Sodium dodecyl sulphate-ironsilicophosphate (SDS-FeSP) nanocomposite has been fabricated by using co-precipitation method. The resultant SDS-FeSP nanocomposite showed excellent ion exchange capacity, high stability and selectivity towards specific metal ions. The characterization of SDS-FeSP nanocomposite was carried out by using modern techniques including TEM, SEM-EDX and FTIR. SDSFeSP had higher ion exchange capacity (1.45 meq/g) in comparison to its inorganic counterpart FeSP (0.40 meq/g). The physicochemical properties such as pH titrations, elution behavior and thermal stability of SDS-FeSP were examined to find their relation in the context of enhanced ion exchange capacity. The sorption studies for several alkaline and heavy metals were performed in two different eluents. The studies revealed marked selectivity of SDS-FeSP nanocomposite towards Zn2+ and Mg2+ metal ions. Hence, analytical utility of SDS-FeSP nanocomposite was accomplished by performing some binary separations as well as quantitative separation of Mg2+ metal ion from a real sample (Digene) on the column packed with the synthesized SDS-FeSP. (C) 2017 Elsevier B.V. All rights reserved.