The use of hydrotalcite in catalysis has wide attention in academic research and industrial parties. Based on its utilization, hydrotalcite can be active catalyst or support. This research is focused on the investigation of characteristic like spesific surface area of Mg-Al hydrotalcite which is prepared with different temperature of calcination. Synthesis of Mg-Al hydrotalcites with Mg/Al molar ratio 3:1 were prepared by co-precipitation method. Mg(NO 3 ) 3 .6H 2 O and Al(NO 3 ) 3 .9H 2 O as precursors of Mg-Al hydrotalcite. Na 2 CO 3 was used as precipitant agent and NaOH was used as buffer solution. The solution was mixed and aging for 5 hours at 650 o C. The dried precipitate was calcined at 2500 o C, 3500 o C, 450 o C, 550 o C and 650 o C. The characterization of functional group was determined by Fourier Transform Infra Red (FT-IR). The Identical peaks diffractogram were analyzed by X-Ray Diffraction (XRD). The spesific surface area was determined by adsorption-desorption of nitrogen. The largest surface area that obtained from the calcination temperature of 650 o C is 156.252 m 2 /g.