CHLOROBENZENES ARE USED AS INDUSTRIAL SOLVENTS, PESTICIDES, DIELECTRIC FLUIDS, DEODORANT, AND CHEMICAL INTERMEDIATES. THEY CAN ENTER THE AQUATIC ENVIRONMENT THROUGH SOLID AND LIQUID EFFLUENTS AND ATMOSPHERIC DISCHARGES. BECAUSE THEY ARE RELATIVELY RESISTANT TO ABIOTIC AND BIOTIC DEGRADATION THEY TEND TO PERSIST IN THE ENVIRONMENT. CHLOROBENZENES ARE ESSENTIALLY UBIQUITOUS IN THE AQUATIC ENVIRONMENT, THEY CAN BE DETECTED IN WATER, SEDIMENT AND AQUATIC BIOTA [1].ELECTROSPINNING IS A SIMPLE, INEXPENSIVE TECHNIQUE THAT CREATESNANOFIBERS THROUGH AN ELECTRICALLY CHARGED JET OF POLYMER SOLUTIONOR MELT. THIS METHOD SHOULD PROVIDE ANAPPROACH TO GENERATE HIGH SURFACE AREA FIBERS AND THE VERSATILITYTO ALTER THE SPME FIBER COMPOSITION BY CHANGING THE POLYMERSOLUTION FOR ELECTROSPINNING [2, 3].IN THIS STUDY, SPME FIBERS WERE PRODUCED BY ELECTROSPINNING OF POLYACRYLONITRILE ON ALIMINIUM WIRES AND THEN THE NANOFIBERS WERE PYROLYZED TO GENERATE CARBON NANOFIBER SPME COATINGS. THE FIBER WAS THEN APPLIED FOR PRECONCENTRATIONAND DETERMINATION OF 1, 4-DICHLOROBENZENE (1, 4-DCB), 1, 2, 3-TRICHLOROBENZENE (1, 2, 3-TCB) AND 1, 2, 4-TRICHLOROBENZENE (1, 2, 4-TCB) IN WATER SAMPLES.VARIOUS FACTORS WHICH INFLUENCED THE RECOVERY OF THE ANALYTES WERE INVESTIGATED SUCH AS: FIBER THICKNESS, SALT ADDITION, EXTRACTION TIME, EXTRACTION TEMPERATURE, DESORPTIONTEMPERATURE AND TIME.DETECTION LIMITS WERE 10, 40, AND 400 NG/LFOR 1, 2, 4-TCB, 1, 2, 3-TCB, AND 1, 4-DCB, RESPECTIVELY.ALL RSDS WERE<9% (FORN=5). THE PROPOSED METHOD WAS APPLIED FOR THE ANALYSIS OF CHLOROBENZES IN SURFACE WATERS.