This research used raw kaolinite (RK), thermally activated Kaolinite (TAK), hydroxyiron (iii) kaolinitecomposite (HKC), as adsorbent for the adsorption of phenol and cadmium from aqueous solutions over a concentration range of 5-25 mg/l and 10-50 mg/l respectively. Effect of initial pH on the adsorbates was carried out at pH 2-11 at (298 K), and adsorbent dosage from 0.5-2.5 g with 50 ml adsorbate solution. Adsorption thermodynamics were developed for 25-55°C for 5-25 mg/L and 10-50 mg/L of phenol and cadmium solutions for 1 hr for all the adsorbents. The Physicochemical characteristics of RK, TAK and HKC were shown to be: