A dispersive liquid–liquid microextraction (DLLME) method was developed for the determination of aluminium. An appropriate mixture of methanol and chloroform was injected rapidly into the aqueous sample containing aluminium–pyrocatechol violet complex and cetyltrimethyl ammonium bromide (CTAB) ione paire as a result cloudy mixture was formed [1]. After this stage, centrifugation was used to sediment these droplets to the bottom of the conical tube. After removing bulk aqueous phase by a microsyringe, proper type and volume of solvents were adapted to properly dilute the concentrated samples, considering the sampling demand of spectrophotometer. After that, the resultant sample solutions were transported to UV-Vis spectrophotometer for the determination of aluminium. The influence factors relevant to DLLME, such as type and volume of extractant and disperser solvent, concentration of chelating reagents, pH, salt effect, extraction time, centrifugation time, interferences were investigated and optimized [2]. Finally, The proposed DLLME technique was successfully applied for the determination of aluminium in various natural water and medicine and blood sampls[3