A novel method is proposed for the extraction of microgram level concentration of iridium(III) from malonate medium with 4-(4-methoxybenzylideneimino)-5-methyl-4H-1,2,4-triazole-3-thiol(MBIMTT) dissolved in chloroform as an extractant. The iridium(III) from the organic phase is stripped with 2 M hydrochloric acid and determined spectrophotometrically with stannous chloride method. The method affords the binary separation and determination of iridium(III) from the alloys and synthetic mixture. The method is highly selective, simple and re-producible