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Magnetic iron oxide-silica shell nanocomposites with different iron oxide/silica ratio were synthesized and structurally characterized by Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), small-angle neutron scattering, magnetic and N2-sorption studies. The composite that resulted with the best properties in terms of contact surface area and saturation of magnetization was selected for Pb2+ adsorption studies from aqueous media. The material presented good absorption capacity (maximum adsorption capacity 14.9 mg·g−1) comparable with similar materials presented in literature. Its chemico-physical stability and adsorption capacity recommend the nanocomposite as a cheap adsorbent material for lead.

Fe(acac)3/silica/PVA hybrid xerogel nanocomposite was obtained by one pot acid catalysed sol-gel synthesis using the homogeneous mixture of iron(III) acetylacetonate (Fe(acac)3), tetraethylorthosilicate (TEOS), and polyvinyl alcohol (PVA). Nominal composition ratio of iron oxide/silica was 15/85 (weight percent). Nitric acid was used as catalyst. Another sample of Fe(acac)3/silica xerogel without PVA addition was prepared in the similar processing conditions. Based on thermal analysis studies, the thermal behaviour of both xerogel samples was unveiled and it allowed choosing the optimal calcination temperatures in order to obtain iron oxide silica magnetic nanocomposite samples. The two xerogel (with and without PVA) samples were thermally treated, in air, at 220, 260 and 300 °C and characterized by different techniques. XRD investigations revealed phase composition evolution with calcination temperature, from cubic spinel phase (maghemite) to hexagonal stable hematite containing nanocomposite of 10–20 nm average crystallite size. These findings were confirmed by Mössbauer spectroscopy. Up to 300 °C, the surface area and total pores volume increased with temperature for all samples. By calcination at the same temperature, the hybrid xerogel containing PVA resulted in significantly higher magnetization and free volume values in comparison with the sample without PVA.