In this study, cadmium(II) has been extracted with 10 mL of 0.0001 M acetyl derivative of calix(6)arene at pH 8.0 by equilibrating for 5 mm Cadmium(II) is stripped quantitatively with 0.5 N hydrochloric acid and determined photometrically by complexation with 4-(2-pyridylazo)resorcinol at 495 nm. The method affords the binary separation of cadmium from associate elements and is further extended to analyse the synthetic mixtures. The nature of the extracted species is determined from the log-log plots. The result shows the formation of an ion pair complex [Cd(HR)(2)](org) in the organic phase. The temperature dependence of the extraction equilibrium is examined by the temperature variation method. The value of square H-0 = +160485.48 J mole(-1) indicates that the extraction reaction is endothermic. The metal loading capacity of the reagent is found to be 150 ppm. The proposed method is applicable to the analysis of real samples and the results obtained are found to be reproducible and accurate.