In this work MgO/Al_2O_3 nanocomposites with weight ratios from 5% to 25% were synthesized by precipitationimpregnation method and their structural properties were characterized. In the next step, the capability of the nanocomposites in H_2S removal compared to Mg–Al spinel(MgAl_2O_4), synthesized through ion-pair complex precursor route and alumina samples, prepared via sol–gel precipitation methods, was investigated. The results indicated that among the studied sorbents Mg–Al spinel presents a distinctly higher H_2S removal. In addition, the MgO/Al_2O_3 nanocomposites compared to the alumina sorbents, exhibited much better performance in H_2S removal. Also CO_2-TPD analysis reveals higher amounts of basic sites for Mg–Al spinel compared to 25 wt% MgO/75 wt% Al_2O_3 nanocomposite. In this work MgO / Al_2O_3 nanocomposites with weight ratios from 5% to 25% were synthesized by precipitation impregnation method and their structural properties were characterized. In the next step, the capability of the nanocomposites in H_2S removal compared to Mg-Al spinel (MgAl_2O_4) , synthesized through ion-pair complex precursor route and alumina samples, prepared via sol-gel precipitation methods, was investigated. The results indicated that among the studied sorbents Mg-Al spinel presents a distinctly higher H2_2 removal. In addition, the MgO / Al 2 O 3 nanocomposites compared to the alumina sorbents, exhibited much better performance in H_2S removal. Also CO_2-TPD analysis reveals higher amounts of basic sites for Mg-Al spinel to 25 wt% MgO / 75 wt% Al_2O_3 nanocomposite.