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PubMed2004

ToF-SIMS depth profiling analysis of the uptake of Ba2+ and Co2+ ions by natural kaolinite clay.

The sorption behavior of Ba(2+) and Co(2+) ions on a natural clay sample rich in kaolinite was studied using time-of-flight secondary ion mass spectrometry (ToF-SIMS). Depth profiling at 10-A steps was performed up to a 70-A matrix depth of the clay prior to and following sorption. The results showed that Co(2+) is sorbed in slightly larger quantities than Ba(2+), with significant numbers of ions fixed on the outermost surface of the clay. Depletion of the ions K(+), Mg(2+), and Ca(2+) from the clay lattice was observed to accompany enrichment with Co(2+) and Ba(2+) ions. The data obtained using X-ray powder diffraction (XRPD) and scanning electron microscopy (SEM) indicated insignificant structural and morphological changes in the lattice of the clay upon sorption of both Ba(2+) and Co(2+) ions. Analysis using energy dispersive X-ray spectroscopy (EDS) showed that the average atomic percentage (+/-S.D.) of Ba and Co on kaolinite surface were 0.49 +/- 0.11 and 0.61 +/- 0.19 , respectively, indicating a limited uptake capacity of natural kaolinite for both ions.

Aluminum Silicates↗
PubMed2005

First insight into catalytic activity of anionic iron porphyrins immobilized on exfoliated layered double hydroxides.

Mg-Al layered double hydroxide (LDH) intercalated with glycinate anions was synthesized through co-precipitation and exfoliated in formamide and the single-layer suspension was reacted with aqueous iron porphyrin solutions (Fe(TDFSPP) and Fe(TCFSPP)). The obtained materials were characterized by X-ray powder diffraction, UV-vis, and electron paramagnetic resonance and investigated in the oxidation reaction of cyclooctene and cyclohexane using iodosylbenzene as oxidant. The iron porphyrin seems to be immobilized at the surface of the glycinate intercalated LDH. The catalytic activities obtained in heterogeneous media for iron porphyrin, Fe(TDFSPP), was superior to the results obtained under homogeneous conditions, but the opposite effect was observed on the Fe(TCFSPP), indicating that, instead of the structural similarity of both iron porphyrins (second-generation porphyrins), the immobilization of each one produced different catalysts. The best catalytic activity of the Fe(TDFSPP)/Gly-LDH, compared to Fe(TCFSPP)/Gly-LDH, can be explained by the easy access of the oxidant and the substrate to the catalytic sites in the former, probably located at the surface of the layered double hydroxide pillared with glycinate anions. A model for the immobilization and a mechanism for the oxidation reaction will be discussed.

Aluminum Hydroxide↗
PubMed2005

Catalytic dehydration of ethanol using transition metal oxide catalysts.

The aim of this work is to study catalytic ethanol dehydration using different prepared catalysts, which include Fe(2)O(3), Mn(2)O(3), and calcined physical mixtures of both ferric and manganese oxides with alumina and/or silica gel. The physicochemical properties of these catalysts were investigated via X-ray powder diffraction (XRD), acidity measurement, and nitrogen adsorption-desorption at -196 degrees C. The catalytic activities of such catalysts were tested through conversion of ethanol at 200-500 degrees C using a catalytic flow system operated under atmospheric pressure. The results obtained indicated that the dehydration reaction on the catalyst relies on surface acidity, whereas the ethylene production selectivity depends on the catalyst chemical constituents.

Journal Article↗
PubMed2005

Paraquat adsorption onto clays and organoclays from aqueous solution.

Clays were compared with organoclays for the sorption of paraquat from aqueous solution. Sepiolite (S), bentonite (B), and illite (I) were used as clay samples. Organoclays were prepared by the modification of the clays with nonyl- and dodecylammonium chlorides, denoted as NS, DS, NB, DB, NI, and DI, respectively. Specific surface area and pore size distribution of the samples were determined by N2 adsorption-desorption at 77 K using the BET method. X-ray powder diffraction analysis of the samples was used to determine the effects of modifying agents on the layer structure of the clays. In the adsorption experiments, C(m) values increased from 0.038 mmol/g for DS to 0.223 mmol/g for NI. Kd0.3 values ranged from 0.177 for DS to 0.843 for NI. The adsorption data indicated that illite and NI are the most effective adsorbents among these clays and organoclay samples, respectively.

Adsorption↗
PubMed2005

Synthesis and characterization of ordered hexagonal and cubic mesoporous tin oxides via mixed-surfactant templates route.

Ordered hexagonal and cubic mesoporous tin oxides were synthesized for the first time in the presence of mixed cationic and neutral surfactants (a mixture of cetyltrimethylammonium bromide cationic surfactant and dodecylamine neutral surfactant) with different alkali and simple inorganic precursors at room temperature. In the synthesis systems, the dodecylamine neutral surfactant may function as a polar organic cosolvent and cosurfactant. The formation of the tin oxide mesostructured material was proposed to be due to the presence of hydrogen-bonding interactions between the supramolecular template and inorganic precursors Sn4+ and OH-, which were assumed to self-assemble around the cationic surfactant molecules. The materials are characterized by X-ray powder diffraction, transmission electron microscopy, thermogravimetric analysis, and N2 adsorption/desorption isotherm. The surface areas of materials evaluated from the N2 sorption isotherms are about 248 m(2)/g for hexagonal mesoporous tin oxide (SnH) and 281 m(2)/g for cubic mesoporous tin oxide (Sn-C) for calcination at 350 degrees C.

Journal Article↗
PubMed2005

AAS, XRPD, SEM/EDS, and FTIR characterization of Zn2+ retention by calcite, calcite-kaolinite, and calcite-clinoptilolite minerals.

In this study, the sorption behavior of Zn2+ on calcite, kaolinite, and clinoptilolite, in addition to mixtures of calcite with kaolinite and clinoptilolite, was investigated at various loadings and mixture compositions using atomic absorption spectroscopy, scanning electron microscopy/energy dispersive X-ray spectroscopy, X-ray powder diffraction, and Fourier transform infrared techniques. According to the obtained results, within the experimental operating conditions, the sorption capacity was enhanced with increasing amount of calcite in both types of mixtures. Under neutral-alkaline pH conditions and high loadings, the order of Zn2+ retention was observed as calcite>clinoptilolite>kaolinite. The experiments on the retention of Zn2+ by pure calcite under conditions of oversaturation showed that the uptake process proceeds via an initial adsorption mechanism (possibly ion-exchange type) followed by a slower mechanism that leads to the overgrowth of the hydrozincite phase, Zn5(OH)6(CO3)2.

Journal Article↗
PubMed2005

Removal of boron from aqueous solution by clays and modified clays.

In order to increase the adsorption capacities of bentonite, sepiolite, and illite for the removal of boron form aqueous solution, the clay samples were modified by nonylammonium chloride. Specific surface areas of the samples were determined as a result of N2 adsorption-desorption at 77 K using the BET method. X-ray powder diffraction analysis of the clays and modified clays was used to determine the effects of modifying agents on the layer structure of the clays. The surface characterization of clays and modified clay samples was conducted using the FTIR technique before and after the boron adsorption. For the optimization of the adsorption of boron on clays and modified clays, the effect of pH and ionic strength was examined. The results indicate that adsorption of boron can be achieved by regulating pH values in the range of 8-10 and high ionic strength. In order to find the adsorption characteristics, Langmuir, Freundlich, and Dubinin-Radushkevich adsorption isotherms were applied to the adsorption data. The data were well described by Freundlich and Dubinin-Radushkevich adsorption isotherms while the fit of Langmuir equation to adsorption data was poor. It was reached that modification of bentonite and illite with nonylammonium chloride increased the adsorption capacity for boron sorption from aqueous solution.

Journal Article↗
PubMed2005

Preparation and characterization of a new layered double hydroxide, Co-Zr-Si.

The layered double hydroxides (LDHs) are nano-ordered layered compounds and well known for their ability to intercalate anionic compounds. Most LDH is prepared conventionally only with divalent and trivalent cations. In this study, Co-Zr-Si LDH, consisting of divalent, tetravalent, and tetravalent cations, was prepared and reacted with monocarboxylic acids at room temperature. The Co-Zr-Si LDH and intercalated compounds have been characterized by energy-dispersive X-ray spectrometry, X-ray powder diffraction, IR spectra, thermal analysis, and scanning electron microscopy (SEM). The insertion of cyanate and carbonate anions into LDH was confirmed by IR spectra. XRD patterns of the prepared Co-Zr-Si LDH showed that the interlayer spacing of the LDH is 0.78 nm. The spacing is similar to that of usual LDH in which chloride, carbonate, or bromide anion is the guest. SEM images showed that Co-Zr-Si LDH can exist as plate-like or fibrous structures.

Journal Article↗
PubMed2006

A simple approach to the synthesis of silver nanowires by hydrothermal process in the presence of gemini surfactant.

Silver nanowires were synthesized by the hydrothermal route in aqueous solution of gemini surfactant 1,3-bis(cetyldimethylammonium) propane dibromide (16-3-16) at a relatively low temperature. The as-prepared silver nanowires were characterized by X-ray photoelectron spectroscopy (XPS), X-ray powder diffraction (XRD), transmission electron microscope (TEM), electron diffraction (ED), and UV-vis absorption spectrum. The obtained silver nanowires are of high aspect ratios with an average diameter of approximately 30 nm and length ranging from several to tens of micrometers.

Journal Article↗
PubMed2006

Arrangement, conformation, and mobility of surfactant molecules intercalated in montmorillonite prepared at different pillaring reagent concentrations as studied by solid-state NMR spectroscopy.

The arrangement, conformation, and mobility of dodecyltrimethylammonium cations (DDTMA+) intercalated in montmorillonite prepared with different pillaring reagent concentrations have been studied by 13C relaxation time measurement, cross-polarization dynamics, and two-dimensional proton wide-line separation (2D WISE) spectroscopy, as well as X-ray powder diffraction (XRD). We demonstrate that the arrangement of DDTMA+ and the mobility of various groups are different, depending on the pillaring concentration, but the conformations of alkyl chains are similar. XRD experiments illustrate that at three different pillaring concentrations (DDmt0.2, DDmt0.5, and DDmt1.0), the organic cations adopt a lateral-monolayer, lateral-monolayer, and pseudotrilayer arrangement, respectively. 13C MAS NMR reveals that the alkyl chains at the three concentrations uniformly display a large amount of mixed trans and gauch conformation (disordered) and a small amount of trans conformation (ordered). 13C spin-lattice relaxation time and 1H-13C cross-polarization dynamics measurement, along with 2D WISE NMR experiments, indicate that the mobility is much different for various groups at a given concentration and for a given group at different concentrations. At each concentration N-methyl unusually possesses the highest mobility, even exceeding that of the terminal methyl; at different concentrations the N-methyl and terminal methyl in DDmt1.0 exhibit the highest mobility compared with the other two samples.

Journal Article↗
PubMed2006

Surfactant-assisted fabrication PbS nanorods, nanobelts, nanovelvet-flowers and dendritic nanostructures at lower temperature in aqueous solution.

PbS nanostructures with different morphologies, such as rod-like, belt-like, downy-velvet-flower-like and dendrite-like, were fabricated successfully under varied reaction conditions in aqueous solution at lower temperature by the assistance of surfactant CTAB. Especially, among all the synthesis methods for PbS nanocrystals, this is the first report using basic acetate of lead, which was formed at initial reaction stage, as a precursor to control the crystal nucleation rate. This synthesis method is a promising one to metal sulfide for its easy control, low-cost and large-scale production. X-ray powder diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), field-emission scanning electron microscopy (FE-SEM) and UV-visible spectrophotometer (UV-vis) were used to characterize the products. A rational mechanism is proposed and three control factors to the crystal directional growth are also concluded.

Journal Article↗
PubMed2006

High chemical reactivity of silver nanoparticles toward hydrochloric acid.

High chemical reactivity of Ag nanoparticles was observed in the reaction with hydrochloric acid: Ag (nanoparticles)+ HCl-->AgCl + H2; the reaction product silver chloride was characterized by X-ray powder diffraction to give a direct evidence for the reaction which has been proved impossible for the bulk Ag.

Journal Article↗
PubMed2006

Dissolution kinetics of nanodispersed gamma-alumina in aqueous solution at different pH: unusual kinetic size effect and formation of a new phase.

The dissolution of a technical, nanodispersed gamma-alumina in water was studied at 25 degrees C in the pH range 3.0 < or = pH < or = 11.0. The obtained kinetic dissolution curves showed a distinct pH dependency, whereas only for pH > or = 4.5 the typical behavior of nanodispersed materials could be observed. X-ray powder diffraction analysis and nitrogen adsorption, as well as IR and UV-Raman spectroscopy, were used to characterize the solid material collected during and at the end of each dissolution experiment. As a result the formation of a new aluminum phase-bayerite-could be proven. The analysis of the equilibrium concentration enabled us to determine the solubility constant of the corresponding phase assuming a pH-dependent species distribution. The rate constants of the dissolution process were evaluated using the model of Gibbs free energy of cluster formation, which considers the size effect, among other things. As a result, we could show that the observed maxima in the concentration profiles are due to a size effect of the starting material having a primary particle radius of 10.1 nm.

Journal Article↗
PubMed2006

One-step incorporation of Pd-Zn catalytic sites into organized mesoporous alumina for use in the oxidative steam reforming of methanol.

In this paper we report the preparation of an organized mesoporous Pd-Zn/alumina system, by a new surfactant-assisted single-step sol-gel synthesis, performed in alcohol, using stearic acid as a chemical template, aluminum sec-butoxide as Al source and metal stearates both as Pd-Zn sources and as structural directing agents. The prepared materials have been characterized using a variety of techniques such as thermogravimetric analysis, atomic absorption spectroscopy, X-ray powder diffraction and N2 adsorption-desorption, and preliminarily tested in the oxidative steam reforming of methanol (OSRM) in the temperature range 100-400 degrees C.

Journal Article↗
PubMed2004

Characterization of steel mill electric-arc furnace dust.

In order to make a complete characterization of electric-arc furnace (EAF) dust, as hazardous industrial waste, and to solve its permanent disposal and/or recovery, bearing in mind both the volumes formed in the Croatian steel industry and experiences of developed industrial countries, a study of its properties was undertaken. For this purpose, samples of EAF dust, taken from the regular production process in the Zeljezara Sisak Steel Mill between December 2000 and December 2001, were subjected to a series of tests. The chemical composition of EAF dust samples was investigated by means of a several different analytical methods. The results from the chemical analysis show that the approximate order of abundance of major elements in EAF dusts is as follows: Fe, Zn, Mn, Ca, Mg, Si, Pb, S, Cr, Cu, Al, C, Ni, Cd, As and Hg. Granular-metric composition of single samples was determined by applying sieve separation. Scanning electron micro-structural examination of EAF dust microstructure was performed and results indicated that all twelve EAF dusts were composed of solid spherical agglomerates with Fe, Zn, Pb, O, Si and Ca as the principal element. The investigation of grain morphology and the mineralogical composition of EAF dust were taken by combination of high resolution Auger electron spectroscopy (HR AES), X-ray photoelectron spectroscopy (XPS) and X-ray powder diffraction analysis. The analysis of XPS-spectra determined the presence of zinc in the form of ZnO phase and the presence of lead in the form of PbO phase, i.e. PbSO3/PbSO4 forms. The results of the X-ray diffraction phase analysis show that the basis of the examined EAF dust samples is made of a mixture of metal oxides, silicates and sulphates. The metal concentration, anions, pH value and conductivity in water eluates was determined in order to define the influence of EAF dust on the environment.

Dust↗
PubMed2004

High temperature removal of hydrogen sulfide using an N-150 sorbent.

In this study, an N-150 sorbent was used as a high temperature desulfurization sorbent for the removal of hydrogen sulfide from coal gas in a fixed bed reactor. The results indicate that the N-150 sorbent could be used for H(2)S removal in the tested temperature ranges. Regeneration test also reveals that utilization of the N-150 sorbent maintains up to 85% compared to the fresh sorbent. No significant degeneration occurs on the N-150 sorbent. In addition, various concentrations of H(2)S, H(2) and CO were also considered in the performance test of the N-150 sorbent. Except for H(2)S, H(2) and CO act the important roles in the high temperature desulfurization. By increasing the H(2) concentration, the sulfur capacity of the sorbent decreases and an adverse result is observed in the case of increasing CO concentration. This can be explained via water-shift reaction. On the basis of the instrument analysis, X-ray powder diffraction determination and SEM images with EDS spectrum characterization, residual sulfur is found in the regenerated N-150 sorbent and this sulfur species is sulfate which resulted by incomplete regeneration. The sulfate formation and sintering effect are major reasons to cause activity loss in the sulfidation/regeneration cycles.

Absorption↗
PubMed2005

Effect of improving flue gas cleaning on characteristics and immobilisation of APC residues from MSW incineration.

The flue gas cleaning system of a MSW incinerator with a capacity of 350 kt/year was changed to improve the HCl elimination efficiency. Instead of the semi-wet operating spray reactor and subsequent baghouse, a two-step wet flue gas cleaning was added behind the baghouse. Elemental composition, X-ray powder diffraction patterns and TGA measurements showed that the resulting APC residue was totally different from the former residue. As a consequence, leaching characteristics of both residues also differed and another treatment was required prior to disposal. For the former residue, mainly leaching of Pb (>100 mg/l), necessitated treatment prior to landfilling. The lower alkalinity of the new residue resulted in a leachate pH of 9.7 and a Pb concentration of 0.8 mg/l. The leachate pH of the former residue was 12.4. The leaching of Pb and Zn increased above 100 mg/l when immobilising the new residue with cement. Better results were obtained when immobilising with micro silica. The high CaCl2 x 2H2O content of the new residue brought along clogging of the bag filter system. Adding 1.4% of CaO (or 1.9% of Ca(OH)2) to the residue already improved these inconveniences but again significantly changed the leaching behaviour of the residue.

Calcium Carbonate↗
PubMed2005

Novel activated alumina-supported iron oxide-composite as a heterogeneous catalyst for photooxidative degradation of reactive black 5.

A novel activated alumina-supported iron oxide-composite (denoted as FeAA-500) was prepared by so-called fluidized-bed reactor (FBR) crystallization. X-ray powder diffraction (XRD), N2 adsorption/desorption, scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) were used to characterize the FeAA-500. The photo-catalytic activity of the FeAA-500 was evaluated in the photooxidative degradation of 0.1 mM azo-dye reactive black 5 (RB5) in the presence of H2O2 and UVA light (lambda = 365 nm) in a solution with a pH of 2.5. Complete decolorization of the model pollutant RB5 was achieved; the total organic carbon (TOC) removal ratio was 95%, and a trace amount of leached ferric ion was detected following 75 min of reaction when 2.0 g/L FeAA-500 was used as a catalyst. FeAA-500 has high photo-catalytic activity; it is therefore a promising heterogeneous photocatalysis of the degradation of organic compounds.

Aluminum Oxide↗