The chemiluminescence (CL) that accompanies the oxidation of acetonitrile with aqueous sodium peroxide in alkaline medium was studied in the presence and absence of luminol. The reaction occurring between acetonitrile and alkaline KOH solution of aqueous sodium peroxide lead to the production of oxygen gas with simultaneous emission of light (CL), which has been detected by PMT and recorded with the aid of PC using interface. The weak CL intensity was enhanced by addition of 10-3 M luminol solution. The influence of concentration of various constituents of the reaction and pH of medium was investigated. The effect of antibiotic sensitizer ciprofloxacin has also been studied.