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BET
Terms modified by BET Selected AbstractsCharacterization of biochar from fast pyrolysis and gasification systemsENVIRONMENTAL PROGRESS & SUSTAINABLE ENERGY, Issue 3 2009Catherine E. Brewer Abstract Thermochemical processing of biomass produces a solid product containing char (mostly carbon) and ash. This char can be combusted for heat and power, gasified, activated for adsorption applications, or applied to soils as a soil amendment and carbon sequestration agent. The most advantageous use of a given char depends on its physical and chemical characteristics, although the relationship of char properties to these applications is not well understood. Chars from fast pyrolysis and gasification of switchgrass and corn stover were characterized by proximate analysis, CHNS elemental analysis, Brunauer-Emmet-Teller (BET) surface area, particle density, higher heating value (HHV), scanning electron microscopy, X-ray fluorescence ash content analysis, Fourier transform infrared spectroscopy using a photo-acoustic detector (FTIR-PAS), and quantitative 13C nuclear magnetic resonance spectroscopy (NMR) using direct polarization and magic angle spinning. Chars from the same feedstocks produced under slow pyrolysis conditions, and a commercial hardwood charcoal, were also characterized. Switchgrass and corn stover chars were found to have high ash content (32,55 wt %), much of which was silica. BET surface areas were low (7,50 m2/g) and HHVs ranged from 13 to 21 kJ/kg. The aromaticities from NMR, ranging between 81 and 94%, appeared to increase with reaction time. A pronounced decrease in aromatic CH functionality between slow pyrolysis and gasification chars was observed in NMR and FTIR-PAS spectra. NMR estimates of fused aromatic ring cluster size showed fast and slow pyrolysis chars to be similar (,7,8 rings per cluster), while higher-temperature gasification char was much more condensed (,17 rings per cluster). © 2009 American Institute of Chemical Engineers Environ Prog, 2009 [source] Synthesis of para -Amino Benzoic Acid,TiO2 Hybrid Nanostructures of Controlled Functionality by an Aqueous One-Step ProcessEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 6 2008Raed Rahal Abstract In situ amino acid surface-modified TiO2 nanoparticle syntheses were performed by a simple one-pot hydrolysis of heteroleptic titanium alkoxide [Ti(OiPr)3(O2CC6H4NH2)]m in water with NnBu4Br. This process allowed precise control of the surface grafting rate by varying the amount of precursors and provided highly functionalized nanomaterials. Their compositions and microstructures were determined by C, H and N elemental analyses, TGA-MS, 13C CP-MAS NMR, XRD, TEM, BET, Raleigh diffusion, FTIR, Raman, XPS and UV/Vis experiments. The results indicated that (i) the aggregation rate increased with an increase in the loading of the organic substrate and (ii) the amino acid is chemisorbed as a carboxylate group onto the TiO2 nanoparticles, which leads to a strong interaction between the amino acid and the TiO2 nanoparticle and good stability of these hybrids. Applications of low-aggregated nanomaterials were demonstrated as efficient protection additive against UVA + UVB radiations.(© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2008) [source] Mineral surfaces and soil organic matterEUROPEAN JOURNAL OF SOIL SCIENCE, Issue 2 2003K. Kaiser Summary The organic carbon content of soil is positively related to the specific surface area (SSA), but large amounts of organic matter in soil result in reduced SSA as determined by applying the Brunauer,Emmett,Teller (BET) equation to the adsorption of N2. To elucidate some of the controlling mechanisms of this relation, we determined the SSA and the enthalpy of N2 adsorption of separates with a density > 1.6 g cm,3 from 196 mineral horizons of forest soils before and after removal of organic matter with NaOCl. Likewise, we investigated these characteristics before and after sorption of increasing amounts of organic matter to four mineral soil samples, oxides (amorphous Al(OH)3, gibbsite, ferrihydrite, goethite, haematite), and phyllosilicates (kaolinite, illite). Sorption of organic matter reduced the SSA, depending on the amount sorbed and the type of mineral. The reduction in SSA decreased at larger organic matter loadings. The SSA of the mineral soils was positively related to the content of Fe oxyhydroxides and negatively related to the content of organic C. The strong reduction in SSA at small loadings was due primarily to the decrease in the micropores to which N2 was accessible. This suggests preferential sorption of organic matter at reactive sites in or at the mouths of micropores during the initial sorption and attachment to less reactive sites at increasing loadings. The exponential decrease of the heat of gas adsorption with the surface loading points also to a filling or clogging of micropores at early stages of organic matter accumulation. Desorption induced a small recovery of the total SSA but not of the micropore surface area. Destruction of organic matter increased the SSA of all soil samples. The SSA of the uncovered mineral matrix related strongly to the amounts of Fe oxyhydroxides and the clay. Normalized to C removed, the increase in SSA was small in topsoils and illuvial horizons of Podzols rich in C and large for the subsoils containing little C. This suggests that micropores preferentially associate with organic matter, especially at small loadings. The coverage of the surface of the soil mineral matrix as calculated from the SSA before and after destruction of organic matter was correlated only with depth, and the relation appeared to be linear. We conclude that mineralogy is the primary control of the relation between surface area and sorption of organic matter within same soil compartments (i.e. horizons). But at the scale of complete profiles, the surface accumulation and stabilization of organic matter is additionally determined by its input. [source] Polyaniline Entrapped in Silver: Structural Properties and Electrical ConductivityADVANCED FUNCTIONAL MATERIALS, Issue 8 2009Guy Nesher Abstract By employing the new methodology of entrapment of organic molecules within metals, we demonstrate the ability to modify the conductivity of a metal by suitable polymer entrapment. Specifically, polyaniline (PANI) in two molecular weights was entrapped in silver at different concentrations and a comprehensive comparison was preformed for a range of the composite properties, characterized by XRD, SEM, BET, TGA, and density measurements. Pressed films were utilized to measure the electrical conductivity of the composites in order to study the PANI-silver interactions at the molecular level and to establish a correlation between the microscopic morphology and the film conduction. Such correlations have been identified, and are interpreted. This work extends the functional applications of the new metallic composites and offers insight on the polymer-metal molecular level interactions. [source] Wettability of Bionic Nanopapilla Particles and Their High Electrorheological Activity,ADVANCED FUNCTIONAL MATERIALS, Issue 11 2005X. Wang Abstract Inspired by the nano- and microscale structure of biological surfaces, a kind of nanopapilla particle possessing both nano- and microscale structure has been prepared via a hydrothermal method. The nanopapilla particles have been analyzed using transmission electron microscopy (TEM), scanning electron microscopy (SEM), Brunauer,Emmett,Teller (BET) methods, energy-dispersive spectroscopy (EDS), X-ray diffraction (XRD), etc. The results show that TiO2 nanopapillae are radially distributed on the surface of thin-flake kaolinite. The BET surface area and the wettability of the nanopapilla particles show a marked improvement compared to kaolinite. Moreover, the oleophilic ability of the kaolinite/TiO2 nanopapilla particles spurs a very high electrorheological activity, which is about fifty times that of pure kaolinite. It is suggested that the significant electrorheological improvement can be attributed to the enhanced dielectric properties of the nanopapilla-particle electrorheological fluid. [source] Quantitative evaluation of automated skull-stripping methods applied to contemporary and legacy images: Effects of diagnosis, bias correction, and slice locationHUMAN BRAIN MAPPING, Issue 2 2006Christine Fennema-Notestine Abstract Performance of automated methods to isolate brain from nonbrain tissues in magnetic resonance (MR) structural images may be influenced by MR signal inhomogeneities, type of MR image set, regional anatomy, and age and diagnosis of subjects studied. The present study compared the performance of four methods: Brain Extraction Tool (BET; Smith [2002]: Hum Brain Mapp 17:143,155); 3dIntracranial (Ward [1999] Milwaukee: Biophysics Research Institute, Medical College of Wisconsin; in AFNI); a Hybrid Watershed algorithm (HWA, Segonne et al. [2004] Neuroimage 22:1060,1075; in FreeSurfer); and Brain Surface Extractor (BSE, Sandor and Leahy [1997] IEEE Trans Med Imag 16:41,54; Shattuck et al. [2001] Neuroimage 13:856,876) to manually stripped images. The methods were applied to uncorrected and bias-corrected datasets; Legacy and Contemporary T1 -weighted image sets; and four diagnostic groups (depressed, Alzheimer's, young and elderly control). To provide a criterion for outcome assessment, two experts manually stripped six sagittal sections for each dataset in locations where brain and nonbrain tissue are difficult to distinguish. Methods were compared on Jaccard similarity coefficients, Hausdorff distances, and an Expectation-Maximization algorithm. Methods tended to perform better on contemporary datasets; bias correction did not significantly improve method performance. Mesial sections were most difficult for all methods. Although AD image sets were most difficult to strip, HWA and BSE were more robust across diagnostic groups compared with 3dIntracranial and BET. With respect to specificity, BSE tended to perform best across all groups, whereas HWA was more sensitive than other methods. The results of this study may direct users towards a method appropriate to their T1 -weighted datasets and improve the efficiency of processing for large, multisite neuroimaging studies. Hum. Brain Mapping, 2005. © 2005 Wiley-Liss, Inc. [source] Moisture sorption characteristics of curd (Indian yogurt) powderINTERNATIONAL JOURNAL OF DAIRY TECHNOLOGY, Issue 1 2009SHIBY VARGHESE K. The moisture sorption behaviour of curd (Indian yogurt) powder was studied at 20, 30, 40 and 50°C for water activity ranging from 0.07 to 0.85. GAB, BET, Henderson, Halsey, Chung & Pfost, Smith, Oswin and Peleg models were applied to analyse the data. Estimated parameters and fitting ability for sorption models were evaluated. The GAB model showed the best fit to the sorption data of curd powder at 20, 30 and 40°C, and the Peleg model fitted well at 50°C. [source] Mathematical modelling of moisture sorption isotherms and determination of isosteric heat of blueberry variety O,NeilINTERNATIONAL JOURNAL OF FOOD SCIENCE & TECHNOLOGY, Issue 10 2009Antonio Vega-Gálvez Summary The sorption isotherms of blueberry variety O'Neil were determined at 20, 40 and 60 °C, for a range of water activity of 0.10,0.95. The isotherms showed that the equilibrium moisture content increased when temperature decreased at constant water activity. The BET, GAB, Halsey, Henderson, Caurie, Smith, Oswin and Iglesias-Chirife equations were tested for modelling the sorption isotherms. The results showed that GAB, BET and Halsey models gave the best fit quality for the experimental desorption data, and BET, Oswin and Henderson for adsorption data as suggested by the statistical tests employed. The net sorption heat was calculated using the Clausius,Clapeyron equation giving 38.62 kJ mol,1 (desorption) and 30.88 kJ mol,1 (adsorption) at a moisture content of 0.01 g water (g d.m.,1). Tsami equation was applied to estimate the net isosteric heat of sorption as function of equilibrium moisture content with satisfactory results. [source] Moisture sorption isotherms and thermodynamic properties of apple Fuji and garlicINTERNATIONAL JOURNAL OF FOOD SCIENCE & TECHNOLOGY, Issue 10 2008Mariana A. Moraes Summary The moisture equilibrium isotherms of garlic and apple were determined at 50, 60 and 70 °C using the gravimetric static method. The experimental data were analysed using GAB, BET, Henderson,Thompson and Oswin equations. The isosteric heat and the differential entropy of desorption were determined by applying Clausius,Clapeyron and Gibbs,Helmholtz equations, respectively. The GAB equation showed the best fitting to the experimental data (R2 > 99% and E% < 10%). The monolayer moisture content values for apple were higher than those for garlic at the studied temperatures; the values varied from 0.050 to 0.056 and from 0.107 to 0.168 for garlic and apple, respectively. The isosteric heat and the differential entropy of desorption were estimated in function of the moisture content. The values of these thermodynamic properties were higher for apple (in range 48,100 kJ mol,1 and 14,150 J mol,1 K,1) than for garlic (in range 43,68 kJ mol,1 and 0,66 J mol,1 K,1). The water surface area values decreased with increasing temperature. The Kelvin and the Halsey equations were used to calculate the pore size distribution. [source] Effect of temperature and initial moisture content on sorption isotherms of banana dried by tunnel drierINTERNATIONAL JOURNAL OF FOOD SCIENCE & TECHNOLOGY, Issue 8 2008Zhengyong Yan Summary Sorption isotherms of intermediate moisture content (IMC) products are essential to predict shelf-life of packaged moisture-sensitive product by modelling moisture uptake during storage and distribution. The effect of temperature and initial moisture content (MC) of IMC banana on the relationship between MC and water activity were investigated. Raw bananas were dried in a tunnel dryer at 2% relative humidity (RH), 70 °C, and a 3.2 ± 0.2 m s,1 air velocity. Drying procedure was carried out a number of times until various IMC levels were obtained (5%, 14%, 22% and 33% db for banana). Sorption isotherms of bananas were determined at 10, 20, 30 and 40 °C. The initial MC of IMC banana had no significant effect on the relationship between MC and water activity according to statistical analysis. All the sorption curves were found to be Type II. BET, GAB, modified GAB, Oswin, Halsey and modified Freundlich models were fitted to the data and it was found that the best results were obtained with a modified Freundlich equation. A secondary modified Freundlich model was built accounting for the effect of aw and temperature on the sample MC. [source] Hybrid Inorganic-Organic Materials Carrying Tertiary Amine and Thiourea Residues Tethered on Mesoporous Silica Nanoparticles: Synthesis, Characterization, and Co-Operative CatalysisADVANCED SYNTHESIS & CATALYSIS (PREVIOUSLY: JOURNAL FUER PRAKTISCHE CHEMIE), Issue 1-2 2009Alessandra Puglisi Abstract Mesoporous silica nanoparticles carrying different loadings of tertiary amine and thiourea residues (residues ratios 53/47, 68/32, and 22/78, respectively) were synthesized by the co-condensation method and fully characterized by CP MAS NMR, powder XRD, SEM, BET, BJH and FT-IR techniques. These materials were tested as bifunctional catalysts in the conjugate addition of acetylacetone to 2-nitrostyrene, a reaction that under solvent-free conditions occurred in quantitative yield. By carrying out several experiments with the bifunctional catalysts featuring different molar ratios of active sites, and with different combinations of monofunctional supported and non-supported catalyst, the co-operativity of the tertiary amine and thiourea residues in catalyzing the reaction was demonstrated. The use of the bifunctional catalyst was extended to the addition of acetylacetone to an activated imine. Catalyst recycling for a total of three reaction cycles was demonstrated without significant erosion of activity. [source] The microencapsulation of terbinafine via in situ polymerization of melamine-formaldehyde and their application to cotton fabricJOURNAL OF APPLIED POLYMER SCIENCE, Issue 6 2010Gökhan Erkan Abstract In this study an antifungal pharmaceutical agent, terbinafine, was microencapsulated by using in situ polymerization. The polymerization was carried out at four mole ratio level and preparations were applied to the 100% cotton fabric. X-ray diffractometry, DSC, FTIR, BET, contact angle measurements, particle size distribution and imaging techniques were performed. Best results were obtained in the case of 8 : 1 mole ratio. Strength of microcapsule applied fabrics to washing and fungus were also determined. After 25 washing cycle, microcapsules were still in the fabric and had antifungal properties against A. niger. Antifungal strength against T. rubrum was observed up to 15 washing cycles. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010 [source] Microporous activated carbon spheres prepared from resole-type crosslinked phenolic beads by physical activationJOURNAL OF APPLIED POLYMER SCIENCE, Issue 5 2008Arjun Singh Abstract Microporous activated carbon spheres (ACSs) with a high specific Brunauer,Emmet,Teller (BET) surface area were prepared from resole-type spherical crosslinked phenolic beads (PBs) by physical activation. The PBs used as precursors were synthesized in our laboratory through the mixing of phenol and formaldehyde in the presence of an alkaline medium by suspension polymerization. The effects of the gasification time, temperature, and flow rate of the gasifying agent on the surface properties of ACSs were investigated. ACSs with a controllable pore structure derived from carbonized PBs were prepared by CO2 gasification. Surface properties of ACSs, such as the BET surface area, pore volume, pore size distribution, and pore diameters, were characterized with BET and Dubinin,Reduchkevich equations based on N2 adsorption isotherms at 77 K. The results showed that ACSs with a 32,88% extent of burn-off with CO2 gasification exhibited a BET surface area ranging from 574 to 3101 m2/g, with the pore volume significantly increased from 0.29 to 2.08 cm3/g. The pore size and its distribution could be tailored by the selection of suitable conditions, including the gasification time, temperature, and flow rate of the gasifying agents. The experimental results of this analysis revealed that ACSs obtained under different conditions were mainly microporous. The development of the surface morphology of ACSs was also studied with scanning electron microscopy. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008 [source] The effect of water on particle size, porosity and the rate of drug release from implanted titania reservoirsJOURNAL OF BIOMEDICAL MATERIALS RESEARCH, Issue 2 2010Tessy Lopez Abstract The implantation of controlled drug release devices represents a new strategy in the treatment of neurodegenerative disorders. Sol,gel titania implants filled with valproic acid, have been used for this purpose to treat induced epilepsy in rats. The kinetics of the drug release depend on: (a) porosity, (b) chemical interactions between valproic acid and surface hydroxyl groups of titania, (c) particle size, and (d) particle size agglomerates. The concentration of water used in the hydrolysis reaction is an important variable in the degree of porosity, hydroxylation, and structural defects of the nanostructured titanium oxide reservoir. The titanium n -butoxide/water ratio was systematically varied during the sol,gel synthesis, while maintaining the amount of valproic acid constant. Characterization studies were performed using DTA-TGA, FTIR, Raman, TEM, SEM, BET, and in vitro release kinetic measurements. The particle agglomerate size and porosity were found to depend on the amount of water used in the sol,gel reaction. © 2010 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 2010 [source] Best Estimated Aroma and Taste Detection Threshold for Guaiacol in Water and Apple JuiceJOURNAL OF FOOD SCIENCE, Issue 4 2005Thomas A. Eisele ABSTRACT: Alicyclobacillus acidoterrestris can produce sufficient guaiacol (methoxyphenol), a metabolic by-product of the bacterium, in apple juice to cause a detectable taint characterized by an antiseptic off-odor or distinct medicinal flavor and lingering aftertaste. Bacterial spoilage may not be visibly detectable. The objective of this study was to determine the best estimate threshold (BET) for detection of guaiacol in water and commercial pasteurized apple juice from concentrate using the forced-choice ascending concentration method of limits with an experienced 17-member sensory panel. The mean BET for aroma detection of guaiacol in water and apple juice was 0.48 ppb and 0.91 ppb, respectively. The mean BET for taste detection of guaiacol in water and apple juice was 0.17 ppb and 0.24 ppb, respectively. Individual aroma BET values ranged from 0.06 ppb to 4.71 ppb guaiacol in water and 0.17 ppb to 4.71 ppb for guaiacol in apple juice. Individual taste BET values ranged from 0.01 ppb to 4.71 ppb for guaiacol in water and apple juice. The taste BET was equal to or lower than the aroma BET for guaiacol in both water and apple juice for all panelists. There was about a 500-fold range in guaiacol taste detection between panelists, with some individuals exhibiting a BET value as low as 10 ppt (trillion). The information should be useful for developing quality assurance sensory methodology to evaluate potential apple juice flavor spoilage by Alicyclobacillus spp. [source] Synthesis, structure, and selective separation behavior of copper-imprinted microporous polymethacrylate beadsAICHE JOURNAL, Issue 12 2009Nguyen To Hoai Abstract Metal ion-imprinted polymethacrylate beads with sizes ranging from 100 to 300 ,m were prepared by suspension polymerization for the application of selective separation of target metal ions. The metal ion contacting area of the beads was enlarged via pore formation (BET 425 m2/g) using toluene as a porogenic agent. The synthesis of the copper-imprinted porous beads was verified using FTIR, SEM, and ESCA. Separation capacity and selectivity were investigated carrying out column separation experiments. The selective adsorption behavior of the imprinted beads was significantly affected by flow rate, pH, and metal ion concentration in the solution. Adsorption of the copper ion, the template metal ion, onto the beads was highly selective, compared with other ions such as nickel and zinc, with the selective coefficients at approximately 5,10. The microporous particles possessing such high selectivity has a potential application as novel column packing materials especially requiring high selective efficiency, which is usually not achievable by commercial ion exchange resins. © 2009 American Institute of Chemical Engineers AIChE J, 2009 [source] Transesterification of dimethyl oxalate with phenol over TiO2/SiO2: Catalyst screening and reaction optimizationAICHE JOURNAL, Issue 12 2008Xia Yang Abstract Physicochemical properties of silica-supported titanium oxide catalysts as well as their performances for transesterification of dimethyl oxalate (DMO) with phenol to methyl phenyl oxalate (MPO) and diphenyl oxalate (DPO) have been investigated systematically. Various wt % of TiO2 were loaded on SiO2 by a two-step wet impregnation method. The surface properties of TiO2/SiO2 catalysts were explored by various characterization techniques (BET, SEM, ICP, XPS, XRD, FTIR of pyridine adsorption, and NH3 -TPD). Catalytic performances of TiO2/SiO2 catalysts were found to be strongly dependent on TiO2 dispersion and surface acidity. Monolayer dispersion capacity of TiO2 on silica was estimated to be about 4.0 TiO2 molecules per nm2 (SiO2) and no crystalline TiO2 was detected at TiO2 loading less than 12 wt %. FTIR and TPD analysis suggested that weak Lewis acid sites on the surface of TiO2/SiO2 were responsible for their unique selectivity to the target products, MPO and DPO. An optimization of reaction conditions for the transesterification of DMO with phenol was performed over 12 wt % TiO2/SiO2 calcined at 550°C. In addition, we studied the disproportionation reaction from MPO to DPO via a catalytic distillation process, which is highly efficient to promote formation of the desired DPO. © 2008 American Institute of Chemical Engineers AIChE J, 2008 [source] Monolithic poly(1,2-bis(p -vinylphenyl)ethane) capillary columns for simultaneous separation of low- and high-molecular-weight compoundsJOURNAL OF SEPARATION SCIENCE, JSS, Issue 15-16 2009Andreas Greiderer Abstract Monolithic poly(1,2-bis(p -vinylphenyl)ethane (BVPE)) capillary columns were prepared by thermally initiated free radical polymerisation of 1,2-bis(p -vinylphenyl)ethane in the presence of inert diluents (porogens) and ,,,,-azoisobutyronitrile (AIBN) as initiator. Polymerisations were accomplished in 200 ,m ID fused silica capillaries at 65°C and for 60 min. Mercury intrusion porosimetry measurements of the polymeric RP support showed a broad bimodal pore-size-distribution of mesopores and small macropores in the range of 5,400 nm and flow-channels in the ,m range. N2 -adsorption (BET) analysis resulted in a tremendous enhancement of surface area (101 m2/g) of BVPE stationary phases compared to typical organic monoliths (,20 m2/g), indicating the presence of a considerable amount of mesopores. Consequently, the adequate proportion of both meso- and (small) macropores allowed the rapid and high-resolution separation of low-molecular-weight compounds as well as biomolecules on the same monolithic support. At the same time, the high fraction of flow-channels provided enhanced column permeability. The chromatographic performance of poly(1,2-bis(p -vinylphenyl)ethane) capillary columns for the separation of biomolecules (proteins, oligonucleotides) and small molecules (alkyl benzenes, phenols, phenons) are demonstrated in this article. Additionally, pressure drop versus flow rate measurements of novel poly(1,2-bis(p -vinylphenyl)ethane) capillary columns confirmed high mechanical robustness, low swelling in organic solvents and high permeability. Due to the simplicity of monolith fabrication, comprehensive studies of the retention and separation behaviour of monolithic BVPE columns resulted in high run-to-run and batch-to-batch reproducibilities. All these attributes prove the excellent applicability of monolithic poly(1,2-bis(p -vinylphenyl)ethane) capillary columns for ,-HPLC towards a huge range of analytes of different chemistries and molecular sizes. [source] Preparation, Characterization, and Photocatalytic Properties of CaNb2O6 NanoparticlesJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 2 2009In-Sun Cho CaNb2O6 nanoparticles with a size range of 30,50 nm were synthesized by heat treatment at 600°C after a solvothermal process and their optical and photocatalytic properties were investigated. The prepared powders were characterized by X-ray powder diffractometer, field-emission scanning electron microscope, transmission electron microscope, UV-Vis diffuse reflectance spectroscopy, Fluorescence spectroscopy, and Raman spectroscopy. Compared with a powder of the same material prepared by a solid-state reaction (SS) method, the nanoparticles exhibited a higher Brunauer,Emmett,Teller (BET) surface area, more efficient light absorption, and enhanced photocatalytic activity for producing H2 from pure water under UV irradiation. The photoluminescence spectra revealed that a radiative recombination process is dominant in the powder prepared by the SS method (strong blue emission at 300 K) under UV light irradiation, while no obvious emission was observed in the nanoparticles. This decrease of the radiative recombination as well as the higher optical absorption ability and higher BET surface area resulting from the reduced dimensionality led to enhanced photocatalytic activity of the nanoparticles. [source] Surface Enthalpy, Enthalpy of Water Adsorption, and Phase Stability in Nanocrystalline Monoclinic ZirconiaJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 1 2009A. V. Radha A fundamental issue that remains to be solved when approaching the nanoscale is how the size induces transformation among different polymorphic structures. Understanding the size-induced transformation among the different polymorphic structures is essential for widespread use of nanostructured materials in technological applications. Herein, we report water adsorption and high-temperature solution calorimetry experiments on a set of samples of single-phase monoclinic zirconia with different surface areas. Essential to the success of the study has been the use of a new ternary water-in-oil/water liquid solvothermal method that allows the preparation of monoclinic zirconia nanoparticles with a broad range of (BET) Brunauer,Emmett,Teller surface area values. Thus, the surface enthalpy for anhydrous monoclinic zirconia is reported for the first time, while that for the hydrous surface is a significant improvement over the previously reported value. Combining these data with previously published surface enthalpy for nanocrystalline tetragonal zirconia, we have calculated the stability crossovers between monoclinic and tetragonal phases to take place at a particle size of 28 ± 6 nm for hydrous zirconia and 34 ± 5 nm for anhydrous zirconia. Below these particle sizes, tetragonal hydrous and anhydrous phases of zirconia become thermodynamically stable. These results are within the margin of the theoretical estimation and confirm the importance of the presence of water vapor on the transformation of nanostructured materials. [source] Investigation of the Structural Characterization of Mesoporous Molecular Sieves MCM-41 from SepioliteJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 3 2007Shengming Jin Mesoporous molecular sieves, MCM-41, were synthesized from sepiolite using acid leaching, followed by hydrothermal reconstruction and then calcinations at 540°C for 5 h. The structures and the porosity of MCM-41 were investigated by means of small-angle X-ray diffraction patterns, Brunaer-Emmett-Teller (BET), 29Si MAS NMR, Fourier transform infrared (FTIR), and high resolution transmission electron microscope (HRTEM) methods. The results showed that the hexagonal MCM-41 was formed in an alkaline solution of pH 12, when crystallization was carried out at 100°C for 24 h. The specific surface area, pore diameter, and pore volumes of MCM-41 from sepiolite were 1036 m2/g, 2.98 nm, and 1.06 cm3/g, respectively. 29Si MAS NMR results revealed that amorphous silica decomposed into Si,O chains consisting of two layers of Si atoms, with Q3 configurations resulting in an increase in the fraction of Q3 configuration during the crystallization of post-Mg-extraction sepiolite. The IR results illustrated that the complex of ,,SiO,,CTA+ was formed during the synthesis of MCM-41 from post-Mg-extraction sepiolite. [source] Synthesis and Characterization of Mixed-Metal Oxide Nanopowders Along the CoOx,Al2O3 Tie Line Using Liquid-Feed Flame Spray PyrolysisJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 9 2006Jose Azurdia We report here the use of liquid-feed flame spray pyrolysis (LF-FSP) to produce a series of nanopowders along the CoOx,Al2O3 tie line. The process is a general aerosol combustion synthesis route to a wide range of lightly agglomerated oxide nanopowders. The materials reported here were produced by aerosolizing ethanol solutions of alumatrane [Al(OCH2CH2)3N] and a cobalt precursor, made by reacting Co(NO3)2·6H2O crystals with propionic acid. The compositions of the as-produced nanopowders were controlled by selecting the appropriate ratios of the precursors. Nine samples with compositions (CoO)y(Al2O3)1,y, y=0,1 along the CoOx,Al2O3 tie line were prepared and studied. The resulting nanopowders were characterized by X-ray fluorescence, BET, scanning electron microscopy, high-resolution transmission electron micrographs, X-ray diffraction (XRD), thermogravimetric analysis (TGA), and FTIR. The powders typically consist of single-crystal particles <40 nm diameter and specific surface areas (SSAs) of 20,60 m2/g. XRD studies show a gradual change in powder patterns from ,-Al2O3 to Co3O4. The cobalt aluminate spinel phase is observed at stoichiometries (21 and 37 mol%) not seen in published phase diagrams, likely because LF-FSP processing involves a quench of >1000°C in microseconds frequently leading to kinetic rather than thermodynamic products. Likewise, the appearance of Co3O4 rather than CoO as the end member in the tie line is thought to be a consequence of the process conditions. TGA studies combined with diffuse reflectance FTIR spectroscopic studies indicate that both physi- and chemi-sorbed H2O are the principal surface species present in the as-processed nanopowders. The only sample that differs is Co3O4, which has some carbonate species present that are detected and confirmed by a sharp mass loss event at ,250°C. The thermal behavior of the high cobalt content samples differs greatly from the low cobalt content samples. The latter behave like most LF-FSP-derived nanopowders exhibiting typical 1%,4% mass losses over the 1400°C range due mostly to loss of water and some CO2. The high cobalt content samples exhibit a sharp mass loss event that can be attributed to the decomposition of Co3O4 to CoO. [source] Physicochemical properties and application of pullulan edible films and coatings in fruit preservationJOURNAL OF THE SCIENCE OF FOOD AND AGRICULTURE, Issue 10 2001Tony Diab Abstract The effects of water, sorbitol and a sucrose fatty acid ester (SE) on the water sorption behaviour and thermal and mechanical properties of pullulan-based edible films as well as the physiological responses of fruit coated with pullulan have been studied. Incorporation of sorbitol or SE in pullulan films resulted in lower equilibrium moisture contents at low to intermediate water activities (aw), but much higher moisture contents at aw,>,0.75; estimates of monolayer values (within 4.1,5.9,gH2O,kg,1 solids) were given by application of the Brunauer,Emmett,Teller (BET) and Guggenheim,Anderson,DeBoer (GAB) models. A single glass,rubber transition (Tg), attributed to the polysaccharide component, was detected by calorimetry and dynamic mechanical thermal analysis (DMTA) at a sorbitol level of 15,30% DM. With both tests the strong plasticising action of water and polyol was evident in the thermal curves, and the Tg vs moisture content data were successfully fitted to the Gordon,Taylor empirical model. Multifrequency DMTA measurements provided estimates for the apparent activation energy of the glass transition in the range of , 300,488,kJ,mol,1. With large-deformation mechanical testing, large decreases in Young's moduli (tensile and three-point bend tests) were observed as a result of water- and/or polyol-mediated glass-to-rubber transition of the polymeric films. In the moisture content range of 2,8%, increases in flexural modulus (E) and maximum stress (,max) with small increases in moisture content were found for films made of pullulan or pullulan mixed with 15% DM sorbitol; a strong softening effect was observed when the water content exceeded this range. Addition of sorbitol increased the water vapour transmission rate of the films, whereas addition of SE had the opposite effect. Application of a pullulan/sorbitol/SE coating on strawberries resulted in large changes in internal fruit atmosphere composition which were beneficial for extending the shelf-life of this fruit; the coated fruit showed much higher levels of CO2, a large reduction in internal O2, better firmness and colour retention and a reduced rate of weight loss. In contrast, similar studies on whole kiwifruits showed increased levels of internal ethylene, which caused acceleration of fruit ripening during storage. © 2001 Society of Chemical Industry [source] Surface Functionalization of Silica with 2-Vinylfuran by Cationic PolymerizationMACROMOLECULAR CHEMISTRY AND PHYSICS, Issue 5-6 2003Susanne Höhne Abstract Cationic surface polymerization of 2-vinylfuran with chlorotriphenylmethane as initiator has been used for the functionalization of silica particles. The influence of monomer/initiator ratio and temperature on grafting efficiency, yield, and degree of grafting has been investigated. Grafting efficiency is a significant function of temperature and monomer/initiator ratio, because crosslinking reactions between cationically active chains increases the amount of the immobilized polyvinylfuran fraction. Thus, larger initiator concentrations on the silica cause higher polymer content on the surface. Polymer structure elucidation and surface properties are analyzed by means of solid-state NMR spectroscopy, UV-vis spectroscopy, BET , measurements, and scanning electron microscopy. [source] Physical adsorption vs. chemical binding of undecylenic acid on porous silicon surface: a comparative study of differently functionalized materialsPHYSICA STATUS SOLIDI (C) - CURRENT TOPICS IN SOLID STATE PHYSICS, Issue 7 2009E. Pastor Abstract To imply miscibility to porous silicon (PSi) used for biomedical purposes a number of functionalization methods are employed. In order to distinguish between a non-specific surfactant-like interaction (physical sorption) and chemical binding of unsaturated chemicals (undecylenic acid, UD) to H-terminated PSi surface we studied the two differently treated materials. Differential scanning calorimetry (DSC) and thermogravimetry (TGA), BET and FTIR measurements were performed with the PSi powder samples (n+ doped). Changes in surface area, weight loss, calorific effect and chemical composition that accompanied the thermal treatment have shown that the physisorbed UD molecules undergo a chemical process (binding) with the Si-Hx surface groups at about 150 °C in both, N2 inert atmosphere and in a synthetic air, oxidative atmosphere. Controlled conversion of physically sorbed molecules to the chemically attached ones is discussed with respect to methods of surface modification of PSi materials for increasing their biocompatibility. (© 2009 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] The preparation of MnZn-ferrite nanoparticles in a water/CTAB, 1-butanol/1-hexanol reverse microemulsionPHYSICA STATUS SOLIDI (C) - CURRENT TOPICS IN SOLID STATE PHYSICS, Issue 12 2004Abstract Manganese zinc ferrite nanoparticles were prepared using a precipitation in reverse microemulsion system consisting of hexadecyltrimethyl ammonium bromide (CTAB) as a surfactant, 1-butanol as a co-surfactant, 1-hexanol as an oil phase and an aqueous solution of metal sulfates. Tetramethyl ammonium hydroxide (TMAH) served as the precipitating agent. The influence of the microemulsion's composition on the nature of the spinel product was studied. The synthesized nanoparticles were characterized using transmission electron microscopy (TEM), X-ray diffractometry (XRD), specific surface area (BET) and magnetometry. (© 2004 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] The Effect of Preparation Procedures on the Morphology of Melanin from the Ink Sac of Sepia officinalisPIGMENT CELL & MELANOMA RESEARCH, Issue 1 2003Yan Liu The structure of melanin extracted from the ink sac of the cuttlefish Sepia officinalis was examined for different methods of isolation and purification of the pigment. Scanning electron microscopy (SEM) images of Sepia eumelanin prepared by different procedures establish that multi-,m-sized aggregates reported by previous workers are generated by their sample preparation, and that the dominant constituents of Sepia melanin are ,150 nm spherical granules. Brunauer-Emmett-Teller (BET) measurements reveal that Sepia eumelanin from Sigma (prepared by spray drying the pigment) has a surface area of 14.3 m2/g. Pigment extracted directly from the fresh ink sac and then freeze-dried has a surface area of 21.5 m2/g, while CO2 -supercritically dried has a surface area of 37.5 m2/g. This is consistent with SEM images showing that the process of freeze-drying produces aggregates, but to a lesser extent than spray drying. Supercritical drying of the sample produces suspensions of the individual ,150 nm granule, which is more reflective of the natural pigment. Brunauer-Emmett-Teller surface area analysis and Barrett-Joyner-Halenda (BJH) pore volume analysis indicate that the surface of the granules is not smooth and the interior of the granules is not porous, but rather the aggregates of granules are porous. Ultra-high resolution SEM and atomic force microscopy (AFM) images show the granules are easily deformed and are comprised of smaller constituents. De-aggregation of the granules by sonication and ultra-filtration reveal a range of structures depending on the pore size of the membrane used. The implications of these results on quantifying photochemical properties and kinetic reaction rate constants of melanin are discussed. [source] A novel continuous reactor for catalytic reduction of NOx,fixed bed simulationsTHE CANADIAN JOURNAL OF CHEMICAL ENGINEERING, Issue 3 2008Terris T. Yang Abstract A novel dual-zone fluidized bed reactor was proposed for the continuous adsorption and reduction of NOx from combustion flue gases. The adsorption and reaction behaviour of such a reactor has been simulated in a fixed bed reactor using Fe/ZSM-5 catalyst and propylene reductant with model flue gases. Fe/ZSM-5 exhibited acceptable activity at T,=,350°C and GHSV,=,5000 h,1 when O2 concentration was controlled at levels lower than 1% with a HC to NO molar ratio of about 2:1. XPS and BET surface area measurement revealed the nature of the deactivation of the catalyst. Those performance data demonstrated the feasibility of a continuous dual-zone fluidized bed reactor for catalytic reduction of NOx under lean operating conditions. Un nouveau réacteur à lit fluidisé à double zone est proposé pour l'adsorption et la réduction en continu de NOx à partir de gaz de carneau de combustion. Le comportement d'adsorption et de réaction d'un tel réacteur a été simulé dans un réacteur à lit fixe utilisant un catalyseur Fe/ZSM-5 et un agent réducteur avec des gaz de carneau modèle. Le Fe/ZSM-5 montre une activité acceptable à T,=,350°C et GHSV,=,5000 h,1 lorsque la concentration d'O2 est contrôlée à des niveaux inférieurs à 1% avec un rapport molaire HC,NO d'environ 2:1. La mesure de surface par XPS et BET a permis de caractériser la désactivation du catalyseur. Ces données de performance illustre la faisabilité du réacteur à lit fluidisé à double zone Fe/ZSM-5 pour la réduction catalytique de NOx dans des conditions opératoires pauvres. [source] Effect of Catalysis on Plasma Assisted Catalytic Removal of Nitrogen Oxides and SootCHEMICAL ENGINEERING & TECHNOLOGY (CET), Issue 10 2006X. Peng Abstract An active perovskite-type catalyst (La0.8K0.2Cu0.05Mn0.95O3) was prepared and characterized using XRD, BET, and SEM. Then, the effect of catalysis on plasma assisted catalytic removal of nitrogen oxides and soot was investigated by combining temperature programmed reaction (TPR) and the analysis of Fourier transform infrared spectroscopy (FT-IR). When the C3H6 concentration in the feed gas is 0.27,%, the maximum NOx removal rate increases from 43.5,% to 72.2,% after adding catalyst. FT-IR results indicate that the addition of catalyst will promote the removal of NOx, HC, and soot. There is still great amount of NOx and HC remaining after plasma reaction, little NOx and almost no HC after catalytic reaction, and no NOx and HC after plasma assisted catalytic reaction. [source] In-Situ Preparation of Polymer-Coated Alumina Nanopowders by Chemical Vapor SynthesisCHEMICAL VAPOR DEPOSITION, Issue 1 2003M. Schallehn Abstract Nanocrystalline alumina particles coated with polyethylene have been prepared by a two-step chemical vapor synthesis (CVS) process using a hot-wall reactor to synthesize the nanocrystalline alumina core, and a RF plasma reactor for the subsequent polymer coating. The particle radius is about 4,nm, with the radius of the ceramic core being about 2.5,nm and the coating thickness about 1.5,nm. The powders have been characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), Brunauer,Emmett,Teller (BET), small-angle neutron scattering (SANS), and high-resolution transmission electron microscopy (HRTEM). [source] | |||||||||||||||||||||||||||||||||||||||||||||||||