A cloud point extraction process using mixed micelle of the cationic surfactant CTAB and non-ionic surfactant Triton X-100 to extract thorium(IV) from aqueous solutions was investigated. The method is based on the color reaction of thorium with 5-(2`,4`-dimethylphenylazo)-6-hydroxypyrimidine-2,4-dione (DMPAHPD) in the presence of potassium iodide in hexamethylenetetramine buffer media and mixed micelle-mediated extraction of complex. The optimal extraction and reaction conditions (e.g. surfactant concentration, reagent concentration, effect of time) were studied and the analytical characteristics of the method (e.g. limit of detection, linear range, molar absorptivity, Sandell sensitivity, preconcentration, and improvement factors) were obtained. Linearity was obeyed in the range of 0.5-15 ng mL − 1 of thorium(IV) ion and the detection limit of the method is 0.16 ng mL − 1 . The interference effect of some anions and cations was also tested. The proposed method was successfully applied for the preconcentration of trace thorium in natural water samples as well as in plant material and soil samples prior to its determination by inductively coupled plasma atomic emission spectrometry (ICP-AES) with satisfactory results. A Perkin-Elmer Lambda 12 UV/Vis spectrometer was used for recording absorbance spectra with 1.0-mm quartz cell. A Perkin Elmer model 5300 DV; ICP-AES (Waltham, MA, USA) was used for all ICP-AES measurements. An Orion research model 601 A/digital ionalyzer pH meter was used for checking the pH of solutions. A water bath with good temperature control and a centrifuge with 10-mL calibrated centrifuge tubes (Superior, Germany) were used to accelerate the phase separation process. Tabletop Low Speed Large Capacity Centrifuge model L-550 was used Reagents Unless otherwise stated, reagents of analytical purity were used for all experiments and doubly distilled water (DDW) was used throughout. The surfactants, Triton X-100 and cethyltrimethylammonium bromide (CTAB) (obtained from Sigma company) were used without further purification. Stock solution of thorium at a concentration of 0.025 M thorium(IV) solution is prepared by dissolving 3.675 g of thorium nitrate [Th(NO 3 ) 4 .6H 2 O] in distilled water containing a few drops of nitric acid. The solution is made upto 250 mL and standardized gravimetrically by employing the iodide method. 0.1 M. working standard solutions were obtained by appropriate dilution of the stock. 5-(2`,4`-Dimethylphenylazo)-6-hydroxypyrimidine-2,4-dione (DMPAHPD) was prepared using conventional diazotization and coupling methods. 25 A solution of 1.0×10 − 3 M of DMPAHPD was prepared by dissolving appropriate amounts of this reagent in bidistilled water. The solution pH 7.8 ± 0.2 was adjusted with hexamethylenetetramine (HTM)/ hydrochloric acid buffer. N,N-dimethyl formamide (DMF) solvent and potassium iodide salt were purchased from Merck.