Novel route for silylation of silica gel and aliphatic amines immobilization based on microwave-assisted solvent free synthesis and their applications for Cu(II) and Fe(III) removal from natural water samples

Abstract

This article describes a new route for silica gel silylation and immobilization of aliphatic amines based on microwave-assisted solvent free synthesis to produce new solid phase extractors. The mode of synthesis was optimized under microwave conditions and achieved in a short time without using solvents. The produced phases named: silica gel- monoamine (SG-MA), silica gel- ethylenediamine (SG-EDA) and silica gel- diethylenetriamine (SG-DETA). The selectivity of these phases towards the uptake of Cu(II) and Fe(III) was checked using batch equilibration technique. Microwave radiation power and time of radiation were optimized to obtain the highest metal uptake values. The novel synthesized silica amine phases were characterized using Fourier transform infrared spectra and scanning electron microscope. The effects of different parameters including, hydrogen ion concentration, initial metal ion concentration, mass of the phase and shaking time on binding capacities of both Cu(II) and Fe(III) were explored. Results of sorption isotherms of the phases were better fitted with the Langmuir model (r² ≥ 0.950). In addition, the kinetics data were best fitted with the pseudo–second-order type (r² = 0.999). Application of SG-MA for removal of Cu(II)- and Fe(III)-spiked natural water samples was achieved satisfactorily using batch experiments. The results were found to refer to superior recovery percentages (90.0–97.01 ± 0.010–0.521%) with no significant matrix interferences.

Keywords:

• Silica gel
• monoamine
• ethylenediamine
• diethylenetriamine
• radiation
• heavy metal ions
• real water samples
• isotherm
• kinetics.