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Activated carbon nanofibers (ACNF) have been successfully prepared using an electrospinning method with coconut shell charcoal (CSC) as a carbon source and poly(vinyl alcohol) (PVA) as a spinning polymer agent. The high voltage of 10 kV was applied for the electrospinning system. The positive electrode of the high voltage power supply was connected to the needle tip, and the grounded electrode was connected to the metallic collector wrapped with an aluminum foil. The dry fibers in the form of a fibrous mat were collected in the aluminum foil. The average pore diameters of the generated fibers for all variables ranging from 2.23 to 3.73 nm corresponding to mesoporous carbon nanofibers. The total pore volumes were ranging from 0.50 to 0.92 cm³/g. IACNF-60 had the largest surface area of 1,277 m²/g obtained from the use of PVA 12 w/v %, 60 wt% CSC, and the use of iodine treatment before thermal …