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The novel organic compound of ammonium (4-chlro-2-mercaptophenyl)carbamodithioate (ACMPC) was prepared and then subsequently grafted onto the mesoporous silica by direct approach for the preparation of composite adsorbent (CPA). The lanthanide (Ln(III)) intra-series separation behavior was measured using CPA and then the samarium (Sm(III)) ion was selected according to the high adsorption ability by CPA for effective separation, adsorption, and recovery in the solid-liquid approach. The mesoporous silica and CPA were characterized systematically for the evaluation of affecting experimental criterion. The solution acidity played an important factor as the alkaline pH area was avoided due to the hydroxide precipitation probability and pH 5.0 was selected for selective and effective Sm(III) ion separation and recovery. The data clarified that CPA exhibited high kinetic performances with high adsorption …