In this study, PVA/PAA, PVA/PAA/PVP, PVA/PAA/PVP-I and PVA/PAA/PVP/Chitosan fiber mats were prepared via electrospinning. Synthesized nanofibers were characterized by DSC, FT-IR and SEM. DSC results showed that the nanofibers were degraded at 400 degrees C and 450 degrees C. The addition of PVP-K30, PVP-I and chitosan to PVA/PAA structure increased the thermal stability of the nanofibers. SEM micrographs showed that synthesized nanofibers are linear. Fiber diameter measurements showed that average diameters of the fibers are less than 0.5 micron. The average diameters of PVA/PAA, PVA/PAA/PVP, PVA/PAA/PVP-I and PVA/PAA/PVP/Chitosan fibers were calculated as 458nm, 237nm, 139nm, and 270nm, respectively.