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Ethylenediaminetetraacetic acid (EDTA) functionalized silica adsorbent has been synthesized using (3-aminopropyl) triethoxylsilane (APTES) as a bridging link between silanol groups (SiOH) of silica and carboxylic group of EDTA. Fourier transform infrared spectroscopy (FTIR) and Temperature-programmed oxidation (TPO) analysis confirmed the grafting of EDTA onto the silica. The synthesized EDTA-silica was investigated as an adsorbent for removal of Cu(II), Zn(II) and Ni(II) from aqueous solution. The effect of solution pH, initial solution concentration, and contact time were studied. The removal of metal ions increased with the increase in solution pH, contact time and concentration. The maximum equilibrium time was found to be 45min for all three metal ions. Kinetics studies revealed that the adsorption of Cu(II), Zn(II) and Ni(II) onto EDTA-silica followed the pseudo-second order kinetics and film diffusion and intra-particle diffusion mechanism were involved. Adsorption equilibrium data were well fitted to Langmuir isotherm model and maximum monolayer adsorption capacity for Cu(II), Zn(II) and Ni(II) was 79.36, 74.07 and 67.56mg g(-1), respectively. Thermodynamic results reveal that the removal of metals onto EDTA-silica was endothermic and spontaneous in nature., (Copyright © 2013 Elsevier Inc. All rights reserved.)

Deactivation mechanisms of alumina-supported, Ni-based catalysts for tar reforming in biomass-derived syngas were evaluated using extended X-ray absorption fine structure (EXAFS) spectroscopy. Catalysts were characterized before and after catalytic reaction cycles and regeneration procedures, which included oxidation by a mixture of steam and air, and reduction in hydrogen. Qualitative analysis of the EXAFS spectra revealed that oxidation of a portion of the Ni in the catalysts to form an oxide phase and/or a sulfide phase were likely scenarios that led to catalyst deactivation with time-on-stream and with increased reaction cycles. Deactivation through carbon deposition, phosphorus poisoning, or changes in particle size were deemed as unlikely causes. Quantitative analysis of the EXAFS spectra indicated sulfur poisoning occurred with time-on-stream, and the contaminating species could not be completely removed during the regeneration protocols. The results also verified that Ni-containing oxide phases (most likely a spinel also containing Mg and Al) formed and contributed to the deactivation. This study validates the need for developing catalyst systems that will protect Ni from sulfur poisoning and oxide formation at elevated reaction and regeneration temperatures.