Solid phase extraction of Pb(II) in water samples using a new hybrid inorganic-organic mesoporous silica prior to its determination by FAAS

A mesoporous silica has been chemically modified with 5-mercapto-1-methyltetrazole. The newly synthesized material was characterized by powder X-ray diffraction, N2 adsorption, FT-IR, 13C-NMR spectroscopy and elemental analysis, and used to preconcentrate Pb(II) from aqueous solutions. The effect of several variables on the adsorption capacity (i.e. stirring time, pH, interfering ions, presence of other heavy metals in the medium, etc.) has been studied using batch and column techniques. The adsorption capacity of the material followed the order: Pb(II) >> Cu(II) > Cd(II) >>Mn(II) > Ni(II) > Co(II). In column experiments a pre-concentration factor of 200 was obtained for Pb(II). Spiked tap water, mineral water and river water were used for the preconcentration and determination of Pb(II) by flame atomic absorption spectrometry, and a 101–103% recovery was obtained. The limit of detection and quantification values of the method were found to be 2.22·10−6 mM and 8.20·10−6 mM, respectively. The relative standard deviation for four preconcentration experiments was found to be ≤9% in all cases.