DYES ARE WIDELY USED IN INDUSTRIES SUCH AS THE TEXTILE, PULP MILL, PAPER PRODUCTION, FOOD TECHNOLOGY, PRINTING, LEATHER TANNING, AND PLASTICS INDUSTRIES. MANY DYES ARE TOXIC TO SOME ORGANISMS, CARCINOGENIC AND MUTAGENIC TO HUMANS. METHYL ORANGE (MO) IS AN INTENSELY COLORED AZO DYE COMPOUND WHICH IS WIDELY USED FOR DYEING AND PRINTING OF TEXTILES, PHARMACEUTICAL, FOOD INDUSTRIES AND AS INDICATOR. THE PRESENCE OF AZO GROUP (N=N) ON MO AND ITS LOW BIODEGRADABILITY MAKES IT AN ISSUE OF CONCERN FOR ENVIRONMENTAL SCIENCE. MO IS REGARDED AS ALLERGY MATERIALS AFTER CONTACTING BY SKIN, WHICH CAUSES SHIN ECZEMA AND EVEN BE POISONOUS IF SWALLOWED [1]. THEREFORE, THE DEVELOPMENT OF SIMPLE AND SENSITIVE ANALYTICAL METHODS FOR ACCURATE DETERMINATION OF TRACE AMOUNT OF METHYL ORANGE IS IMPORTANT FOR ITS ENVIRONMENTAL MONITORING. DISPERSIVE LIQUID-LIQUID MICROEXTRACTION (DLLME) IS AN ATTRACTIVE MODE OF LIQUID MICROEXTRACTION WHICH HAS RECEIVED MUCH ATTENTION FOR SAMPLE PRETREATMENT. THIS METHOD HAS BEEN APPLIED FOR THE SEPARATION AND PRECONCENTRATION OF TRACE METAL IONS AND ORGANIC POLLUTANTS IN THE DIFFERENT MATRICES [2, 3]. IN THE PRESENT STUDY A DISPERSIVE LIQUID-LIQUID MICROEXTRACTION (DLLME) METHOD COUPLED TO UV-vis spectrophotometry IS DEVELOPED FOR THE SENSITIVE DETERMINATION OFMETHYL ORANGE. THE METHOD IS BASED ON EXTRACTION OF METHYL ORANGE WITH DLLME PROCEDURE USING CARBON TETRACHLORIDE (EXTRACTION SOLVENT) CONTAINING METHYLTRIOCTYL AMMONIUM CHLORIDE WHICH PROVIDES COUNTER ION AND ALSO ACTS AS AN DISPERSER. AFTER EXTRACTION, THE PHASE SEPARATION IS PERFORMED WITH A RAPID CENTRIFUGATION, AND METHYL ORANGE IS DETERMINED IN THE ENRICHED PHASE BY UV-vis spectrophotometry. UNDERTHE OPTIMUM EXTRACTION CONDITION, THE METHOD YIELDS A LINEAR CALIBRATION CURVE IN THE CONCENTRATION RANGE OF 5 TO 400 NG ML-1, AND THE LIMITS OF DETECTION WAS 1.53 NG ML-1 FOR TARGET ANALYTES. THE RELATIVE STANDARD DEVIATION FOR TEN REPLICATE MEASUREMENTS OF 50 AND 300 NG ML-1 OF METHYL ORANGE WAS 3.61 AND 1.43%, RESPECTIVELY. THE PROPOSED METHOD WAS SUCCESSFULLY APPLIED TO DETERMINATION OF TRACE AMOUNTS OF METHYL ORANGE IN REAL SAMPLES WITH SATISFACTORY RESULTS.