MIL-53(Fe) material has been successfully synthesized by the hydrothermal method from FeCl3-6H2O combined with terephthalic acid organic linker in the presence of DMF. The material was characterized by a variety of modern methods including X-ray diffraction (XRD), infrared (IR), transmission electron microscopy (TEM), thermo gravimetric analysis (TGA) and Adsorption-Desorption isotherms method. The XRD patterns represented that MIL-53(Fe) had well crystalline structures. The material was a highly crystallized yellow powder with a very large surface area of about 3000 m2/g. The vapor-phase adsorption of benzene and the liquid-phase adsorption of arsenic were investigated. The results showed that the maximum adsorption capacity for benzene at the relative pressure P/Po - 1 was about 500 mg/g, the saturated adsorption capacity for arsenic (C/arsenic = 100 ppm) was about 50 mg/g.