ANTIMONY (SB) IS USUALLY FOUND IN TWO OXIDATION STATES (III AND V) IN ENVIRONMENTAL, BIOLOGICAL AND GEOCHEMICAL SAMPLES. DETERMINATION OF ANTIMONY IS OF GREAT IMPORTANCE OWING TO THE LARGE DIFFERENCES REGARDING THEIR TOXIC PROPERTIES. ELEMENTAL ANTIMONY IS MORE TOXIC THAN ITS SALTS, AND GENERALLY, TRIVALENT ANTIMONY COMPOUNDS HAVE HIGHER TOXICITY THAN THE PENTAVALENT ANTIMONY SPECIES. PENTAVALENT ANTIMONIALS, INCLUDING MEGLUMINE ANTIMONIATE, ARE THE DRUGS OF CHOICE FOR THE TREATMENT OF LEISHMANIASES. SINCE ANTIMONY IS THE ACTIVE SPECIES, THE KNOWLEDGE OF THE EXACT METAL CONCENTRATION IN COMMERCIAL FORMULATIONS IS CRITICAL FOR ITS CLINICAL USE [1, 2].RECENTLY, Optical CHEMICAL sensorS THAT POSE AN APPROPRIATE SENSING LAYER WITH THE ABILITY FOR SELECTIVE AND REVERSIBLE RECOGNITION OF THE ANALYTES HAVE SEEN A GROWTH IN INTEREST.Optical sensorS (OPTODES) ARE A PARTICULAR TYPE OF CHEMICAL sensor WHERE SPECTROSCOPIC MEASUREMENTS ASSOCIATED WITH CHEMICAL REACTIONS ARE CARRIED OUT. OPTODES FOR HEAVY METAL IONS, AS VIABLE ALTERNATIVES TO OTHER TYPES OF sensorS, OFFER SEVERAL ADVANTAGES SUCH AS EASE OF PREPARATION AND PROCEDURES, SMALL SIZE, LOW COST, RELATIVELY FAST RESPONSE, WIDE RESPONSE RANGE, REASONABLE SELECTIVITY AND HIGH SENSITIVITY [3, 4].IN THE PRESENT WORK, AN Optical CHEMICAL sensor FOR THE DETERMINATION OF ANTIMONY HAS BEEN CONSTRUCTED BY IMMOBILIZATION OF METHYLTRIOCTYLAMMONIUM CHLORIDE ON TRIACETYLCELLULOSE MEMBRANE. THE EXCHANGE OF CHLORIDE AS COUNTER ION WITH IODIDE IN THE MEMBRANE CHANGES THE COLORLESS FILM TO YELLOW, WHEN IT IS PLACED IN ACIDIC SOLUTION CONTAINING SB (III) AND ASCORBIC ACID. THE sensor CAN READILY BE REGENERATED BY 0.1 MOL L-1 SODIUM CITRATE SOLUTION. UNDER OPTIMUM CONDITIONS, THE PROPOSED MEMBRANE IS CAPABLE OF DETERMINING SB (III) OVER A DYNAMIC RANGE BETWEEN 6.5 × 10-7 AND 2.3 × 10-4 MOL L-1 WITH A LIMIT OF DETECTION 3.3 × 10-7 MOL L-1. THE RELATIVE STANDARD DEVIATION FOR EIGHT REPLICATE MEASUREMENTS OF 1.96 × 10-5 AND 1.31 × 10-4 MOL L-1 OF SB WAS 4.28 AND 1.20 %, RESPECTIVELY. THE sensor WAS SUCCESSFULLY APPLIED TO THE DETERMINATION OF ANTIMONY IN DRUG AND WATER SAMPLES.