A Zn/Al hydrotalcite-like compound (HTlc) was prepared by co-precipitation (at constant pH) method and was characterized by XRD, TG/DTA, FTIR, and BET surface area. The ability of Zn/Al oxide to remove F- from aqueous solution was investigated. All the adsorption experiments were carried out as a function of time, pH, concentration of adsorbate, adsorbent dose, temperature etc. It was found that the maximum adsorption takes place within 4 h at pH 6.0. The percentage of adsorption increases with increase in the adsorbent dose, but decreases with increase in the adsorbate concentration. From the temperature variation it was found that the percentage of adsorption decreases with increase in temperature, which shows that the adsorption process is exothermic in nature. The adsorption data fitted well into the linearly transformed Langmuir equation. Sulfate and phosphate were found to have profound effects on fluoride removal. Thermodynamic parameters such as DeltaG(0), DeltaH(0), and DeltaS(0) were calculated. The negative value of DeltaH(0) indicates that the adsorption process is exothermic. The apparent equilibrium constants (K-a) are also calculated and found to decrease with increase in temperature. With 0.01 M NaOH the adsorbed F- could be completely desorbed from Zn/Al oxide in 6 h. (C) 2003 Elsevier Science (USA). All rights reserved.