ACNFs are found to be ACNFs MgO–ACNFs Al 2 O 3 –ACNFs Al 2 O 3 Plus–ACNFs MgO Plus–ACNFs. Fourier Transform Infrared studies indicated that after destructive adsorption of 2-CEES by MgO and Al 2 O 3 -embedded ACNFs, a covalent bond (alkoxide bond) e.g. Mg–O–C and Al–O–C is formed between the nanoparticles and 2-CEES residual, respectively.