CHROMATOGRAPHY IS A TECHNIQUE FOR SEPARATION AND QUANTIFICATION OF COMPLEX SAMPLES CONTAINING SEVERAL ANALYTES. GENERALLY, FOR HEAVY METAL ANALYSIS ATOMIC SPECTROSCOPIC METHODS ARE PREFERRED. BUT WITH APPROPRIATE DERIVATIZATIONS, WE CAN DEVELOP CHROMATOGRAPHIC METHODS FOR THIS PURPOSE [1].HOLLOW FIBER SUPPORTED LIQUID-PHASE MICROEXTRACTION (HFLPME) OFFERS AN EFFICIENT ALTERNATIVE TO CLASSICAL TECHNIQUES FOR SAMPLE PREPARATION AND PRECONCENTRATION. HF-LPME RELIES ON THE EXTRACTION OF TARGET ANALYTES FROM AQUEOUS SAMPLES INTO A SUPPORTED LIQUID MEMBRANE (SLM) SUSTAINED IN THE PORES OF THE WALL OF A POROUS HOLLOW FIBER, AND THEN INTO AN ACCEPTOR PHASE (THAT CAN BE AQUEOUS OR ORGANIC) IN THE LUMEN OF THE HOLLOW FIBER. AFTER EXTRACTION, THE ACCEPTOR SOLUTION IS DIRECTLY SUBJECTED TO A CHEMICAL ANALYSIS [2]. IN THIS STUDY, A HOLLOW FIBER LIQUID PHASE MICROEXTRACTION (HF-LPME) METHOD WAS USED FOR PRECONCENTRATION OF CO (II), FE (III) AND AL (III) CATIONS AS THEIR OXINATE COMPLEXES FROM WATER SAMPLES. VARIOUS PARAMETERS LIKE LIGAND AND ITS CONCENTRATION, EXTRACTION PH, ACCEPTOR SOLVENT AND … WERE OPTIMIZED. N-OCTANOL WAS LOADED IN THE POROUS WALL OF THE HOLLOW FIBER AND TOLUENE WAS SELECTED AS THE BEST ACCEPTOR SOLVENT IN THE LUMEN OF THE HOLLOW FIBER. PHOSPHATE BUFFER WAS USED FOR ADJUSTING PH (PH=8). SEPARATION AND QUANTIFICATION OF THE ANALYTES WAS PERFORMED USING HIGH PERFORMANCE LIQUID CHROMATOGRAPHY WITH UV DETECTION (MOBILE PHASE: METHANOL: WATER (65: 35) +0.03 M OXINE, COLUMN: C18, 4.6×250 MM, 5 ΜM, DETECTOR: 380 NM). FINALLY THE METHOD WAS SUCCESSFULLY APPLIED FOR DETERMINATION OF THE CO (II), AL (III) AND FE (III) CATIONS IN RIVER WATER, WELL WATER AND WASTE WATER SAMPLES.