Graphene (a carbon allotrope) is a single graphite sheet consisting of carbon atoms with sp2 in a hexagonal form. Graphene oxide is in fact functionalized graphene with oxygen carrying groups like epoxy and hydroxyl. Graphene oxide and graphene are used due to their unique properties such as electrical conductivity, thermal conductivity as well as high mechanical strength in various fields including electronics, fabrication of supercapacitors and chemical gas sensors. In comparison to graphene, graphene oxide has a better disperse ability in solvents and matrices. Literature review shows that graphene and graphene oxide incorporated nanocomposite nanofibers have gained importance. However, most of the researches carried out in nanocomposites containing graphene and graphene oxides have been limited to films as the matrix. The present research aim at investigating nanofibers as the matrix. In this research, graphene oxide particles were synthesized according to Hummer’s method. Some of the graphene oxide was functionalized with chlorosulphonic acid. Poly(acrylonitrile) solutions (10% w/v) containing different amounts of graphene oxide and functionalized graphene oxide were electrospun. The electrospun nanofibers were then activated by heat treatment. The activated nanofibers were compared with the samples before activation. A sample of activated nanofibers containing graphene oxide was functionalized. FESEM, FTIR, Raman, XRD and EDX as well as specific surface area measurement were employed in the following investigations. It was found that, the nanofibers containing graphene oxide lose their fiber form upon activation and the nanofibrous webs find a network structure. However, the samples with functionalized graphene oxide still show some fiber form. XRD analysis showed that incorporating graphene and graphene oxide does not lead to a considerable structural change in the microstructure of the nanofibers. FTIR proved the existence of graphene oxide and functionalized (chlorosulphonic acid) graphene oxide in nanofibers. Raman analysis showed that higher amounts of graphene oxide leads to lower amounts of defects in the activated composite nanofibers. BET analysis confirmed that carbon nanofibers containing graphene oxide and functionalized graphene oxide have a high specific surface area.