SEMICONDUCTOR NANOPARTICLES OR QUANTUM DOTS (QDS) HAVE DEVELOPED AS LUMINESCENT PROBES FOR SENSING EVENTS [1]. QDS, AS A BRAND NEW CLASS OF FLUORESCENT RECEPTORS, HAVE THE THREE DIMENSIONS CONFINED TO 1–8 NM LENGTH SCALE. QDS POSSESS AN EXCELLENT PHOTOSTABILITY, HIGH QUANTUM YIELDS, AND LONG FLUORESCENCE LIFETIMES [2]. HOWEVER, DUE TO THE UNIQUE AND NOVEL PROPERTIES OF THE QD BASED LUMINESCENT SENSORS SUCH AS LOW COST FABRICATION, RELIABILITY, REPRODUCIBILITY, ACCURACY, HIGH SENSITIVITY AND SELECTIVITY, EXPANDING APPLICATIONS OF QDS TO DEVELOP INORGANIC ANIONS, CATIONS, DRUGS, ORGANIC DYES, EXPLOSIVE COMPOUNDS AND BIOMOLECULAR SENSORS IS A TOPIC OF CURRENT INTEREST [3].IN THIS RESEARCH, A RAPID AND SIMPLE FLUORESCENCE METHOD IS PRESENTED FOR SELECTIVE AND SENSITIVE DETERMINATION OF HAZARDOUS CYANIDE ION IN AQUEOUS SOLUTION BASED ON FUNCTIONALIZED ZINC SULFIDE (ZNS) QUANTUM DOT AS LUMINESCENT PROB. THE ULTRA-SMALL ZNS QDS WERE SYNTHESIZED USING A CHEMICAL CO-PRECIPITATION METHOD IN THE PRESENCE OF 2-MERCAPTOETHANOL (ME) AS AN EFFICIENT CAPPING AGENT. THE PREPARED PURE ZNS QDS WAS APPLIED AS AN OPTICAL SENSOR FOR DETERMINATION OF CYANIDE IONS IN AQUEOUS SOLUTIONS. ZNS NANOPARTICLES HAVE EXHIBITED A STRONG FLUORESCENT EMISSION AT ABOUT 424 NM. THE FLUORESCENCE INTENSITY OF QDS IS LINEARLY PROPORTIONAL TO THE CYANIDE ION CONCENTRATION IN THE RANGE 2.44×10-6 TO 2.59×10-5 M WITH A DETECTION LIMIT AS 1.70×10-7 M AT PH 11. THE DESIGNED FLUORESCENT SENSOR POSSESSES REMARKABLE SELECTIVITY FOR CYANIDE ION OVER OTHER ANIONS SUCH AS CL-, BR-, F-, I-, IO3-, CLO4-, BRO3-, CO32-, NO2-, NO3-, SO42-, S2O42-, C2O42-, SCN-, N3-, CITRATE AND TARTARATE WITH NEGLIGIBLE INFLUENCES ON THE CYANIDE DETECTION BY FLUORESCENCE SPECTROSCOPY.