Rice husk (RH) agro-waste was used as a raw material for synthesizing mesoporous molecular sieves, MCM-41. The Fe-MCM-41 was prepared by the hydrothermal technique (HT), resulting in a higher surface area and crystallinity than when prepared under ambient conditions. In addition, a hexagonal structure was clearly seen with hydrothermal technique (HT) preparation. The adsorption of arsenate by HT-Fe-MCM-41 was investigated. The factors studied affecting arsenate adsorption capacity were ferric content in MCM-41, contact time, pH of solution, and initial arsenate concentration. It was found that HT-Fe-MCM-41 at the Si/Fe mole ratio of 10 gave the highest adsorption capacity. Arsenate adsorption reached equilibrium within 4 h. The adsorption capacity of HT-Fe-MCM-41 (Si/Fe = 10) was affected by the initial pH value and the initial arsenate concentration. The adsorption capacity was highest at pH 3 and decreased thereafter with increases in the pH of solution value. The Langmuir model fit the arsenate adsorption isotherm well. The maximum adsorption capacity for arsenate was 1,111 microg g(-1).