A simple route for preparation of organically modified spherical silica (SiO2) nanoparticles with CYANEX 921 has been discussed. These modified particles has been used to remove Fe3+-SCN complex from 9M phosphoric acid. SEM, XRD, IR and EDS have been used to Characterized the powder in its several stages. The effect of SiO2 weight, thiocyanate concentration, initial Fe (III) concentration, H3PO4 concentration, stirring time, temperature and loaded SiO2 weight have been used to study the removal percent. The loaded silica succeeded in removal of 70% of Fe (HI). Langmuir isotherm model well fit the experimental data with maximum sorption capacity 45.45 mg/g. The reaction kinetic is found to follow the pseudo second order kinetic model the adsorption reaction shows exothermic behavior.