Synthesis of Aminopropyl Triethoxysilane-Functionalized Silica and Its Application in Speciation Studies of Vanadium(iv) and Vanadium(v)

Abstract

A solid phase extraction sorbent, aminopropyl triethoxysilane-functionalized silica was prepared and used for vanadium speciation prior to inductively coupled plasma mass spectrometric determination. The necessary sorption parameters such as sorption pH, reaction temperature, sorbent amount and sample volume were optimized. The sorption for V(V) and V(IV) under the optimized conditions was 98% (±1) and was lower than 10%, respectively. The sorption process was investigated both from a kinetic perspective and also in terms of Freundlich, Dubinin-Radushkevich and Langmuir isotherm models to characterize the uptake of vanadate ion by the functionalized silica. Desorption from the sorbent was realized with 0.5 mol L−1 thiourea prepared in 0.2 mol L−1 HCl. Among the possible interfering species tested, Te(IV), Se(IV), Se(VI) and Fe(III) showed interference effects with V(V) signal. The validity of the method was first checked via spike recovery experiments with four different types of water; namely ultra pure, bottled drinking, tap, and sea water for different concentrations of V(V). The percent recovery values changed between 87 and 108 for all water types. The accuracy of the proposed methodology was also checked by analyzing a standard reference material (NIST, SRM 1643e) and a good agreement was found between the determined and the certified value. The proposed methodology has also been shown to be applicable for the separate sorption of V(V) in the absence/presence of V(IV) and for the sorption of both V(IV) and V(V) in waters. The amount of V(IV) can then be determined from the difference.