Silica gel is an amorphous inorganic polymer containing an internal siloxane group (Si-O-Si) with silanol groups (Si-OH) distributed on the surface.1,2 It is commonly used as a rigid matrix for ligand immobilization. 3 The chemical modification of silica gel surfaces with donor atoms such as N, S, O and P is primarily aimed at improving the adsorption and exchange properties of the silica gel along with incorporation of the particular selective characteristics into the modified silica gel phases towards certain metal ions. 4 The immobilization of chelating materials containing donor atoms on the silica gel surface can occur via chemical bond formation between organic modifiers like amino or chloro modified silica gel phases or through simple physical adsorption processes.5 Such a process often incorporates selectivity in synthesized materials. 6,7 Several new chemically modified silica gels were synthesized, and applied as normal or selective solid phase extractor for many toxic and other metal ions. They were found to be superior to the conventional ion exchange resins in their ability to extract and selectively preconcentrate the heavy metal ions from solutions containing high concentrations of alkali and alkaline earth metal ions. [8][9][10] Advantages of the modified solid phase extractors compared with the classical liquid extractor's were reported in many references.
11,12Schiff bases, having multidentate coordination sites, are known to form complexes with transition metal ions readily.
13,14The Schiff bases derived from salicylaldehyde (Salens) as polydentate ligands are known to form stable complexes with transition metal ions. 15,16 The present work describes the syntheses of two new chemically modified silica gel covalently bonded with 4,4′-diaminodiphenylether and 4,4′-diaminodiphenylsulfonesalicylaldehyde Schiff bases.The synthesized chelating materials were used for the preconcentration and separation of Cr 3+ , Zn 2+ , and Mn 2+ from dilute aqueous solutions. They were compared to determine their metal binding, extraction and selective abilities using batch techniques. The more reactive chelating material, Si-DDE-o-HB, was utilized in a column technique for the preconcentration of Zn 2+ and Cr 3+ . Elution of the sorbed cations in column experimental studies provided an example of using the chelating material in continuous cycle operation and recovery of the metal ions. The analytical precision and accuracy of the result were tested with satisfactory results, and the method was found to be rapid, precise, simple and convenient to use.
Experimental
ApparatusThe specific surface areas of the dry silica and loaded silica were determined by BET method on NOVA 1000, high speed gas sorption analyzer, Quantachrome Corporation, USA. A Shimadzu atomic absorption spectrophotometer (Model AA-680) equipped with a single element hollow cathode lamp and an air-acetylene burner was used for the estimation of metal ions. The instrument parameters were those recommended by the manufacturer. The wave lengths (nm) s...