Synthesis and structural evaluation of freeze-cast porous alumina

Energy Technology Data Exchange (ETDEWEB)

Souza, Douglas F., E-mail: souzadf@outlook.com [Department of Metallurgical and Materials Engineering, Federal University of Minas Gerais — UFMG, Avenida Presidente Antônio Carlos, 6627, Campus UFMG, Belo Horizonte, MG CEP: 31270-901, Escola de Engenharia, bloco 2, sala 2230 (Brazil); Nunes, Eduardo H.M., E-mail: eduardohmn@gmail.com [Department of Metallurgical and Materials Engineering, Federal University of Minas Gerais — UFMG, Avenida Presidente Antônio Carlos, 6627, Campus UFMG, Belo Horizonte, MG CEP: 31270-901, Escola de Engenharia, bloco 2, sala 2230 (Brazil); Pimenta, Daiana S.; Vasconcelos, Daniela C.L. [Department of Metallurgical and Materials Engineering, Federal University of Minas Gerais — UFMG, Avenida Presidente Antônio Carlos, 6627, Campus UFMG, Belo Horizonte, MG CEP: 31270-901, Escola de Engenharia, bloco 2, sala 2230 (Brazil); Nascimento, Jailton F.; Grava, Wilson [Petrobras/CENPES, Avenida Horácio Macedo 950, Cidade Universitária, Ilha do Fundão, Rio de Janeiro, RJ CEP:21941-915 (Brazil); Houmard, Manuel [Department of Materials Engineering and Civil Construction, Federal University of Minas Gerais — UFMG, Avenida Presidente Antônio Carlos, 6627, Campus UFMG, Belo Horizonte, MG CEP: 31270-901, Escola de Engenharia, bloco 1, sala 3304 (Brazil); Vasconcelos, Wander L., E-mail: wlv@demet.ufmg.br [Department of Metallurgical and Materials Engineering, Federal University of Minas Gerais — UFMG, Avenida Presidente Antônio Carlos, 6627, Campus UFMG, Belo Horizonte, MG CEP: 31270-901, Escola de Engenharia, bloco 2, sala 2230 (Brazil)

2014-10-15

In this work we fabricated alumina samples by the freeze-casting technique using tert-butanol as the solvent. The prepared materials were examined by scanning electron microscopy and X-ray microtomography. Next, they were coated with sol–gel silica films by dip-coating. Permeability tests were carried out in order to assess the permeation behavior of the materials processed in this study. We observed that the sintering time and alumina loading showed a remarkable effect on both the structural properties and flexural strength of the freeze-cast samples. Nitrogen adsorption tests revealed that the silica prepared in this study exhibited a microporous structure. It was observed that the presence of silica coatings on the alumina surface decreased the CO{sub 2} permeance by about one order of magnitude. Because of the similar kinetic diameters of nitrogen and carbon dioxide, the CO{sub 2}/N{sub 2} system showed a separation efficiency that was lower than that observed for the He/CO{sub 2} and He/N{sub 2} systems. We noticed that increasing the feed pressure improved the separation capacity of the obtained materials. - Highlights: • Porous alumina samples obtained by the freeze-casting technique • Microporous silica coating prepared by a simple sol–gel dip-coating methodology • Samples examined by SEM, μ-CT, and nitrogen sorption tests • Mechanical tests were carried out in the freeze-cast samples. • The presence of silica coatings on the alumina surface decreased the CO{sub 2} permeance.

Ceramic protective coatings applied by sol-gel or electrophoresis

International Nuclear Information System (INIS)

Stoch, A.

1993-01-01

Sol-gel and electrophoresis are the complementary techniques which may be used for obtaining the ceramic coatings. The composition of such a coatings depends on the composition of electrophoresis bath or sol solution. Thermal treatment is used for densifying the coating and promoting the adherence of coating to the substrate. In presented work silica, silica-alumina or alumina coatings are applied by sol-gel dip coating procedure on steel, aluminium or ceramic substrates. Electrophoresis is employed for obtaining zirconia, alumina or hydroxyapatite coatings on stainless steel. (author). 7 refs

Pecan drying with silica gel

Energy Technology Data Exchange (ETDEWEB)

Ghate, S.R.; Chhinnan, M.S.

1983-07-01

High moisture in-shell pecans were dried by keeping them in direct and indirect contact with silica gel to investigate their drying characteristics. In-shell pecans were also dried with ambient air from a controlled environment chamber and with air dehumidified by silica gel. Direct contact and dehumidified air drying seemed feasible approaches.

Environmentally stable adsorbent of tetrahedral silica and non-tetrahedral alumina for removal and recovery of malachite green dye from aqueous solution

International Nuclear Information System (INIS)

Kannan, Chellapandian; Sundaram, Thiravium; Palvannan, Thayumanavan

2008-01-01

The conventional adsorbents like activated carbon, agricultural wastes, molecular sieves, etc., used for dye adsorption are unstable in the environment for long time, and hence the adsorbed dyes again gets liberated and pollute the environment. To avoid this problem, environmentally stable adsorbent of silica and alumina should be employed for malachite green adsorption. The adsorbents were characterized by Fourier transformed infrared spectroscopy (FT-IR) to confirm the tetrahedral framework of silica and non-tetrahedral framework of alumina. The adsorption equilibrium of dye on alumina and silica were 4 and 5 h, respectively, this less adsorption time on alumina might be due to the less activation energy on alumina (63.46 kJ mol -1 ) than silica (69.93 kJ mol -1 ). Adsorption increased with increase of temperature on silica, in alumina, adsorption increased up to 60 deg. C, and further increase of temperature decreased the adsorption due to the structural change of non-tetrahedral alumina in water. The optimum pH for dye adsorption on alumina was 5 and silica was 6. The dye adsorptions on both adsorbents followed pseudo-second-order kinetics. The adsorption well matched with Langmuir and Freundlich adsorption isotherms and found that adsorption capacity on alumina was more than silica. The thermodynamic studies proved that the adsorption was endothermic and chemisorptions (ΔH o > 40 kJ mol -1 ) on alumina and silica. Recovery of dye on alumina and silica were studied from 30 to 90 deg. C and observed that 52% of dye was recovered from alumina and only 3.5% from silica. The less recovery on silica proved the strong adsorption of dye on silica than alumina

Environmentally stable adsorbent of tetrahedral silica and non-tetrahedral alumina for removal and recovery of malachite green dye from aqueous solution

Energy Technology Data Exchange (ETDEWEB)

Kannan, Chellapandian [Department of Chemistry, Periyar University, Salem 636011, Tamilnadu (India)], E-mail: chellapandiankannan@gmail.com; Sundaram, Thiravium [Department of Chemistry, Periyar University, Salem 636011, Tamilnadu (India); Palvannan, Thayumanavan [Department of Biochemistry, Periyar University, Salem 636011, Tamilnadu (India)

2008-08-30

The conventional adsorbents like activated carbon, agricultural wastes, molecular sieves, etc., used for dye adsorption are unstable in the environment for long time, and hence the adsorbed dyes again gets liberated and pollute the environment. To avoid this problem, environmentally stable adsorbent of silica and alumina should be employed for malachite green adsorption. The adsorbents were characterized by Fourier transformed infrared spectroscopy (FT-IR) to confirm the tetrahedral framework of silica and non-tetrahedral framework of alumina. The adsorption equilibrium of dye on alumina and silica were 4 and 5 h, respectively, this less adsorption time on alumina might be due to the less activation energy on alumina (63.46 kJ mol{sup -1}) than silica (69.93 kJ mol{sup -1}). Adsorption increased with increase of temperature on silica, in alumina, adsorption increased up to 60 deg. C, and further increase of temperature decreased the adsorption due to the structural change of non-tetrahedral alumina in water. The optimum pH for dye adsorption on alumina was 5 and silica was 6. The dye adsorptions on both adsorbents followed pseudo-second-order kinetics. The adsorption well matched with Langmuir and Freundlich adsorption isotherms and found that adsorption capacity on alumina was more than silica. The thermodynamic studies proved that the adsorption was endothermic and chemisorptions ({delta}H{sup o} > 40 kJ mol{sup -1}) on alumina and silica. Recovery of dye on alumina and silica were studied from 30 to 90 deg. C and observed that 52% of dye was recovered from alumina and only 3.5% from silica. The less recovery on silica proved the strong adsorption of dye on silica than alumina.

Silica scintillating materials prepared by sol-gel methods

International Nuclear Information System (INIS)

Werst, D.W.; Sauer, M.C. Jr.; Cromack, K.R.; Lin, Y.; Tartakovsky, E.A.; Trifunac, A.D.

1993-01-01

Silica was investigated as a rad-hard alternative to organic polymer hosts for organic scintillators. Silica sol-gels were prepared by hydrolysis of tetramethoxysilane in alcohol solutions. organic dyes were incorporated into the gels by dissolving in methanol at the sol stage of gel formation. The silica sol-gel matrix is very rad-hard. The radiation stability of silica scintillators prepared by this method is dye-limited. Transient radioluminescence was measured following excitation with 30 ps pulses of 20 MeV electrons

Silica reinforced triblock copolymer gels

DEFF Research Database (Denmark)

Theunissen, E.; Overbergh, N.; Reynaers, H.

2004-01-01

The effect of silica and polymer coated silica particles as reinforcing agents on the structural and mechanical properties of polystyrene-poly(ethylene/butylene)-polystyrene (PS-PEB-PS) triblock gel has been investigated. Different types of chemically modified silica have been compared in order...

Effect of support on hydro-metathesis of propene: A comparative study of W(CH 3 ) 6 anchored to silica vs. silica-alumina

KAUST Repository

Tretiakov, Mykyta

2018-03-27

Hydro-metathesis of propene was carried out by using well-defined W(CH3)6 supported on silica and silica-alumina. It was observed that W(CH3)6 supported silica-alumina catalyst is much better (TON 4577) than the silica supported catalyst (TON 2104). We demonstrated that the present catalysts are much better than the previously reported (tantalum hydride/KCC-1, TON 786) catalyst. For the first time, we observed the formation of n-decane from propene, which enables us to think of using cheaper raw materials and converting them to petroleum range alkanes using hydro-metathesis reaction.

Characterization of alumina suspensions by electroacoustics

Energy Technology Data Exchange (ETDEWEB)

Galassi, C.; Roncari, E.; Greenwood, R.; Piancastelli, A. [CNR, Faenza (Italy). Research Inst. for Ceramics Technology

1997-12-31

Using the acoustophoresis technique three different dispersants were selected to investigate the effect of the volume fraction of the suspension on the minimum amount of dispersant required to give the maximum zeta potential. No effect was detected over a volume fraction range 0.11 to 0.35. The acoustosizer was used to screen many dispersants for alumina in a relatively short time. From the viewpoint that the most stable suspensions are those with the greatest zeta potentials, then the following dispersants can be recommended: Reotan LA (0.25 mg/m{sup 2}) Dolapix CA (0.20 mg/m{sup 2}) and Dolapix PC33 (0.30 mg/m{sup 2}). Vanisperse and Borresperse are poor. Polyacrylic acid and polymethacrylic acid were better than some commercially available products. (orig.) 2 refs.

Mesoporous silica materials modified with alumina polycations as catalysts for the synthesis of dimethyl ether from methanol

Energy Technology Data Exchange (ETDEWEB)

Macina, Daniel; Piwowarska, Zofia; Tarach, Karolina; Góra-Marek, Kinga [Jagiellonian University, Faculty of Chemistry, Ingardena 3, 30-060 Kraków (Poland); Ryczkowski, Janusz [Maria Curie Skłodowska University, Faculty of Chemistry, Maria Curie-Skłodowska 2, 20-031 Lublin (Poland); Chmielarz, Lucjan, E-mail: chmielar@chemia.uj.edu.pl [Jagiellonian University, Faculty of Chemistry, Ingardena 3, 30-060 Kraków (Poland)

2016-02-15

Highlights: • Deposition of alumina ologoctaions on mesoporous silicas modified with surface −SO{sub 3}H groups. • Alumina aggregates generated acid properties in the silica supports. • Alumina modified SBA-15 and MCF were active and selective catalysts in DME synthesis. - Abstract: Mesoporous silica materials (SBA-15 and MCF) were used as catalytic supports for the deposition of aggregated alumina species using the method consisting of the following steps: (i) anchoring 3-(mercaptopropyl)trimethoxysilane (MPTMS) on the silica surface followed by (ii) oxidation of −SH to−SO{sub 3}H groups and then (iii) deposition of aluminum Keggin oligocations by ion-exchange method and (iv) calcination. The obtained samples were tested as catalysts for synthesis of dimethyl ether from methanol. The modified silicas were characterized with respect to the ordering of their porous structure (XRD), textural properties (BET), chemical composition (EDS, CHNS), structure ({sup 27}Al NMR, FTIR) and location of alumina species (EDX-TEM), surface acidity (NH{sub 3}-TPD, Py-FTIR) and thermal stability (TGA). The obtained materials were found to be active and selective catalysts for methanol dehydration to dimethyl ether (DME) in the MTD process (methanol-to-dimethyl ether).

Silica promoted self-assembled mesoporous aluminas. Impact of the silica precursor on the structural, textural and acidic properties

NARCIS (Netherlands)

Perez, Lidia Lopez; Zarubina, Valeriya; Mayoral, Alvaro; Melian-Cabrera, Ignacio

2015-01-01

This paper investigates the effect of silica addition on the structural, textural and acidic properties of an evaporation induced self-assembled (EISA) mesoporous alumina. Two silica addition protocols were applied while maintaining the EISA synthesis route. The first route is based on the addition

Radiation effect on polystyrene deposited and grafted on silica gel

International Nuclear Information System (INIS)

Kusama, Y.; Udagawa, A.; Takehisa, M.

1978-01-01

The effect of radiation on polystyrene was studied in the presence and absence of silica gel by molecular weight measurement with gel permeation chromatography (GPC). Polystyrene crosslinked under vacuum in the absence of silica gel, but it either crosslinked or degraded by radiation, depending on the molecular weight of the polymer in the presence of silica gel. part of the deposited polymer bonded to silica gel by radiation; the G value for graft-chain formation is in the range of 0.01 to 0.1. Irradiation of polystyrene grafted on silica gel resulted in degradation of the graft chain because of the transfer of energy from silica gel. The G value for main chain scission was about 2 when graft polymer was irradiated in the absence of homopolymer. The degradation of graft polymer was suppressed when the polymer was irradiated in the presence of homopolymer, and the amount of unextractable polymer from silica gel increased with increasing irradiation. This adds evidence to the estimation that an increase in grafting percent coupled with a slight decrease in molecular weight at a later stage of radiation-induced polymerization of styrene adsorbed on slica gel is due to a secondary effect of radiation on the polymer

Synthesis and characterization of mesoporous ceria/alumina nanocomposite materials via mixing of the corresponding ceria and alumina gel precursors.

Science.gov (United States)

Khalil, Kamal M S

2007-03-01

Mesoporous ceria/alumina, CeO(2)/Al(2)O(3), composites containing 10, 20 and 30% (w/w) ceria were prepared by a novel gel mixing method. In the method, ceria gel (formed via hydrolysis of ammonium cerium(IV) nitrate by aqueous ammonium carbonate solution) and alumina gel (formed via controlled hydrolysis of aluminum tri-isopropoxide) were mixed together. The mixed gel was subjected to subsequent drying and calcination for 3 h at 400, 600, 800 and 1000 degrees C. The uncalcined (dried at 110 degrees C) and the calcined composites were investigated by different techniques including TGA, DSC, FTIR, XRD, SEM and nitrogen adsorption/desorption isotherms. Results indicated that composites calcined for 3 h at 800 degrees C mainly kept amorphous alumina structure and gamma-alumina formed only upon calcinations at 1000 degrees C. On the other hand, CeO(2) was found to crystallize in the common ceria, cerinite, phase and it kept this structure over the entire calcination range (400-1000 degrees C). Therefore, high surface areas, stable surface textures, and non-aggregated nano-sized ceria dispersions were obtained. A systematic texture change based on ceria ratio was observed, however in all cases mesoporous composite materials exposing thermally stable texture and structure were obtained. The presented method produces composite ceria/alumina materials that suit different applications in the field of catalysis and membranes technology, and throw some light on physicochemical factors that determine textural morphology and thermal stability of such important composite.

The Effect of Various Acids to the Gelation Process to the Silica Gel Characteristic Using Organic Silica

Science.gov (United States)

Rahman, NA; Widiyastuti, W.; Sigit, D.; Ajiza, M.; Sujana, W.

2018-01-01

Bagasse ash is solid waste of cane sugar industry which contain of silica more than 51%. Some previous study of silica gel from bagasse ash have been conducted often and been applied. This study concerns about the effect of various acid used in the process of gelation to the characteristic of silica gel produced. Then, this silica gel will be used as adsorbent. As that, the silica gel must fulfill the requirements of adsorbent, as have good pores characteristics, fit in mesoporous size so that adsorbent diffusion process is not disturbed. A fitted pores size of silica gel can be prepared by managing acid concentration used. The effect of acid, organic acid (tartaric acid) and inorganic acid (hydrochloric acid), is investigated in detail. The acid is added into sodium silicate solution in that the gel is formed, the pores structures can be investigated with BET, the crystal form is analyzed with XRD and the pore structure is analyzed visually with SEM. By managing the acid concentration added, it gets the effect of acid to the pore structure of silica gel. The bigger concentration is, the bigger the pore’s size of silica gel produced.

Silica gel matrix immobilized Chlorophyta hydrodictyon africanum ...

African Journals Online (AJOL)

Chlorophyta hydrodictyon africanum was immobilized on a silica gel matrix to improve its mechanical properties. The algae-silica gel adsorbent was used for batch sorption studies of a cationic dye, methylene blue (MB). Optimum adsorption was obtained with a dosage of 0.8 g bio sorbent. Results from sorption studies ...

Radiation hardening in sol-gel derived Er3+-doped silica glasses

International Nuclear Information System (INIS)

Hari Babu, B.; León Pichel, Mónica; Ollier, Nadège; El Hamzaoui, Hicham; Bigot, Laurent; Savelii, Inna; Bouazaoui, Mohamed; Poumellec, Bertrand; Lancry, Matthieu; Ibarra, Angel

2015-01-01

The aim of the present paper is to report the effect of radiation on the Er 3+ -doped sol-gel silica glasses. A possible application of these sol-gel glasses could be their use in harsh radiation environments. The sol-gel glasses are fabricated by densification of erbium salt-soaked nanoporous silica xerogels through polymeric sol-gel technique. The radiation-induced attenuation of Er 3+ -doped sol-gel silica is found to increase with erbium content. Electron paramagnetic resonance studies reveal the presence of E′ δ point defects. This happens in the sol-gel aluminum-silica glass after an exposure to γ-rays (kGy) and in sol-gel silica glass after an exposure to electrons (MGy). The concentration levels of these point defects are much lower in γ-ray irradiated sol-gel silica glasses. When the samples are co-doped with Al, the exposure to γ-ray radiation causes a possible reduction of the erbium valence from Er 3+ to Er 2+ ions. This process occurs in association with the formation of aluminum oxygen hole centers and different intrinsic point defects

Peptide bond formation of alanine on silica and alumina surfaces as a catalyst

Science.gov (United States)

Sánchez Arenillas, M.; Mateo-Martí, E.

2012-09-01

Polymerization of amino acids has been important for the origin of life because the peptides may have been the first self-replicating systems. The amino acid concentrations in the oceans may have been too diluted in the early phases of the Earth. The formation of the biopolymers could have been due to the catalytic action of various minerals (such as silica or alumina). Our work is based on the comparison between alumina and silica minerals with and without prior activation of their silanol groups for the formation of peptide bonds using alanina like amino acid which it is the simplest quiral amino acid.

Hydrothermal Diamond Anvil Cell Investigations Into the Alumina-Silica-Water System up to 1073 K and 4 GPa

Science.gov (United States)

Davis, M. K.; Stixrude, L. P.

2004-12-01

Understanding fluid chemistry in the subduction zone environment is key to unraveling the details of element transport from the slab to the surface. Solubility of different mineral assemblages in predominantly water-rich fluid along with pressure and temperature conditions control the chemical structure of the aqueous fluid and govern the transport opportunities for various chemical components away from the subducting slab. In-situ Raman experiments were performed in the alumina-silica-water system in an externally heated Bassett-type hydrothermal diamond anvil cell in the Department of Geological Sciences at the University of Michigan. Natural quartz samples (from the Owl Creek Mountains, Wyoming) were used as the silica source and synthetic ruby was used for the alumina source. Temperatures inside the diamond cell were monitored using type-K thermocouples wrapped around the diamonds and the pressure calibrated by the Raman shift of diamond or quartz or the fluorescence of ruby depending on conditions. Raman measurements of the aluminosilicate fluid show the presence of multiple alumina, silica, and mixed species. As predicted by calculations an aluminosilicate specie possibly of the form (HO)3SiOAl(OH)32- as well as the silica monomer and dimer specie were observed in the aluminosilicate fluid. There also appeared to be at least one hydrous alumina specie based on the presence of a Raman peaks at 228 cm-1, 339 cm-1 and 970 cm-1 in the fluid and a comparative analysis between Raman peaks in aqueous fluid in the silica-water, alumina-water, and alumina-silica-water systems. Solid phases formed during experiments (diaspore, kyanite) were confirmed with Raman spectroscopy.

Study of silica sol-gel materials for sensor development

Science.gov (United States)

Lei, Qiong

Silica sol-gel is a transparent, highly porous silicon oxide glass made at room temperature by sol-gel process. The name of silica sol-gel comes from the observable physical phase transition from liquid sol to solid gel during its preparation. Silica sol-gel is chemically inert, thermally stable, and photostable, it can be fabricated into different desired shapes during or after gelation, and its porous structure allows encapsulation of guest molecules either before or after gelation while still retaining their functions and sensitivities to surrounding environments. All those distinctive features make silica sol-gel ideal for sensor development. Study of guest-host interactions in silica sol-gel is important for silica-based sensor development, because it helps to tailor local environments inside sol-gel matrix so that higher guest loading, longer shelf-life, higher sensitivity and faster response of silica gel based sensors could be achieved. We focused on pore surface modification of two different types of silica sol-gel by post-grafting method, and construction of stable silica hydrogel-like thin films for sensor development. By monitoring the mobility and photostability of rhodamine 6G (R6G) molecules in silica alcogel thin films through single molecule spectroscopy (SMS), the guest-host interactions altered by post-synthesis grafting were examined. While physical confinement remains the major factor that controls mobility in modified alcogels, both R6G mobility and photostability register discernable changes after surface charges are respectively reversed and neutralized by aminopropyltriethoxysilane (APTS) and methyltriethoxysilane (MTES) grafting. The change in R6G photostability was found to be more sensitive to surface grafting than that of mobility. In addition, silica film modification by 0.4% APTS is as efficient as that by pure MTES in lowering R6G photostability, which suggests that surface charge reversal is more effective than charge neutralization

Glass properties in the yttria-alumina-silica system

Science.gov (United States)

Hyatt, M. J.; Day, D. E.

1987-01-01

The glass formation region in the yttria-alumina-silica system was investigated. Properties of glasses containing 25 to 55 wt pct yttria were measured and the effect of the composition was determined. The density, refractive index, thermal-expansion coefficient, and microhardness increased with increasing yttria content. The dissolution rate in 1N HCl increased with increasing yttria content and temperature. These glasses were also found to have high electrical resistivity.

Catalytic fast pyrolysis of durian rind using silica-alumina catalyst: Effects of pyrolysis parameters.

Science.gov (United States)

Tan, Y L; Abdullah, A Z; Hameed, B H

2018-05-18

Silica-alumina catalyst was prepared and used in the catalytic fast pyrolysis of durian rind in a drop-type two-stage reactor. The effects of catalytic temperature (400 °C-600 °C) and catalyst-to-durian rind ratio (1:30-3:30) were evaluated. Bio-oil yield was increased with increased catalytic temperature due to considerable dehydration process, but it was reduced with high catalyst loading due to the overcracking of organics into light gases. Silica-alumina catalyst possessed good selectivity and the products changed according to the temperature. The major components in bio-oil were hydrocarbons, furan derivatives, and aromatic compounds at 400 °C, 500 °C, and 600 °C, respectively. The hydrogen and carbon contents of bio-oil were reduced with high catalyst loading due to the overcracking of organics, and the deoxygenation process became unfavorable. The silica-alumina catalyst worked well in catalytic fast pyrolysis of durian rind, and the condition may be adjusted based on the desired products. Copyright © 2018 Elsevier Ltd. All rights reserved.

Extraction of gelatin from catfish bone using NaOH and its utilization as a template on mesoporous silica alumina

Science.gov (United States)

Nuryanto, R.; Trisunaryanti, W.; Falah, I. I.; Triyono

2018-04-01

Gelatin extraction from catfish bone using NaOH and its utilization as a template on a synthesis of mesoporous silica-alumina had been investigated. The extraction was prepared by immersing 25 g catfish bone in 125 mL of NaOH in concentration of 0.0; 0.05; 0.10; 0.15 and 0.20 M for 24 h, then washing with demineralized water until pH 7, followed by immersed the bone into 125 mL of 1 M HCl for 1 h, then washed using demineralized water into pH 5. To produce gelatin the bone was refluxed with 100 mL demineralized water at 70°C for 5 h then evaporated at 50°C. The dry gelatin was characterized using FTIR and electrophoresis (SDS-PAGE). The best performance of gelatin was produced by NaOH 0.10 M. The gelatin consists of amide A, B, I, II, III and molecular weight of 25-200kDa. Silica and Alumina material prepared from Lapindo mud extraction. Dry Lapindo mud crushed and filtered until pass 100 mesh, then reflux using 6 M HCl (1:4 w/V) at 90°C for 5h then filtered. The filtrate was consisting alumina solution adding with 6 M NaOH (2/3 V/V) them filtered. The filtrate then injected by CO2 gas for 30 minutes and filtered, the residue was calcined at 500°C for 5h. The residual of Lapindo mud dried and refluxed with 6 M NaOH (1:4 w/v) at 90 °C. After 5h filtered and the filtrate added by HCl to pH 8 and filtered, the residual then dried. The Si and Al were then analyzed by XRF and consist of silica and alumina for 99.1 and 87.73%, respectively. Silica-alumina was prepared using silica and alumina extracted from Lapindo mud. 6 g of SiO2 and 2 g of NaOH was immersed in 62 mL of demineralized water then added with alumina solution (0.204 g alumina in 30 mL demineralized water). The gelatin solution (5 g gelatin in 70 mL demineralized water) was dropped into the silica-alumina while stirring at 50°C for 4 h and aging for 24 h. The synthesized silica alumina was analysed using FTIR and surface area analyser. The FT-IR spectra indicated the TO4 (T=Si, Al) vibration at wave

Fractal dimensions of silica gels generated using reactive molecular dynamics simulations

International Nuclear Information System (INIS)

Bhattacharya, Sudin; Kieffer, John

2005-01-01

We have used molecular dynamics simulations based on a three-body potential with charge transfer to generate nanoporous silica aerogels. Care was taken to reproduce the sol-gel condensation reaction that forms the gel backbone as realistically as possible and to thereby produce credible gel structures. The self-similarity of aerogel structures was investigated by evaluating their fractal dimension from geometric correlations. For comparison, we have also generated porous silica glasses by rupturing dense silica and computed their fractal dimension. The fractal dimension of the porous silica structures was found to be process dependent. Finally, we have determined that the effect of supercritical drying on the fractal nature of condensed silica gels is not appreciable

A review on chemical methodologies for preparation of mesoporous silica and alumina based materials.

Science.gov (United States)

Naik, Bhanudas; Ghosh, Narendra Nath

2009-01-01

The discovery of novel family of molecular sieves called M41S aroused a worldwide resurgence in the field of porous materials. According to IUPAC definition inorganic solids that contain pores with diameter in the size range of 20-500 A are considered mesoporous materials. Mesoporous silica and alumina based materials find applications in catalysis, adsorption, host- guest encapsulation etc. This article reviews the current state of art and outline the recent patents in mesoporous materials research in three general areas: Synthesis, various mechanisms involved for porous structure formation and applications of silica and alumina based mesoporous materials.

Study on the bound water of several high specific surface-area oxides (beryllia, alumina, silica-alumina)

International Nuclear Information System (INIS)

Rouquerol, J.

1964-11-01

This study is concerned with the bound water of several oxides (beryllia, alumina, silica-alumina) at different steps of their dehydration (heating temperatures between 150 and 1100 deg. C). The following techniques have been used simultaneously: Thermal analysis (a new method has been developed), nitrogen adsorption (study of the texture), Diborane hydrolysis (qualitative and quantitative analysis of surface water), Infra-red spectrography (in the absorption range of water), Nuclear magnetic resonance (in the resonance range of protons). Thanks to these different techniques, five kinds of bound water have been observed. Attention is called on the great influence of the thermal treatment conditions on the evolution of the products resulting from the decomposition of alumina α-trihydrate Al(OH) 3 and beryllium α-hydroxide, in the course of the dehydration. Moreover, the author emphasizes the peculiar properties of the two kinds of oxides (alumina and beryllia) prepared through a new method of treatment under low pressure and constant speed of decomposition. Such particular features concern mainly texture, bound water, and consequently, also catalytic activity. (author) [fr

The Influence of Microgravity on Silica Sol-Gel Formation

Science.gov (United States)

Sibille, L.; Smith, D. D.; Cronise, R.; Hunt, A. J.; Wolfe, D. B.; Snow, L. A.; Oldenberg, S.; Halas, N.; Rose, M. Franklin (Technical Monitor)

2000-01-01

We discuss space-flight experiments involving the growth of silica particles and gels. The effect of microgravity on the growth of silica particles via the sol-gel route is profound. In four different recipes spanning a large range of the parameter space that typically produces silica nanoparticles in unit-gravity, low-density gel structures were instead formed in microgravity. The particles that did form were generally smaller and more polydisperse than those grown on the ground. These observations suggest that microgravity reduces the particle growth rate, allowing unincorporated species to form aggregates and ultimately gel. Hence microgravity favors the formation of more rarefied structures, providing a bias towards diffusion-limited cluster-cluster aggregation. These results further suggest that in unit gravity, fluid flows and sedimentation can significantly perturb sol-gel substructures prior to gelation and these deleterious perturbations may be "frozen" into the resulting microstructure. Hence, sol-gel pores may be expected to be smaller, more uniform, and less rough when formed in microgravity.

Exploring encapsulation mechanism of DNA and mononucleotides in sol-gel derived silica.

Science.gov (United States)

Kapusuz, Derya; Durucan, Caner

2017-07-01

The encapsulation mechanism of DNA in sol-gel derived silica has been explored in order to elucidate the effect of DNA conformation on encapsulation and to identify the nature of chemical/physical interaction of DNA with silica during and after sol-gel transition. In this respect, double stranded DNA and dAMP (2'-deoxyadenosine 5'-monophosphate) were encapsulated in silica using an alkoxide-based sol-gel route. Biomolecule-encapsulating gels have been characterized using UV-Vis, 29 Si NMR, FTIR spectroscopy and gas adsorption (BET) to investigate chemical interactions of biomolecules with the porous silica network and to examine the extent of sol-gel reactions upon encapsulation. Ethidium bromide intercalation and leach out tests showed that helix conformation of DNA was preserved after encapsulation. For both biomolecules, high water-to-alkoxide ratio promoted water-producing condensation and prevented alcoholic denaturation. NMR and FTIR analyses confirmed high hydraulic reactivity (water adsorption) for more silanol groups-containing DNA and dAMP encapsulated gels than plain silica gel. No chemical binding/interaction occurred between biomolecules and silica network. DNA and dAMP encapsulated silica gelled faster than plain silica due to basic nature of DNA or dAMP containing buffer solutions. DNA was not released from silica gels to aqueous environment up to 9 days. The chemical association between DNA/dAMP and silica host was through phosphate groups and molecular water attached to silanols, acting as a barrier around biomolecules. The helix morphology was found not to be essential for such interaction. BET analyses showed that interconnected, inkbottle-shaped mesoporous silica network was condensed around DNA and dAMP molecules.

Kinetics Study of Gas Pollutant Adsorption and Thermal Desorption on Silica Gel

Directory of Open Access Journals (Sweden)

Rong A

2017-06-01

Full Text Available Silica gel is a typical porous desiccant material. Its adsorption performance for gaseous air pollutants was investigated to determine its potential contribution to reducing such pollutants. Three gaseous air pollutants, toluene, carbon dioxide, and methane, were investigated in this paper. A thermogravimetric analyzer was used to obtain the equilibrium adsorption capacity of gases on single silica gel particles. The silica gel adsorption capacity for toluene is much higher than that for carbon dioxide and methane. To understand gas pollutant thermal desorption from silica gel, the thermogravimetric analysis of toluene desorption was conducted with 609 ppm toluene vapor at 313 K, 323 K, and 333 K. The overall regeneration rate of silica gel was strongly dependent on temperature and the enthalpy of desorption. The gas pollutant adsorption performance and thermal desorption on silica gel material may be used to estimate the operating and design parameters for gas pollutant adsorption by desiccant wheels.

All-silica nanofluidic devices for DNA-analysis fabricated by imprint of sol-gel silica with silicon stamp

DEFF Research Database (Denmark)

Mikkelsen, Morten Bo Lindholm; Letailleur, Alban A; Søndergård, Elin

2011-01-01

We present a simple and cheap method for fabrication of silica nanofluidic devices for single-molecule studies. By imprinting sol-gel materials with a multi-level stamp comprising micro- and nanofeatures, channels of different depth are produced in a single process step. Calcination of the imprin......We present a simple and cheap method for fabrication of silica nanofluidic devices for single-molecule studies. By imprinting sol-gel materials with a multi-level stamp comprising micro- and nanofeatures, channels of different depth are produced in a single process step. Calcination...... of the imprinted hybrid sol-gel material produces purely inorganic silica, which has very low autofluorescence and can be fusion bonded to a glass lid. Compared to top-down processing of fused silica or silicon substrates, imprint of sol-gel silica enables fabrication of high-quality nanofluidic devices without...

Effect of Al content on the gas-phase dehydration of glycerol over silica-alumina-supported silicotungstic acid catalysts

International Nuclear Information System (INIS)

Kim, Yong Tae; You, Su Jin; Park, Eun Duck; Jung, Kwangdeog

2012-01-01

The gas-phase dehydration of glycerol to acrolein was carried out over silicotungstic acid (H 4 SiW 12 O 40 ·xH 2 O, HSiW) catalysts supported on SiO 2 , η-Al 2 O 3 , and silica-alumina with different Al contents. The HSiW catalysts supported on silica-alumina showed higher glycerol conversions and acrolein yields during the initial 2 h at 315.deg.C than did SiO 2 - and η-Al 2 O 3 -supported HSiW catalysts. Among the tested catalysts, HSiW/Si 0.9 Al 0.1Ox exhibited the highest space-time yield during the initial 2 h. The loaded HSiW species can change the acid types and suppress the formation of carbonaceous species on Al-rich silica-alumina. The deactivated HSiW supported on silica-alumina can be fully regenerated after calcination in air at 500.deg.C. As long as the molar ratio between water and glycerol was in the range of 2-11, the acrolein selectivity increased significantly with increasing water content in the feed, while the surface carbon content decreased owing to the suppression of heavy compounds

Thermo-physical properties of silica gel for adsorption desalination cycle

KAUST Repository

Thu, Kyaw; Chakraborty, Anutosh; Saha, Bidyut Baran; Ng, Kim Choon

2013-01-01

Thermo-physical properties, surface characteristics and water vapor uptake capacity are key parameters in the selection of adsorbent for an adsorption desalination (AD) cycle. In the AD cycles, silica gel is used as adsorbent due to their high water vapor uptake capacity, reliability, repeatability and inexpensiveness as compared to other adsorbents. Three types of commercially available silica gels (Type-RD 2560,Type-A5BW and Type-A++) are investigated using a surface characteristic analyzer and their thermo-physical properties are evaluated using several analysis methods. The instrument used in this investigation employs the static volumetric method with liquid Nitrogen at 77 K as the filing fluid. The surface area of each adsorbent is studied using Brunauer-Emmett-Teller (BET) method whilst the pore size distribution (PSD) analysis is conducted with the Non-Local Density Functional Theory (NLDFT). It is observed that the Type-A++ silica gel (granular type) possesses the highest surface area of 863.6 m2/g amongst the three parent silica gels studied. It has a two-maxima or bimodal distribution pattern where the pore diameters are distributed mostly between 10 Å and 30 Å. Water vapor uptake capacity of silica gels are studied with water vapor dosage apparatus and the results show that the Type-A++ silica gel exhibits a highest equilibrium uptake at 537 cm3/g. These thermo-physical properties are essential for the design and the numerical simulation of AD cycles. © 2012 Published by Elsevier Ltd.

Thermo-physical properties of silica gel for adsorption desalination cycle

KAUST Repository

Thu, Kyaw

2013-02-01

Thermo-physical properties, surface characteristics and water vapor uptake capacity are key parameters in the selection of adsorbent for an adsorption desalination (AD) cycle. In the AD cycles, silica gel is used as adsorbent due to their high water vapor uptake capacity, reliability, repeatability and inexpensiveness as compared to other adsorbents. Three types of commercially available silica gels (Type-RD 2560,Type-A5BW and Type-A++) are investigated using a surface characteristic analyzer and their thermo-physical properties are evaluated using several analysis methods. The instrument used in this investigation employs the static volumetric method with liquid Nitrogen at 77 K as the filing fluid. The surface area of each adsorbent is studied using Brunauer-Emmett-Teller (BET) method whilst the pore size distribution (PSD) analysis is conducted with the Non-Local Density Functional Theory (NLDFT). It is observed that the Type-A++ silica gel (granular type) possesses the highest surface area of 863.6 m2/g amongst the three parent silica gels studied. It has a two-maxima or bimodal distribution pattern where the pore diameters are distributed mostly between 10 Å and 30 Å. Water vapor uptake capacity of silica gels are studied with water vapor dosage apparatus and the results show that the Type-A++ silica gel exhibits a highest equilibrium uptake at 537 cm3/g. These thermo-physical properties are essential for the design and the numerical simulation of AD cycles. © 2012 Published by Elsevier Ltd.

On the role of acidity in amorphous silica-alumina based catalysts

NARCIS (Netherlands)

Poduval, D.G.

2011-01-01

Amorphous silica-alumina (ASA) is widely used as a solid acid catalyst or as a carrier for well-dispersed metal sulfide or metal catalysts. They are often involved in hydrocracking catalyst formulations, especially so when the aim is to produce middle distillates from heavy oil fractions. With

ADSORPSI ION SIANIDA DALAM LARUTAN MENGGUNAKAN ADSORBEN HIBRIDA AMINOPROPIL SILIKA GEL DARI SEKAM PADI TERIMPREGNASI ALUMINIUM (Adsorption of Cyanide Ions in Solution Using a Hybrid Adsorbent Aminopropyl Silica Gel from Rice Husks of Impregnated With

Directory of Open Access Journals (Sweden)

Amaria Amaria

2012-03-01

aminopropil silica gel from rice husk that has been impregnated with aluminum (APSG-Al and silica gel impregnated with aluminum (SG-Al of rice husk silica gel as the material for the adsorption of cyanide ions in solution. The interaction between the adsorbent with cyanide ions in solution performed in a batch system. The parameters examined in this study were the influence of medium pH, the effect of interaction time and the effect of initial concentration of cyanide ion adsorption ability of adsorbent hybrid amino silica gel impregnated with aluminum. Quantitative Analysis of cyanide ions left in the filtrate was tested by means of ion selective electrode. The effect of interaction time data were analyzed with kinetic model, the data of the influence of cyanide ion concentration was analyzed by Langmuir adsorption isotherm model and Freundlich. The results showed that the infrared spectroscopic identification results show APSG-Al adsorbent has silanol groups (Si-OH, siloxil (Si-O-Si, primary amine group, NH2. The result of XRD analysis of the price of 2θ at 65.51 indicates that the aluminum impregnated with the silica in the form of alumina Al2O3. The result of adsorption of cyanide by the hybrid silica gel impregnated with aluminum aminopropil (APSG-Al showed maximum adsorption occurred at pH 5 was 67.62%, silica gel impregnated with aluminum was 51,11%. Study the kinetics of the effect of interaction time showed that the adsorbent APSG-Al and SG-Al-Al has the adsorption rate constant k1 is 2.7, 10-3and 1.9,10-3 min-1, respectively. Adsorption equilibrium data showed that the adsorbent APSG-Al and SG-Al tend to follow the adsorption isotherm model Freundlich.

Analysis of separation quality of scandium-46 and titanium using silica gel column

International Nuclear Information System (INIS)

Muhamad Basit Febrian; Yanuar Setiadi; Duyeh Setiawan; Titin Sri Mulyati; Nana Suherman

2015-01-01

In this study, quality test of scandium and titanium mixture separation system using a silica gel column has been conducted. This system will be used in the separation of medical radioisotopes of 47 Sc from TiO 2 enriched targets. 20 mg of TiO 2 and 5 mg of Sc 2 O 3 dissolved using 0.5 mL of 50% HF solvent with gentle heating at 60°C - 80°C for 1 hour then 4.5 mL H 2 O was added. Sc and Ti mixture is separated by passing it through a column of silica gel. In the determination of scandium released from silica gel, Sc-46 radiotracer was used. Only 51.60 ± 4.5% of 5 mg of scandium could be retained in the silica gel column. From 51.60% of absorbed scandium in the column, 98.29 ± 3.4% were eluted with 5 mL of H 2 O eluent. During elution of scandium from silica gel column, 2.81 grams of 20 mg of titanium came apart as breakthrough. In determination of recovery of titanium from silica gel, 51.76 ± 5.5% of the 20 mg Ti can be recovered from silica gel column using 5M HCl eluent, whereas remaining Ti were eluted using 40 ml of HCl 5M. Based on those result, it can be concluded that there are still titanium portion in scandium after the separation using a silica gel column. Further purification step using fresh silica gel column, can separate escaped titanium from scandium. (author)

A silica sol-gel design strategy for nanostructured metallic materials

NARCIS (Netherlands)

Warren, S.C.; Perkins, M.R.; Adams, A.M.; Kamperman, M.M.G.

2012-01-01

Batteries, fuel cells and solar cells, among many other high-current-density devices, could benefit from the precise meso- to macroscopic structure control afforded by the silica sol–gel process. The porous materials made by silica sol–gel chemistry are typically insulators, however, which has

Methanol adsorption by amorphous silica alumina in the critical temperature range

NARCIS (Netherlands)

Kuczynski, M.; van Ooteghem, A.; Westerterp, K.R.

1986-01-01

The methanol adsorption capacity of an amorphous silica-alumina was measured using an equilibrium technique. The experimental temperature range was of 140 to 260°C and the pure methanol pressure range was 0.1 to 1.2 MPa. A multilayer adsorption was found, also for temperatures above the critical

Steady-state leaching of tritiated water from silica gel

DEFF Research Database (Denmark)

Das, H.A.; Hou, Xiaolin

2009-01-01

Aqueous leaching of tritium from silica gel, loaded by absorption of water vapor, makes part of reactor de-commissioning. It is found to follow the formulation of steady-state diffusion.......Aqueous leaching of tritium from silica gel, loaded by absorption of water vapor, makes part of reactor de-commissioning. It is found to follow the formulation of steady-state diffusion....

Alumina plate containing photosystem I reaction center complex oriented inside plate-penetrating silica nanopores.

Science.gov (United States)

Kamidaki, Chihiro; Kondo, Toru; Noji, Tomoyasu; Itoh, Tetsuji; Yamaguchi, Akira; Itoh, Shigeru

2013-08-22

The photosynthetic photosystem I reaction center complex (PSI-RC), which has a molecular diameter of 21 nm with 100 pigments, was incorporated into silica nanopores with a 100-nm diameter that penetrates an alumina plate of 60-μm thickness to make up an inorganic-biological hybrid photocell. PSI-RCs, purified from a thermophilic cyanobacterium, were stable inside the nanopores and rapidly photoreduced a mediator dye methyl viologen. The reduced dye was more stable inside nanopores suggesting the decrease of dissolved oxygen. The analysis by a cryogenic electron spin paramagnetic resonance indicated the oriented arrangement of RCs inside the 100-nm nanopores, with their surface parallel to the silica wall and perpendicular to the plane of the alumina plate. PSI RC complex in the semicrystalline orientation inside silica nanopores can be a new type of light energy conversion unit to supply strong reducing power selectively to other molecules inside or outside nanopores.

Tritium isotope separation by water distillation column packed with silica-gel beads

International Nuclear Information System (INIS)

Fukada, Satoshi

2004-01-01

Tritium enrichment or depletion by water distillation was investigated using a glass column of 32cm in height packed with silica-gel beads of 3.4mm in average diameter. The total separation factor of the silica-gel distillation column, α H-T , was compared with those of an open column distillation tower and of a column packed with stainless-steel Dixon rings. Depletion of the tritium activity in the distillate was enhanced by isotopic exchange with water absorbed on silica-gel beads that have a higher affinity for HTO than for H 2 O. The value of α H-T -1 of the silica-gel distillation column was about four times larger than that of a column without any packing and about two times larger than that of the Dixon-ring column. The improvement of α H-T by the silica-gel adsorbent indicated that the height of the distillation-adsorption column becomes shorter than that of the height of conventional distillation columns. (author)

Synthesis and characterization of silica gel from siliceous sands of southern Tunisia

Directory of Open Access Journals (Sweden)

Ali Sdiri

2014-09-01

Full Text Available The present work aimed to achieve valorization of Albian sands for the preparation of sodium silicates that are commonly used as a precursor to prepare silica gel. A siliceous sand sample was mixed with sodium carbonate and heated at a high temperature (1060 °C to prepare sodium silicates. The sodium silicates were dissolved in distilled water to obtain high quality sodium silicate solution. Hydrochloric acid was then slowly added to the hydrated sodium silicates to obtain silica gel. The collected raw siliceous sands, as well as the prepared silica gels, were characterized by different techniques, such as X-ray fluorescence (XRF, X-ray diffraction (XRD, scanning electron microscopy (SEM and thermal analysis (DSC. XRF confirmed that the detrital sand deposits of southern Tunisia contain high amounts of silica, with content ranging from 88.8% to 97.5%. The internal porosity varied between 17% and 22%, and the specific surface area was less than 5 m2/g. After the treatment described above, it was observed that the porosity of the obtained silica gel reached 57% and the specific surface area exceeded 340 m2/g. Nitrogen adsorption isotherms showed that the prepared silica gels are microporous and mesoporous materials with high adsorption capacities. These results suggest that the obtained silica gels are promising materials for numerous environmental applications.

thesis of high-purity carbon nanotubes over alumina and silica supported bimetallic catalysts

Directory of Open Access Journals (Sweden)

Sanja Ratković

2009-10-01

Full Text Available Carbon nanotubes (CNTs were synthesized by a catalytic chemical vapor deposition method (CCVD of ethylene over alumina and silica supported bimetallic catalysts based on Fe, Co and Ni. The catalysts were prepared by a precipitation method, calcined at 600 °C and in situ reduced in hydrogen flow at 700 °C. The CNTs growth was carried out by a flow the mixture of C2H4 and nitrogen over the catalyst powder in a horizontal oven. The structure and morphology of as-synthesized CNTs were characterized using SEM. The as-synthesized nanotubes were purified by acid and basic treatments in order to remove impurities such as amorphous carbon, graphite nanoparticles and metal catalysts. XRD and DTA/TG analyses showed that the amounts of by-products in the purified CNTs samples were reduced significantly. According to the observed results, ethylene is an active carbon source for growing high-density CNTs with high yield but more on alumina-supported catalysts than on their silica- supported counterparts. The last might be explained by SMSI formed in the case of alumina-supported catalysts, resulting in higher active phase dispersion.

Silica Sol-Gel Entrapment of the Enzyme Chloro peroxidase

International Nuclear Information System (INIS)

Le, T.; Chan, S.; Ebaid, B.; Sommerhalter, M.

2015-01-01

The enzyme chloro peroxidase (CPO) was immobilized in silica sol-gel beads prepared from tetramethoxysilane. The average pore diameter of the silica host structure (∼3 nm) was smaller than the globular CPO diameter (∼6 nm) and the enzyme remained entrapped after sol-gel maturation. The catalytic performance of the entrapped enzyme was assessed via the pyrogallol peroxidation reaction. Sol-gel beads loaded with 4 μg CPO per mL sol solution reached 9-12% relative activity compared to free CPO in solution. Enzyme kinetic analysis revealed a decrease in K_cat but no changes in K_M or K_I . Product release or enzyme damage might thus limit catalytic performance. Yet circular dichroism and visible absorption spectra of transparent CPO sol-gel sheets did not indicate enzyme damage. Activity decline due to methanol exposure was shown to be reversible in solution. To improve catalytic performance the sol-gel protocol was modified. The incorporation of 5, 20, or 40% methyltrimethoxysilane resulted in more brittle sol-gel beads but the catalytic performance increased to 14% relative to free CPO in solution. The use of more acidic casting buffers (ph 4.5 or 5.5 instead of 6.5) resulted in a more porous silica host reaching up to 18% relative activity

Uranyl adsorption kinetics within silica gel: dependence on flow velocity and concentration

Science.gov (United States)

Dodd, Brandon M.; Tepper, Gary

2017-09-01

Trace quantities of a uranyl dissolved in water were measured using a simple optical method. A dilute solution of uranium nitrate dissolved in water was forced through nanoporous silica gel at fixed and controlled water flow rates. The uranyl ions deposited and accumulated within the silica gel and the uranyl fluorescence within the silica gel was monitored as a function of time using a light emitting diode as the excitation source and a photomultiplier tube detector. It was shown that the response time of the fluorescence output signal at a particular volumetric flow rate or average liquid velocity through the silica gel can be used to quantify the concentration of uranium in water. The response time as a function of concentration decreased with increasing flow velocity.

Analysis of the retention of water vapor on silica gel; Analisis de la retencion del vapor de agua en silica gel

Energy Technology Data Exchange (ETDEWEB)

Herranz, M.; Pinilla, J. L.; Alegria, N.; Idoeta, R.; Legarda, F.

2011-07-01

Among the various sampling systems tritium content in the atmosphere as water vapor, one of the most basic and, therefore, of widespread use in the environmental field, is the retention on silica gel. However, the behavior of the collection efficiency of silica gel under varying conditions of air temperature and relative humidity makes it difficult to define the amount of this necessary for proper completion of sampling, especially in situations of prolonged sampling. This paper presents partial results obtained in a study on the analysis of these efficiencies under normal conditions of sampling. (Author)

The increase in pH during aging of porous sol-gel silica spheres

NARCIS (Netherlands)

Titulaer, M.K.; Kegel, W.K.; Jansen, J.B.H.; Geus, John W.

1994-01-01

The increase in pH in the hydrothermal fluid is studied after hydrothermal aging of porous silica gel spheres of 1–3 mm diameter. The porous silica spheres are formed by the sol-gel process from a supersaturated silica solution. The increase of the pH of the hydrothermal solution affects the silica

Sampling tritiated water vapor from the atmosphere by an active system using silica gel

Energy Technology Data Exchange (ETDEWEB)

Herranz, M. [Department of Nuclear Engineering and Fluid Mechanics, E.T.S.I. de Bilbao, University of the Basque Country (UPV/EHU), Alameda de Urquijo, s/n 48013 Bilbao (Spain); Alegria, N., E-mail: natalia.alegria@ehu.es [Department of Nuclear Engineering and Fluid Mechanics, E.T.S.I. de Bilbao, University of the Basque Country (UPV/EHU), Alameda de Urquijo, s/n 48013 Bilbao (Spain); Idoeta, R.; Legarda, F. [Department of Nuclear Engineering and Fluid Mechanics, E.T.S.I. de Bilbao, University of the Basque Country (UPV/EHU), Alameda de Urquijo, s/n 48013 Bilbao (Spain)

2011-11-15

Among the different methods used to collect the tritiated water vapor (HTO) contained in the atmosphere, one of the most worldwide used is its collection using an air pump, which forces the air to pass through a dry silica gel trap. The silica gel is then distilled to remove the water collected, which is measured in a liquid scintillation counting system. In this paper, an analysis of the water collection efficiency of the silica gel has been done as a function of the temperatures involved, the dimensions of the pipe driving the air into the silica gel traps, the air volume passing through the trap and the flow rates used. Among the obtained conclusions, it can be pointed out that placing the traps inside a cooled container, the amount of silica gel needed to collect all the water contained in the air passing through these traps can be estimated using a weather forecast and a psychometric chart. To do this, and as thermal equilibrium between incoming and open air should be established, a suitable design of the sampling system is proposed. - Highlights: > To recollect the atmosphere air tritiated water vapor, an active system was used. > The system is an air pump and three traps with silica gel connected by a rubber pipe. > The silica gel retention depends on the meteorological conditions and the flow rate. > The amount of water collected and the mass of silica gel need were calculated, F.

Effect of gamma radiation on silica gel, (3)

International Nuclear Information System (INIS)

Ogura, Hajime; Nakazato, Chiyoko; Kondo, Masaharu; Sawai, Teruko; Sawai, Takeshi.

1979-01-01

The γ-irradiation of silica gel degassed for 24 h above 400 0 C produces visible color center (lambda sub(max) = 530 nm). The color center instantly disappears on exposure to H 2 at room temperature and irreversible adsorption of H 2 is concurrently observed. On the basis that color center is attributed to the positive hole due to substitutional impurity of Al in silica matrix, the yield of color center and H 2 adsorption have been investigated as a function of Al content in silica gel deliberatly prepared by us from silicon tetrachloride to contain Al in the range of 10 -3 -- 5w/0. Absorbance at 530 nm, A 530 , due to color center as well as the amount of H 2 adsorbed, (H 2 )sub(ads), increase with the Al content in the matrix. A 530 /(H 2 )sub(ads) is 1.0 x 10 6 (O.D. unit g/mol) in these gels. This ratio is seen almost same with two samples of gel commercially available. By assuming that 1 mol of H 2 reacts with 2 mol of positive hole, the extinction coefficient of color center at 530 nm is evaluated as 1.0 x 10 6 (g/mol.cm). (author)

Finger-like voids induced by viscous fingering during phase inversion of alumina/PES/NMP suspensions

KAUST Repository

Wang, Bo

2012-07-01

The formation mechanism of phase-inversion ceramic hollow fibre membranes has not been well understood. In this paper, we report on the formation of finger-like macrovoids during non-solvent-induced phase inversion of alumina/PES/NMP suspensions. A membrane structure without such finger-like macrovoids was observed when the suspension was slowly immersed into pure ethanol or a mixture of 70. wt% NMP and 30. wt% water, whereas finger-like macrovoids occurred when the suspension was slid into the non-solvents at higher speeds. We found that the formation process of finger-like macrovoids could be fully or partially reversed when nascent membranes were taken out from water shortly after immersion, depending on the duration of the immersion. Splitting of the fingers during the formation of the macrovoids was also observed during the phase inversion of two alumina/PES/NMP suspensions. These experimental observations were not predicted by current theories of finger-like macrovoid formation in polymer membranes, but appear to mimic the well-known viscous fingering phenomenon. We therefore propose that in the phase inversion of ceramic suspensions, the viscous fingering phenomenon is an important mechanism in the formation of finger-like voids. © 2012 Elsevier B.V.

Regenerated silica gel as stationary phase on vacuum column chromatography to purify temulawak’s extracts

International Nuclear Information System (INIS)

Cahyono, Bambang; Maduwu, Ratna Dewi; Widayat,; Suzery, Meiny

2015-01-01

Commercial silica gel only used once by many researchers and affected high cost for purification process, also less support the green chemistry program. This research focused in regeneration silica gel that used purification of temulawak’s extracts (Curcuma xanthorrhiza Roxb) by vacuum column chromatography. Sample extracts (contains 10.1195±0.5971% of curcuminoids) was purified by vacuum column chromatography (pressure: 45 kPa, column: 100mm on length and 16mm on diameter). Ethanol 96% and acetone were compared as eluent. The amount of solvent and yield of curcuminoids used as indicator purification. The silica gel was regenerated with heating in 600°C for 8 hours The silica gels were analyzed by IR spectroscopy and X-ray diffraction. Furthermore, regenerated silica gel was used as the stationary phase in vacuum column chromatography under the same conditions with the previous purification. All the purification experiments were performed in three repetitions. Based on regression equation, y=0.132x+0.0011 (r 2 =0.9997) the yield of curcuminoids on purified products using ethanol as the eluent was improved 4.26% (to 14.3724±0.5749%) and by acetone was improved 3,03% (to 13.1450 ±0.6318%). The IR spectrum of both silica gel showed the same vibration profile and also there were three crystallinity peaks missing on its X-ray diffraction. Regenerated silica gel has the same performance with new silica gel in purification of temulawak’s extract: by ethanol has increased 4.08% (14.1947±0.7415%) and 2.93% (13.0447±0.4822) by acetone. In addition, all purification products showed similar TLC profiles. Purification using regenerated silica gel as the adsorbent on vacuum column chromatography has exactly same potential with the new silica gel

Regenerated silica gel as stationary phase on vacuum column chromatography to purify temulawak’s extracts

Energy Technology Data Exchange (ETDEWEB)

Cahyono, Bambang; Maduwu, Ratna Dewi; Widayat,; Suzery, Meiny [Organic Chemistry Laboratory, Departement of Chemistry, Diponegoro University Jln Prof. Soedharto SH, Tembalang, Semarang 50275, Indonesia Tel / Fax: (024) 7460058 (Indonesia)

2015-12-29

Commercial silica gel only used once by many researchers and affected high cost for purification process, also less support the green chemistry program. This research focused in regeneration silica gel that used purification of temulawak’s extracts (Curcuma xanthorrhiza Roxb) by vacuum column chromatography. Sample extracts (contains 10.1195±0.5971% of curcuminoids) was purified by vacuum column chromatography (pressure: 45 kPa, column: 100mm on length and 16mm on diameter). Ethanol 96% and acetone were compared as eluent. The amount of solvent and yield of curcuminoids used as indicator purification. The silica gel was regenerated with heating in 600°C for 8 hours The silica gels were analyzed by IR spectroscopy and X-ray diffraction. Furthermore, regenerated silica gel was used as the stationary phase in vacuum column chromatography under the same conditions with the previous purification. All the purification experiments were performed in three repetitions. Based on regression equation, y=0.132x+0.0011 (r{sup 2}=0.9997) the yield of curcuminoids on purified products using ethanol as the eluent was improved 4.26% (to 14.3724±0.5749%) and by acetone was improved 3,03% (to 13.1450 ±0.6318%). The IR spectrum of both silica gel showed the same vibration profile and also there were three crystallinity peaks missing on its X-ray diffraction. Regenerated silica gel has the same performance with new silica gel in purification of temulawak’s extract: by ethanol has increased 4.08% (14.1947±0.7415%) and 2.93% (13.0447±0.4822) by acetone. In addition, all purification products showed similar TLC profiles. Purification using regenerated silica gel as the adsorbent on vacuum column chromatography has exactly same potential with the new silica gel.

Adsorption characteristics of lithium in sea water with coprecipitated alumina-magnesia gel

International Nuclear Information System (INIS)

Kaneko, Shoji; Takahashi, Wataru

1988-01-01

Alumina-magnesia mixed-oxide gel exhibited adsorptive ability for lithium in sea water attributed to weak acidic sites and micropores of diameter 20-30 A. The adsorption of lithium proceeded predominantly by the mechanism of ion-exchange, on which the facility was shown in the order of Na + > H + > NH 4 + . The elution of lithium adsorbed on the gel was complete with dilute hydrochloric acid. (author)

Morphology of one-time coated palladium-alumina composite membrane prepared by sol-gel process and electroless plating technique

Science.gov (United States)

Sari, R.; Dewi, R.; Pardi; Hakim, L.; Diana, S.

2018-03-01

Palladium coated porous alumina ceramic membrane tube was obtained using a combination of sol-gel process and electroless plating technique. The thickness, structure and composition of palladium-alumina composite membrane were analyzed by transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX), and atomic force microscopy (AFM). Palladium particle size was 6.18 to 7.64 nm. Palladium membrane with thickness of approximately 301.5 to 815.1 nm was formed at the outer surface of the alumina layer. EDX data confirmed the formation of palladium-alumina membrane containing 45% of palladium. From this research it shows the combination of sol-gel process and electroless plating technique with one-time coating can produce a homogeneous and smoother palladium nano layer film on alumina substrate.

Synthesis and separation properties of an α-alumina-supported high-silica MEL membrane

NARCIS (Netherlands)

Kosinov, N.; Hensen, E.J.M.

2013-01-01

A thin high-silica MEL membrane was synthesized on a porous a-alumina hollow fiber support by a secondary growth approach. The membrane quality was evaluated by permporometry, single-gas permeation and butane isomer separation. Comparison of the pervaporation performance of MEL membranes with a MFI

Aliphatic Hydrocarbons from Lignocellulose by Pyrolysis over Cesium-Modified Amorphous Silica Alumina Catalysts

NARCIS (Netherlands)

Zabeti, M.; Sai Sankar Gupta, Karthick Babu; Raman, G.; Lefferts, Leon; Schallmoser, Stefan; Lercher, Johannes A.; Seshan, K.

2015-01-01

Cesium-modified amorphous silica alumina (Cs/ASA) is a promising catalyst for the production of hydrocarbons through pyrolysis of biomass. Catalytic pyrolysis of pinewood over Cs/ASA in a pyrolyzer system in conjunction with a gas chromatograph and mass spectrometer resulted in a 22% yield of

Controllable damping of high-Q violin modes in fused silica suspension fibers

Science.gov (United States)

Dmitriev, A. V.; Mescheriakov, S. D.; Tokmakov, K. V.; Mitrofanov, V. P.

2010-01-01

Fused silica fiber suspension of the test masses will be used in the interferometric gravitational wave detectors of the next generation. This allows a significant reduction of losses in the suspension and thermal noise associated with the suspension. Unfortunately, unwanted violin modes may be accidentally excited in the suspension fibers. The Q-factor of the violin modes also exceeds 108. They have a ring-down time that is too long and may complicate the stable control of the interferometer. Results of the investigation of a violin mode active damping system are described. An original sensor and actuator were especially developed to realize the effective coupling of a thin, optically transparent, non-conducting fused silica fiber with an electric circuit. The damping system allowed the changing of the violin mode's damping rate over a wide range.

Preparation and characterization of quercetin-loaded silica microspheres stabilized by combined multiple emulsion and sol-gel processes

Directory of Open Access Journals (Sweden)

Kim Young Ho

2015-01-01

Full Text Available Despite exhibiting a wide spectrum of cosmeceutical properties, flavonoids and related compounds have some limitations related to their stability and solubility in distilledwater. In this project, we prepared silica microspheres using a novel method that uses polyol-in-oil-in-water (P/O/W emulsion and sol-gel methods as techniques for stabilizing quercetin. A stable microsphere suspension was successfully preparedusing a mixed solvent system comprising a polyol-phase medium for performing the sol-gel processing of tetraethyl orthosilicate (TEOS as an inorganic precursor with outer water phase. The morphology of the microsphere was evaluated using a scanning electron microscope (SEM, which showed a characteristic spherical particle shape with a smooth surface. Furthermore, SEM/EDSanalysis of a representative microsphere demonstrated that the inner structure of the silica microspheres was filled with quercetin. The mean diameter of the microsphere was in the range 20.6-35.0 μm, and the encapsulation efficiency ranged from 17.8% to 27.5%. The free and encapsulated quercetin samples were incubated in separateaqueous solutions at 25 and 42°C for 28 days. The residualcontent of the quercetin encapsulated by silica microspheres was 82% at 42°C. In contrast, that of the free quercetin stored at 42°C decreased to ~24%.

Preparation of silica by sol-gel method using formamide

Directory of Open Access Journals (Sweden)

R.F.S. Lenza

2001-07-01

Full Text Available In this work we obtained microporous and mesoporous silica gels by sol-gel processing. Tetraethylortosilicate (TEOS was used as precursor. Nitric acid and hydrofluoric acid were used as catalysts. In order to study the affect of formamide as drying additive, we used a molar ratio alkoxide/formamide of 1/1. The performance of formamide in obtaining crack-free gels was evaluated through monolithicity measurements. The structural evolution occurring in the interconnected network of the gels during thermal treatment was monitored by Fourier transform infrared spectroscopy (FTIR, shrinkage and density measurements and nitrogen gas sorption. We noted that in the presence of formamide, the Si-O-Si bonds are stronger and belong to a more cross-linked structure. The samples obtained in the presence of formamide have larger pore volume and its pore structure is in the range of mesoporosity. The samples obtained without additive are microporous. Formamide allowed the preparation of crack-free silica gels stabilized at high temperatures.

Gas-phase acylation of aminopropyl-silica gel in the synthesis of some chemically bonded silica materials for analytical applications

International Nuclear Information System (INIS)

Basiuk, Vladimir; Khil'chevskaya, E.G.

1991-01-01

Gas-phase acylation of aminopropyl-silica gel with aliphatic dicarboxylic (succinic, adipic and sebacic) and 4-aminobenzoic acids is proposed as a rapid and efficient one-step method for the synthesis of carboxyalkyl- and 4-aminophenylamidopropyl-silica gels, usually used as zwitterion exchangers for liquid chromatography and matrices for multi-step syntheses of silica-bound aromatic azo reagents for the sorption and chromatographic separation of metal ions. Acylation degrees of 59-90% are achieved after 0.5 h. IR spectra of the acylation products and near-UV-visible spectra for bonded aromatic azo compounds, based on 4-aminobenzamidopropyl-silica gel, are presented. Some positive and negative aspects of the gas-phase acylation are discussed. (author). 34 refs.; 2 figs.; 2 tabs

Hydrogen Production by Steam Reforming of Ethanol over Nickel Catalysts Supported on Sol Gel Made Alumina: Influence of Calcination Temperature on Supports.

Science.gov (United States)

Yaakob, Zahira; Bshish, Ahmed; Ebshish, Ali; Tasirin, Siti Masrinda; Alhasan, Fatah H

2013-05-30

Selecting a proper support in the catalyst system plays an important role in hydrogen production via ethanol steam reforming. In this study, sol gel made alumina supports prepared for nickel (Ni) catalysts were calcined at different temperatures. A series of (Ni/Al S.G. ) catalysts were synthesized by an impregnation procedure. The influence of varying the calcination temperature of the sol gel made supports on catalyst activity was tested in ethanol reforming reaction. The characteristics of the sol gel alumina supports and Ni catalysts were affected by the calcination temperature of the supports. The structure of the sol gel made alumina supports was transformed in the order of γ → (γ + θ) → θ-alumina as the calcination temperature of the supports increased from 600 °C to 1000 °C. Both hydrogen yield and ethanol conversion presented a volcano-shaped behavior with maximum values of 4.3 mol/mol ethanol fed and 99.5%, respectively. The optimum values were exhibited over Ni/Al S.G800 (Ni catalyst supported on sol gel made alumina calcined at 800 °C). The high performance of the Ni/Al S.G800 catalyst may be attributed to the strong interaction of Ni species and sol gel made alumina which lead to high nickel dispersion and small particle size.

11C-radioisotope study of methanol co-reaction with ethanol over Ni-MCM-41 silica-alumina and Ni-alumina

International Nuclear Information System (INIS)

Sarkadi-Priboczki, E.; Kovacs, Z.; Tsoncheva, T.; Kumar, N.; Murzin, D.Yu.

2009-01-01

Complete text of publication follows. The Ni modifies the properties of acidic alumina and light acidic MCM-41 silica-alumina supports. The radioisotopic method is a suitable tool for distinction of the 11 Cradioisotopic methanol and its co-derivates from derivates of non-radioactive ethanol on these catalysts. Experimental. The Ni/A l 2O 3 (5 wt % Ni) is commercially available while H-MCMN-41 (Si/Al=20) and Ni-ion-exchanged MCM-41 silica-alumina (5 wt % Ni) were prepared and characterized in previous works. Before catalysis the Ni/Al 2 O 3 and Ni-MCM-41 were pre-reduced. The 11 C-methanol was formed by a radiochemical process from 11 C-carbon dioxide produced at cyclotron (T 1/2 = 20.4 min). The mixture of equivalent volume of radioactive methanol and non-radioactive ethanol was introduced into glass tube micro-flow reactor at ambient temperature. After adsorption, the valves were closed and the catalyst was heated up to the required temperatures. The desorption rate of the remaining 11 C-derivatives on catalysts were continuously followed by radiodetectors and the derivatives of methanol with ethanol were analyzed by Radio/FID-gas chromatography (FID is coupled on-line with a radiodetector). The ethanol and its derivates were identified by FID while the 11 C-methanol and its co-derivates (with ethanol) were detected by both of FID and radiodetector. Results The 11 C-dimethyl ether was the common product of the single 11 C-methanol transformation on H-MCM-41, Ni-MCM-41 and Ni- Al 2 O 3 at low temperature (200-280 degC) due to middle strong acid sites. At higher temperature (280-350 degC), the dimethyl ether and hydrocarbons were the dominant products on H-MCM-41 while dimethyl ether selectivity decreased on Ni-alumina and Ni-MCM-41 in favor of methane. The selectivities of methanol to formaldehyde and methane were the highest on Ni-MCM-41. During co-reaction of 11 C-methanol with non-radioactive ethanol, the 11 C-labeled coethers, namely 11 C-methyl ethyl ether

Influence of ultrasonic frequency on the regeneration of silica gel by applying high-intensity ultrasound

International Nuclear Information System (INIS)

Zhang Weijiang; Yao Ye; Wang Rongshun

2010-01-01

Ultrasonic frequency is the key parameter considered in ultrasonic applications. In order to provide a basic knowledge about the influence of ultrasonic frequency on the regeneration of silica gel assisted by power ultrasound, the experiments about silica gel regeneration under the radiation of constant-power (60 W) ultrasound with different frequencies (i.e., 23, 27, and 38 kHz) and that without ultrasound were carried out at different regeneration temperatures (i.e., 35, 45, 55, and 65 deg. C). The experimental results showed that the lower frequency was beneficial for the application of power ultrasound in the regeneration of silica gel. The fact was theoretically explained by the ultrasonic power attenuation model which indicates that the ultrasound of lower frequency will lead to more uniform energy distribution and hence achieve higher efficiency of utilization. Meanwhile, the effect of ultrasonic frequency on silica gel regeneration would be influenced by the regeneration temperature and the moisture ratio in silica gel. As investigated in this study, the effect of ultrasonic frequency on the regeneration would be more significant at the lower regeneration temperature or at the higher moisture ratio in silica gel. In addition, the mean regeneration speed model of silica gel dependent of the regeneration temperature and the ultrasonic frequency was established according to the experimental data.

Controllable damping of high-Q violin modes in fused silica suspension fibers

Energy Technology Data Exchange (ETDEWEB)

Dmitriev, A V; Mescheriakov, S D; Mitrofanov, V P [Faculty of Physics, Moscow State University, Moscow 119991 (Russian Federation); Tokmakov, K V, E-mail: dmitriev@hbar.phys.msu.r, E-mail: mitr@hbar.phys.msu.r [Present address: Department of Physics, SUPA, University of Strathclyde, Glasgow G4 0NG (United Kingdom)

2010-01-21

Fused silica fiber suspension of the test masses will be used in the interferometric gravitational wave detectors of the next generation. This allows a significant reduction of losses in the suspension and thermal noise associated with the suspension. Unfortunately, unwanted violin modes may be accidentally excited in the suspension fibers. The Q-factor of the violin modes also exceeds 10{sup 8}. They have a ring-down time that is too long and may complicate the stable control of the interferometer. Results of the investigation of a violin mode active damping system are described. An original sensor and actuator were especially developed to realize the effective coupling of a thin, optically transparent, non-conducting fused silica fiber with an electric circuit. The damping system allowed the changing of the violin mode's damping rate over a wide range.

Controllable damping of high-Q violin modes in fused silica suspension fibers

International Nuclear Information System (INIS)

Dmitriev, A V; Mescheriakov, S D; Mitrofanov, V P; Tokmakov, K V

2010-01-01

Fused silica fiber suspension of the test masses will be used in the interferometric gravitational wave detectors of the next generation. This allows a significant reduction of losses in the suspension and thermal noise associated with the suspension. Unfortunately, unwanted violin modes may be accidentally excited in the suspension fibers. The Q-factor of the violin modes also exceeds 10 8 . They have a ring-down time that is too long and may complicate the stable control of the interferometer. Results of the investigation of a violin mode active damping system are described. An original sensor and actuator were especially developed to realize the effective coupling of a thin, optically transparent, non-conducting fused silica fiber with an electric circuit. The damping system allowed the changing of the violin mode's damping rate over a wide range.

Zeolite - a possible substitute of silica gel in spectrophotometric determination of uranium?

International Nuclear Information System (INIS)

Foeldesova, M; Dillinger, P.

2006-01-01

Zeolites sorption abilities differ from the ones of the silica gel, which is normally used for uranium determination by spectrophotometric method. The difference is obvious mainly in the case of zeolites chemically modified with 1 or 2 mol/L NaOH solution. Absorbances measured using these zeolites on an radioactive water samples were 4 to 4.2 times bigger than the ones with silica gel. This avoids a use of one universal calibration curve for experimental data evaluation. Within delivered experimental data only a calibration curve for silica gel was provided. Its application to zeolites caused substantial misinterpretation of the results. Calculational construction of individual calibration curves made at this work shaw, that zeolites have a potential to replace the silica gel. This possibility is necessary to confirm by more experiments. Better sorption abilities of the modified zeolites would be utilized to reduce the lower limit for uranium determination by spectrophotometric method. (authors)

Radiation hardening of sol gel-derived silica fiber preforms through fictive temperature reduction.

Science.gov (United States)

Hari Babu, B; Lancry, Matthieu; Ollier, Nadege; El Hamzaoui, Hicham; Bouazaoui, Mohamed; Poumellec, Bertrand

2016-09-20

The impact of fictive temperature (Tf) on the evolution of point defects and optical attenuation in non-doped and Er3+-doped sol-gel silica glasses was studied and compared to Suprasil F300 and Infrasil 301 glasses before and after γ-irradiation. To this aim, sol-gel optical fiber preforms have been fabricated by the densification of erbium salt-soaked nanoporous silica xerogels through the polymeric sol-gel technique. These γ-irradiated fiber preforms have been characterized by FTIR, UV-vis-NIR absorption spectroscopy, electron paramagnetic resonance, and photoluminescence measurements. We showed that a decrease in the glass fictive temperature leads to a decrease in the glass disorder and strained bonds. This mainly results in a lower defect generation rate and thus less radiation-induced attenuation in the UV-vis range. Furthermore, it was found that γ-radiation "hardness" is higher in Er3+-doped sol-gel silica compared to un-doped sol-gel silica and standard synthetic silica glasses. The present work demonstrates an effective strategy to improve the radiation resistance of optical fiber preforms and glasses through glass fictive temperature reduction.

Highly Luminescent and Ultrastable CsPbBr3 Perovskite Quantum Dots Incorporated into a Silica/Alumina Monolith.

Science.gov (United States)

Li, Zhichun; Kong, Long; Huang, Shouqiang; Li, Liang

2017-07-03

We successfully prepared QDs incorporated into a silica/alumina monolith (QDs-SAM) by a simple sol-gel reaction of an Al-Si single precursor with CsPbBr 3 QDs blended in toluene solution, without adding water and catalyst. The resultant transparent monolith exhibits high photoluminescence quantum yields (PLQY) up to 90 %, and good photostability under strong illumination of blue light for 300 h. We show that the preliminary ligand exchange of didodecyl dimethyl ammonium bromide (DDAB) was very important to protect CsPbBr 3 QDs from surface damages during the sol-gel reaction, which not only allowed us to maintain the original optical properties of CsPbBr 3 QDs but also prevented the aggregation of QDs and made the monolith transparent. The CsPbBr 3 QDs-SAM in powder form was easily mixed into the resins and applied as color-converting layer with curing on blue light-emitting diodes (LED). The material showed a high luminous efficacy of 80 lm W -1 and a narrow emission with a full width at half maximum (FWHM) of 25 nm. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Alkali Metal Modification of Silica Gel-Based Stationary Phase in Gas Chromatography

Directory of Open Access Journals (Sweden)

Ashraf Yehia El-Naggar

2013-01-01

Full Text Available Modification of the precipitated silica gel was done by treatment with alkali metal (NaCl before and after calcination. The silica surfaces before and after modification were confirmed by infrared spectroscopy in order to observe the strength and abundance of the acidic surface OH group bands which play an important role in the adsorption properties of polar and nonpolar solutes. The surface-modified silica gels were tested as GC solid stationary phases in terms of the separation efficiency for various groups of non-polar and polar solutes. Also, thermodynamic parameters (ΔH, ΔG, and ΔS were determined using n-hexane as a probe in order to show the adsorbate-adsorbent interaction. It was observed that the non-polar solutes could be separated Independent on the reactivity and porosity of the silica surfaces. The efficiency of the surface-modified silica gels to separate the aromatic hydrocarbons seemed to be strongly influenced by the density of the surface hydroxyls.

Sol-gel Derived Warfarin - Silica Composites for Controlled Drug Release.

Science.gov (United States)

Dolinina, Ekaterina S; Parfenyuk, Elena V

2017-01-01

Warfarin, commonly used anticoagulant in clinic, has serious shortcomings due to its unsatisfactory pharmacodynamics. One of the efficient ways for the improvement of pharmacological and consumer properties of drugs is the development of optimal drug delivery systems. The aim of this work is to synthesize novel warfarin - silica composites and to study in vitro the drug release kinetics to obtain the composites with controlled release. The composites of warfarin with unmodified (UMS) and mercaptopropyl modified silica (MPMS) were synthesized by sol-gel method. The composite formation was confirmed by FTIR spectra. The concentrations of warfarin released to media with pH 1.6, 6.8 and 7.4 were measured using UV spectroscopy. The drug release profiles from the solid composites were described by a series of kinetic models which includes zero order kinetics, first order kinetics, the modified Korsmeyer-Peppas model and Hixson-Crowell model. The synthesized sol-gel composites have different kinetic behavior in the studied media. In contrast to the warfarin composite with unmodified silica, the drug release from the composite with mercaptopropyl modified silica follows zero order kinetics for 24 h irrespective to the release medium pH due to mixed mechanism (duffusion + degradation and/or disintegration of silica matrix). The obtained results showed that warfarin - silica sol-gel composites have a potential application for the development of novel oral formulation of the drug with controlled delivery. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

Influence of organic solvents on interfacial water at surfaces of silica gel and partially silylated fumed silica

International Nuclear Information System (INIS)

Turov, V.V.; Gun'ko, V.M.; Tsapko, M.D.; Bogatyrev, V.M.; Skubiszewska-Zieba, J.; Leboda, R.; Ryczkowski, J.

2004-01-01

The effects of organic solvents (dimethylsulfoxide-d 6 (DMSO-d 6 ), chloroform-d, acetone-d 6 , and acetonitrile-d 3 ) on the properties of interfacial water at surfaces of silica gel Si-40 and partially silylated fumed silica A-380 were studied by means of the 1 H NMR spectroscopy with freezing-out of adsorbed water at 180 1 H NMR investigations were also analysed on the basis of the structural characteristics of silicas and quantum chemical calculations of the chemical shifts δ H and solvent effects. DMSO-d 6 and acetonitrile-d 3 are poorly miscible with water in silica gel pores in contrast to the bulk liquids. DMSO-d 6 and chloroform-d affect the structure of the interfacial water weaker than acetone-d 6 and acetonitrile-d 3 at amounts of liquids greater than the pore volume. Acetone-d 6 and acetonitrile-d 3 can displace water from pores under this condition. The chemical shift of protons in water adsorbed on silica gel is 3.5-6.5 ppm, which corresponds to the formation of two to four hydrogen bonds per molecule. Water adsorbed on partially silylated fumed silica has two 1 H NMR signals at 5 and 1.1-1.7 ppm related to different structures (droplets and small clusters) of the interfacial water

The role seemingly of amorphous silica gel layers in chiral separations by planar chromatography

International Nuclear Information System (INIS)

Sajewicz, M.; Kowalska, T.

2007-01-01

In planar chromatography, silica gel appears as the most frequently used adsorbent. Its preference as planar chromatographic stationary phase is due to its high specific surface area (ca. 700 m2 gl) and relatively simple active sites (silanol groups =Si-OH). The high specific surface area of silica gel and a high density of coverage of its surface with the silanol active sites contribute jointly to an excellent separation performance of this adsorbent. In our experiments on chiral separation of the enantiomer pairs by planar chromatography, contradictory behavior of the silica gel layers versus the chiral compounds was observed. The migration tracks of chiral compounds in the ascending planar chromatographic mode were not vertical but bent on either side being a function of analyte chirality. This deviation of the analytes migration track was noticed, when using the densitometric scanner to quantify the respective chromatograms. In order to confirm the hypothesis as to the microcrystalline nature of silica gel used in liquid chromatography, it was further investigated through circular dichroism (CD) and the data thereof confirmed that the chromatographic silica gels are not amorphous but microcrystalline, contributing to the (partial) horizontal enantioseparation of the antimer pairs. This paper summarizes the results of our investigation on the microcrystalline nature of silica gels used in planar chromatography and their impact on enantioseparation of the selected pairs of antimers. (author)

Diffusion and flow of water vapours in chromatographic Alumina gel

International Nuclear Information System (INIS)

Khan, M.; Shah, H. U.

2005-01-01

The kinetics of sorption of water vapours in chromatographic alumina gel was studied. Water vapours are adsorbed on the gel at temperature (15 degree C) at different constant relative pressure from 0.1-0.93 p/p. Rate constant, Effective diffusivities, Knudsen diffusivities and bulk diffusivities were determined through Fick type equation. Total pore volume is 0.498 cc g-1 and specific surface area comes to be 465 m2 g-1 as obtained by Gurvitsch rule and Kieselve's quantities respectively. An average pore radius (hydraulic) is 1.1x10/sub -7/ cm. The study of these quantities provide a strong basis for evaluating surface properties. (author)

A Short Overview on the Biomedical Applications of Silica, Alumina and Calcium Phosphate-based Nanostructured Materials.

Science.gov (United States)

Ellahioui, Younes; Prashar, Sanjiv; Gómez-Ruiz, Santiago

2016-01-01

This article reviews the use of silica, alumina and calcium phosphate-based nanostructured materials with biomedical applications. A short introduction on the use of the materials in Science, Nanotechnology and Health is included followed by a revision of each of the selected materials. A description of the principal synthetic methods used in the preparation of the materials in nanostructured form is included. The most widely used applications in biomedicine are reviewed including, for example drug-delivery, bone regeneration, imaging, sensoring amongst others. Finally, a short description of the toxicity and cytotoxicity associated with each of the materials of this revision is presented. This short literature revision serves to demonstrate the very promising future ahead of nanosystems based on silica, alumina and calcium phosphate for biological and biomedical applications.

Fluorescence metrology of silica sol-gels

Indian Academy of Sciences (India)

We have developed a new method for measuring in-situ the growth of the nanometre-size silica particles which lead to the formation of sol-gel glasses. This technique is based on the decay of fluorescence polarisation anisotropy due to Brownian rotation of dye molecules bound to the particles. Results to date give near ...

Extraction of metal ions using chemically modified silica gel: a PIXE analysis.

Science.gov (United States)

Jal, P K; Dutta, R K; Sudarshan, M; Saha, A; Bhattacharyya, S N; Chintalapudi, S N; K Mishra, B

2001-08-30

Organic ligand with carboxyhydrazide functional group was immobilised on the surface of silica gel and the metal binding capacity of the ligand-embedded silica was investigated. The functional group was covalently bonded to the silica matrix through a spacer of methylene groups by sequential reactions of silica gel with dibromobutane, malonic ester and hydrazine in different media. Surface area value of the modified silica was determined. The changes in surface area were correlated with the structural change of the silica surface due to chemical modifications. A mixture solution of metal ions [K(I),Cr(III),Co(II),Ni(II),Cu(II),Zn(II),Hg(II) and U(VI)] was treated with the ligand-embedded silica in 10(-3) M aqueous solution. The measurement of metal extraction capacity of the silica based ligand was done by multielemental analysis of the metal complexes thus formed by using Proton Induced X-ray Emission (PIXE) technique.

Comparison study for the CCME reference method for determination of PHC in soil by using internal and external standard methods and by using silica gel column cleanup and in-situ silica gel cleanup methods

International Nuclear Information System (INIS)

Wang, Z.; Fingas, M.; Sigouin, L.; Yang, C.; Hollebone, B.

2003-01-01

The assessment, cleanup, and remediation of hydrocarbon contaminated sites is covered in the Reference Method for Canada-Wide Standard for Petroleum Hydrocarbons-Tier 1 Method. It replaces several analytical methods used in the past by some laboratories and jurisdictions in Canada. The authors conducted two comparative evaluations to validate the Tier 1 Analytical Method. The first compared the Internal and External Standard Methods, and the second compared the Silica Gel Column Cleanup Method with the In-situ Silica Gel Cleanup Method. The Canadian Council of Ministers of the Environment (CCME) Tier 1 Method recommends and requires the External Standard Method to determine petroleum hydrocarbons (PHC) in soil samples. The Internal Method is widely used to quantify various organic and inorganic pollutants in environmental samples. The Tier 1 Method offers two options for the same extract cleanup. They are: Option A - In-situ Silica Gel Cleanup, and Option B - Silica Gel Column Cleanup. Linearity, precision, and PHC quantification results were the parameters considered for diesel and motor oil solutions, for diesel spiked soil samples, and for motor oil spiked soil samples. It was concluded that both the External and Internal Standard Methods for gas chromatograph (GC) determination of PHC in soil possess their own advantages. The PHC results obtained using the In-Situ Silica Gel Cleanup Method were lower than those obtained with the Silica Gel Column Cleanup Methods. The more efficient and effective sample cleanup method proved to be the Silica Gel Column Method. 13 refs., 7 tabs., 7 figs

Fluorescence metrology of silica sol–gels – The effect of D2O and ...

Indian Academy of Sciences (India)

Administrator

industrial quality control and helping fundamental research. ... Of all the possible syntheses, sodium silicate (i.e. water glass) production of silica gel, ... fine silica gel powders used in many applications (e.g. chromatography, toothpaste etc).

Removal mechanism of tritium by variously pretreated silica gel

International Nuclear Information System (INIS)

Nakashima, M.; Tachikawa, E.; Saeki, M.; Aratono, Y.

1981-01-01

Removal mechanisms of HTO from variously pretreated and non-pretreated silica gel columns were investigated with pulse-loading with tritiated water vapor. With non-pretreated silica gel, the HTO physisorbed on the upper part of the column comes into contact with surface hydroxyl groups while passing downward the column, so that in each equilibration a part of the tritium is incorporated into hydroxyl groups by H/T isotopic exchange reactions. With the silica gel pretreated at a temperature below 400 0 C, most of tritium in the applied HTO is easily incorporated into surface hydroxyl groups in the upper part of the column either by H/T isotopic exchange reactions or by rehydration of the dehydrated surface (siloxyl linkage). In the pretreatment above 400 0 C, essentially all the tritium is trapped by siloxyl groups of various stabilities. The ease of rehydration of siloxyl groups by applied HTO depends on their stabilities, which, in turn, depend on the pretreatment temperature. As a general trend, treatment at higher temperature promotes annealing of the constrained siloxyl groups and thus the rate of rehydration becomes slower. (author)

Persistent superhydrophilicity of sol-gel derived nanoporous silica thin films

International Nuclear Information System (INIS)

Ganjoo, S; Azimirad, R; Akhavan, O; Moshfegh, A Z

2009-01-01

In this investigation, sol-gel synthesized nanoporous silica thin films, annealed at different temperatures, with long time superhydrophilic property have been studied. Two kinds of sol-gel silica thin films were fabricated by dip-coating of glass substrates in two different solutions; with low and high water. The transparent coated films were dried at 100 deg. C and then annealed in a temperature range of 200-500 deg. C. The average water contact angle of the silica films prepared with low water content and annealed at 300 deg. C measured about 5 deg. for a long time (6 months) without any UV irradiation. Instead, adding water into the sol resulted in silica films with an average water contact angle greater than 60 deg. Atomic force microscopic analysis revealed that the silica films prepared with low water had a rough surface (∼30 nm), while the films prepared with high water had a smoother surface (∼2 nm). Using x-ray photoelectron spectroscopy, we have shown that with a decrease in the surface water on the film, its hydrophilicity increases logarithmically.

Influence of organic solvents on interfacial water at surfaces of silica gel and partially silylated fumed silica

Energy Technology Data Exchange (ETDEWEB)

Turov, V.V.; Gun' ko, V.M.; Tsapko, M.D.; Bogatyrev, V.M.; Skubiszewska-Zieba, J.; Leboda, R.; Ryczkowski, J

2004-05-15

The effects of organic solvents (dimethylsulfoxide-d{sub 6} (DMSO-d{sub 6}), chloroform-d, acetone-d{sub 6}, and acetonitrile-d{sub 3}) on the properties of interfacial water at surfaces of silica gel Si-40 and partially silylated fumed silica A-380 were studied by means of the {sup 1}H NMR spectroscopy with freezing-out of adsorbed water at 180silicas and quantum chemical calculations of the chemical shifts {delta}{sub H} and solvent effects. DMSO-d{sub 6} and acetonitrile-d{sub 3} are poorly miscible with water in silica gel pores in contrast to the bulk liquids. DMSO-d{sub 6} and chloroform-d affect the structure of the interfacial water weaker than acetone-d{sub 6} and acetonitrile-d{sub 3} at amounts of liquids greater than the pore volume. Acetone-d{sub 6} and acetonitrile-d{sub 3} can displace water from pores under this condition. The chemical shift of protons in water adsorbed on silica gel is 3.5-6.5 ppm, which corresponds to the formation of two to four hydrogen bonds per molecule. Water adsorbed on partially silylated fumed silica has two {sup 1}H NMR signals at 5 and 1.1-1.7 ppm related to different structures (droplets and small clusters) of the interfacial water.

Highly luminescent and ultrastable CsPbBr{sub 3} perovskite quantum dots incorporated into a silica/alumina monolith

Energy Technology Data Exchange (ETDEWEB)

Li, Zhichun; Kong, Long; Huang, Shouqiang; Li, Liang [School of Environmental Science and Engineering, Shanghai Jiao Tong University (China)

2017-07-03

We successfully prepared QDs incorporated into a silica/alumina monolith (QDs-SAM) by a simple sol-gel reaction of an Al-Si single precursor with CsPbBr{sub 3} QDs blended in toluene solution, without adding water and catalyst. The resultant transparent monolith exhibits high photoluminescence quantum yields (PLQY) up to 90 %, and good photostability under strong illumination of blue light for 300 h. We show that the preliminary ligand exchange of didodecyl dimethyl ammonium bromide (DDAB) was very important to protect CsPbBr{sub 3} QDs from surface damages during the sol-gel reaction, which not only allowed us to maintain the original optical properties of CsPbBr{sub 3} QDs but also prevented the aggregation of QDs and made the monolith transparent. The CsPbBr{sub 3} QDs-SAM in powder form was easily mixed into the resins and applied as color-converting layer with curing on blue light-emitting diodes (LED). The material showed a high luminous efficacy of 80 lm W{sup -1} and a narrow emission with a full width at half maximum (FWHM) of 25 nm. (copyright 2017 Wiley-VCH Verlag GmbH and Co. KGaA, Weinheim)

The Role Seemingly of Amorphous Silica Gel Layers in Chiral Separations by Planar Chromatography

Directory of Open Access Journals (Sweden)

Teresa Kowalska

2007-12-01

Full Text Available In planar chromatography, silica gel appears as the most frequently used adsorbent. Its preference as planar chromatographic stationary phase is due to its high specific surface area (ca. 700 m2 g-1 and relatively simple active sites (silanol groups, Si-OH. The high specific surface area of silica gel and a high density of coverage of its surface with the silanol active sites contribute jointly to an excellent separation performance of this adsorbent. In our experiments on chiral separation of the enantiomer pairs by planar chromatography, contradictory behavior of the silica gel layers versus the chiral compounds was observed. The migration tracks of chiral compounds in the ascending planar chromatographic mode were not vertical but bent on either side being a function of analyte chirality. This deviation of the analyte’s migration track was noticed, when using the densitometric scanner to quantify the respective chromatograms. In order to confirm the hypothesis as to the microcrystalline nature of silica gel used in liquid chromatography, it was further investigated through circular dichroism (CD and the data thereof confirmed that the ‘chromatographic’ silica gels are not amorphous but microcrystalline, contributing to the (partial horizontal enantioseparation of the antimer pairs. This paper summarizes the results of our investigation on the microcrystalline nature of silica gels used in planar chromatography and their impact on enantioseparation of the selected pairs of antimers.

Tough ceramic coatings: Carbon nanotube reinforced silica sol-gel

Science.gov (United States)

López, A. J.; Rico, A.; Rodríguez, J.; Rams, J.

2010-08-01

Silica coatings reinforced with carbon nanotubes were produced via sol-gel route using two mixing techniques of the sol-gel precursors, mechanical and ultrasonic mixing, and dip-coating as deposition process on magnesium alloy substrates. Effective incorporation and distribution of 0.1 wt.% of carbon nanotubes in the amorphous silica matrix of the coatings were achieved using both techniques. Fabrication procedure determines the morphological aspects of the coating. Only mechanical mixing process produced coatings dense and free of defects. Nanoindentation technique was used to examine the influence of the fabrication process in the mechanical features of the final coatings, i.e. indentation fracture toughness, Young's modulus and hardness. A maximum toughening effect of about 24% was achieved in silica coatings reinforced with carbon nanotubes produced by the mechanical mixing route. Scanning electron microscopy investigation revealed that the toughening of these reinforced coatings was mainly due to bridging effect of the reinforcement.

The influence of white and blue silica gels as adsorbents in adsorptive-distillation of ethanol-water mixture

Science.gov (United States)

Megawati, Jannah, Reni Ainun; Rahayuningtiyas, Indi

2017-01-01

This research studied the difference of white and blue silica gels when used as an adsorbent for ethanol purification that is processed via Adsorptive-Distillation (AD) at 1 atm pressure. The effect of process duration to purification process is also recorded and studied to evaluate the performance of designed AD equipment. The experiment was conducted using boiling flask covered with a heating mantle and the temperature was maintained at 78°C. The vapour flowed into the adsorbent column and was condensed using water as a cooling medium. The initial ethanol concentration was 90.8% v/v and volume was 300 mL. Experiment shows that designed AD equipment could be used to purify ethanol. The average vapour velocity was about 39.29 and 45.91 m/s for white and blue silica gels, respectively, which is considered very high. Therefore the saturated adsorption could not be obtained. Highest ethanol concentration achieved using white silica gel is about 96.671% v/v after 50 minutes. Thus AD with white silica gel showed good performance and passed azeotropic point. But AD with blue silica gel showed a different result, the adsorption of blue silica gel failed to break the azeotropic point. The outlet average water concentration for white and blue silica gels is 3.54 and 3.42 mole/L. Based on the weight ratio of adsorbed water per adsorbent, at 55th minutes of time; this ratio of blue silica gel is about 0.053 gwater/gads. The time required by the blue silica to achieve 0.5 wwater-adsorbed/wwater-initial is 45 minutes, and the average outlet water concentration is 3.42 mole/L. Meanwhile, the time required by a white silica to complete 0.5 wwater-adsorbed/wwater-initial is 35 minutes, and the average outlet water level is 3.54 mole/L. Based on the results, the blue silica as an adsorbent for AD of ethanol-water mixture is better than white silica gel.

A comparative study of the nanoscale and macroscale tribological attributes of alumina and stainless steel surfaces immersed in aqueous suspensions of positively or negatively charged nanodiamonds

Science.gov (United States)

Curtis, Colin K; Marek, Antonin; Smirnov, Alex I

2017-01-01

This article reports a comparative study of the nanoscale and macroscale tribological attributes of alumina and stainless steel surfaces immersed in aqueous suspensions of positively (hydroxylated) or negatively (carboxylated) charged nanodiamonds (ND). Immersion in −ND suspensions resulted in a decrease in the macroscopic friction coefficients to values in the range 0.05–0.1 for both stainless steel and alumina, while +ND suspensions yielded an increase in friction for stainless steel contacts but little to no increase for alumina contacts. Quartz crystal microbalance (QCM), atomic force microscopy (AFM) and scanning electron microscopy (SEM) measurements were employed to assess nanoparticle uptake, surface polishing, and resistance to solid–liquid interfacial shear motion. The QCM studies revealed abrupt changes to the surfaces of both alumina and stainless steel upon injection of –ND into the surrounding water environment that are consistent with strong attachment of NDs and/or chemical changes to the surfaces. AFM images of the surfaces indicated slight increases in the surface roughness upon an exposure to both +ND and −ND suspensions. A suggested mechanism for these observations is that carboxylated −NDs from aqueous suspensions are forming robust lubricious deposits on stainless and alumina surfaces that enable gliding of the surfaces through the −ND suspensions with relatively low resistance to shear. In contrast, +ND suspensions are failing to improve tribological performance for either of the surfaces and may have abraded existing protective boundary layers in the case of stainless steel contacts. This study therefore reveals atomic scale details associated with systems that exhibit starkly different macroscale tribological properties, enabling future efforts to predict and design complex lubricant interfaces. PMID:29046852

A comparative study of the nanoscale and macroscale tribological attributes of alumina and stainless steel surfaces immersed in aqueous suspensions of positively or negatively charged nanodiamonds

Directory of Open Access Journals (Sweden)

Colin K. Curtis

2017-09-01

Full Text Available This article reports a comparative study of the nanoscale and macroscale tribological attributes of alumina and stainless steel surfaces immersed in aqueous suspensions of positively (hydroxylated or negatively (carboxylated charged nanodiamonds (ND. Immersion in −ND suspensions resulted in a decrease in the macroscopic friction coefficients to values in the range 0.05–0.1 for both stainless steel and alumina, while +ND suspensions yielded an increase in friction for stainless steel contacts but little to no increase for alumina contacts. Quartz crystal microbalance (QCM, atomic force microscopy (AFM and scanning electron microscopy (SEM measurements were employed to assess nanoparticle uptake, surface polishing, and resistance to solid–liquid interfacial shear motion. The QCM studies revealed abrupt changes to the surfaces of both alumina and stainless steel upon injection of –ND into the surrounding water environment that are consistent with strong attachment of NDs and/or chemical changes to the surfaces. AFM images of the surfaces indicated slight increases in the surface roughness upon an exposure to both +ND and −ND suspensions. A suggested mechanism for these observations is that carboxylated −NDs from aqueous suspensions are forming robust lubricious deposits on stainless and alumina surfaces that enable gliding of the surfaces through the −ND suspensions with relatively low resistance to shear. In contrast, +ND suspensions are failing to improve tribological performance for either of the surfaces and may have abraded existing protective boundary layers in the case of stainless steel contacts. This study therefore reveals atomic scale details associated with systems that exhibit starkly different macroscale tribological properties, enabling future efforts to predict and design complex lubricant interfaces.

Synthesis of Silica Nanoparticles by Sol-Gel: Size-Dependent Properties, Surface Modification, and Applications in Silica-Polymer Nano composites-A Review

International Nuclear Information System (INIS)

Ismail, A.R.; Vejayakumaran, P.

2012-01-01

Application of silica nanoparticles as fillers in the preparation of nano composite of polymers has drawn much attention, due to the increased demand for new materials with improved thermal, mechanical, physical, and chemical properties. Recent developments in the synthesis of monodispersed, narrow-size distribution of nanoparticles by sol-gel method provide significant boost to development of silica-polymer nano composites. This paper is written by emphasizing on the synthesis of silica nanoparticles, characterization on size-dependent properties, and surface modification for the preparation of homogeneous nano composites, generally by sol-gel technique. The effect of nano silica on the properties of various types of silica-polymer composites is also summarized.

Rice Husk Ash as a Renewable Source for the Production of Value Added Silica Gel and its Application: An Overview

Directory of Open Access Journals (Sweden)

Ram Prasad

2012-06-01

Full Text Available In recent years, silica gels have developed a lot of interest due to their extraordinary properties and their existing and potential applications in science and technology. Silica gel has a wide range of applications such as a desiccant, as a preservation tool to control humidity, as an adsorbent, as a catalyst and as a cata-lyst support. Silica gel is a rigid three-dimensional network of colloidal silica, and is classified as: aqua-gel, alco-gel, xero-gel and aero-gel. Out of all known solid porous materials, aero-gels are particularly known for their high specific surface area, high porosity, low bulk density, high thermal insulation value, ultra low dielectric constant and low index of refraction. Because of these extraordinary properties silica aero-gel has many commercial applications such as thermal window insulation, acoustic barriers, super-capacitors and catalytic supports. However, monolithic silica aero-gel has been used extensively in high energy physics in Cherenkov radiation detectors and in shock wave studies at high pressures, inertial confinement fusion (ICF radio-luminescent and micrometeorites. Silica gel can be prepared by using various sol gel precursors but the rice husk (RH is considered as the cheapest source for silica gel production. Rice husk is a waste product abundantly available in rice producing countries during milling of rice. This review article aims at summarizing the developments carried out so far in synthesis, properties, characterization and method of determination of silica, silica gel, silica aero-gel and silica xero-gel. The effect of synthesis parameters such as pH, temperature of burning the rice husk, acid leaching prior to formation of rice husk ash (RHA on the properties of final product are also described. The attention is also paid on the application of RH, RHA, sil-ica, silica aero-gel and silica xero-gel. Development of economically viable processes for getting rice husk silica with specific

Synthesis and characterization of α-alumina col-gel nanometric: elaboration of biomaterials nanostructured for biomedical applications

International Nuclear Information System (INIS)

Passoni, L.S.; Feit, G.; Camargo, N.H.A.

2010-01-01

The production of nanostructured biomaterials are research themes for these present new characteristics of biocompatibility and bioactivity. The sol-gel process allows obtaining α-alumina nanometric with purity 99.99%. The use of nanoparticles of Al 2 O 3 -α, SiO 2 and TiO 2 are being employed as a second stage in the development of nanocomposites biomaterials. The presence of the second phase within a ceramic matrix leads to obtaining nanomaterials with micropores in micro and nanostructures interconnected, what contributes within the processes of osseous integration, osseous induction. The goal of this work focused on synthesis and characterization of an α- alumina by sol-gel process. Characterization studies were conducted using the various techniques: X-ray diffraction, scanning electron microscopy, exploratory differential scanning calorimetry and infrared spectrometry by Fourier transforms. The preliminary results showed the attainment the nanometric α-alumina powder. (author)

Preparation and Properties of Pt-Mo Sulfide System Supported on Mesoporous Silica-Alumina

Czech Academy of Sciences Publication Activity Database

Gulková, Daniela; Vít, Zdeněk

2006-01-01

Roč. 162, - (2006), s. 489-496 ISSN 0167-2991. [International Symposium Scienctific Bases for Heterogeneous Catalysts /9./. Louvain-la-Neuve, 10.09.2006-14.09.2006] R&D Projects: GA ČR(CZ) GA104/06/0870 Institutional research plan: CEZ:AV0Z40720504 Keywords : silica-alumina * Pt-Mo * hydrotreating Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 0.307, year: 2005

Evaluation of an ambient air sampling system for tritium (as tritiated water vapor) using silica gel adsorbent columns

International Nuclear Information System (INIS)

Patton, G.W.; Cooper, A.T.; Tinker, M.R.

1995-08-01

Ambient air samples for tritium analysis (as the tritiated water vapor [HTO] content of atmospheric moisture) are collected for the Hanford Site Surface Environmental Surveillance Project (SESP) using the solid adsorbent silica gel. The silica gel has a moisture sensitive indicator which allows for visual observation of moisture movement through a column. Despite using an established method, some silica gel columns showed a complete change in the color indicator for summertime samples suggesting that breakthrough had occurred; thus a series of tests was conducted on the sampling system in an environmental chamber. The purpose of this study was to determine the maximum practical sampling volume and overall collection efficiency for water vapor collected on silica gel columns. Another purpose was to demonstrate the use of an impinger-based system to load water vapor onto silica gel columns to provide realistic analytical spikes and blanks for the Hanford Site SESP. Breakthrough volumes (V b ) were measured and the chromatographic efficiency (expressed as the number of theoretical plates [N]) was calculated for a range of environmental conditions. Tests involved visual observations of the change in the silica gel's color indicator as a moist air stream was drawn through the column, measurement of the amount of a tritium tracer retained and then recovered from the silica gel, and gravimetric analysis for silica gel columns exposed in the environmental chamber

Phospholipid Fatty Acids as Physiological Indicators of Paracoccus denitrificans Encapsulated in Silica Sol-Gel Hydrogels

Directory of Open Access Journals (Sweden)

Josef Trögl

2015-02-01

Full Text Available The phospholipid fatty acid (PLFA content was determined in samples of Paracoccus denitrificans encapsulated in silica hydrogel films prepared from prepolymerized tetramethoxysilane (TMOS. Immediately after encapsulation the total PLFA concentration was linearly proportional to the optical density (600 nm of the input microbial suspension (R2 = 0.99. After 7 days this relationship remained linear, but with significantly decreased slope, indicating a higher extinction of bacteria in suspensions of input concentration 108 cells/mL and higher. trans-Fatty acids, indicators of cytoplasmatic membrane disturbances, were below the detection limit. The cy/pre ratio (i.e., ratio of cyclopropylated fatty acids (cy17:0 + cy19:0 to their metabolic precursors (16:1ω7 + 18:1ω7, an indicator of the transition of the culture to a stationary growth-phase, decreased depending on co-immobilization of nutrients in the order phosphate buffer > mineral medium > Luria Broth rich medium. The ratio, too, was logarithmically proportional to cell concentration. These results confirm the applicability of total PLFA as an indicator for the determination of living biomass and cy/pre ratio for determination of nutrient limitation of microorganisms encapsulated in sol-gel matrices. This may be of interest for monitoring of sol-gel encapsulated bacteria proposed as optical recognition elements in biosensor construction, as well as other biotechnological applications.

Preparation and characterization of silk/silica hybrid biomaterials by sol-gel crosslinking process

Energy Technology Data Exchange (ETDEWEB)

Hou Aiqin, E-mail: aiqinhou@dhu.edu.c [National Engineering Research Center for Dyeing and Finishing of Textiles, Donghua University, 3H, 2999 North Renmin Road, Songjiang, Shanghai 201620 (China); Chen Huawei [National Engineering Research Center for Dyeing and Finishing of Textiles, Donghua University, 3H, 2999 North Renmin Road, Songjiang, Shanghai 201620 (China)

2010-03-15

The silk/silica hybrid biomaterials are synthesized by sol-gel crosslinking process. The chemical and morphological structures of silk/silica hybrids are investigated with micro-FT-IR spectra, X-ray diffraction, SEM, AFM, and DSC. The results show that the crosslinking reactions among inorganic nano-particles, fibroin and 2,4,6-tri[(2-epihydrin-3-bimethyl-ammonium)propyl]-1,3,5-triazine chloride (Tri-EBAC) take place during sol-gel process. The silk/silica hybrids form new molecular structures containing not only organic fibroin but also inorganic nano-silica particles. The inorganic particles are bounded to the fibroin through covalent bonds. The silk/silica hybrids can form excellent film with very even nanometer particles. The thermal properties of organic/inorganic hybrid are improved.

Preparation and characterization of silk/silica hybrid biomaterials by sol-gel crosslinking process

International Nuclear Information System (INIS)

Hou Aiqin; Chen Huawei

2010-01-01

The silk/silica hybrid biomaterials are synthesized by sol-gel crosslinking process. The chemical and morphological structures of silk/silica hybrids are investigated with micro-FT-IR spectra, X-ray diffraction, SEM, AFM, and DSC. The results show that the crosslinking reactions among inorganic nano-particles, fibroin and 2,4,6-tri[(2-epihydrin-3-bimethyl-ammonium)propyl]-1,3,5-triazine chloride (Tri-EBAC) take place during sol-gel process. The silk/silica hybrids form new molecular structures containing not only organic fibroin but also inorganic nano-silica particles. The inorganic particles are bounded to the fibroin through covalent bonds. The silk/silica hybrids can form excellent film with very even nanometer particles. The thermal properties of organic/inorganic hybrid are improved.

Effect of silica and water content on the glass transition of poly(ethylene glycol) monomethylether-silica gel-lithium perchlorate ormolytes

International Nuclear Information System (INIS)

Korwin, Rebecca S.; Masui, Hitoshi

2005-01-01

The effect of silica and water content on the glass transition temperature, T g , of MPEG2000-silica-LiClO 4 ormolytes was assessed by differential scanning calorimetry (DSC). The sol-gel synthesized ormolytes consisted of various amounts of poly(ethylene glycol) monomethylether (M.W. 2000 g/mol; i.e., MPEG2000) tethered to silica gel through the hydroxyl terminus via a urethane linkage. DSC features corresponding to physisorbed and hydrogen-bonded water, as well as the glass transition of the polyether, were identified. Both silica and LiClO 4 raise the T g and suppress crystallization of the polyether component. Water plasticizes the polyether and stoichiometrically solvates and sequesters Li + , thereby, lowering T g

Silica, alumina and aluminosilicates as solid stationary phases in gas chromatography

Directory of Open Access Journals (Sweden)

S. Faramawy

2016-09-01

Full Text Available Silica, alumina and Aluminosilicates of different Si/Al ratios were prepared by conventional precipitation or co-precipitation methods and then subjected to thermal treatment at 800 °C. The parent and thermally treated materials were characterized by means of FTIR, SEM and thermal analysis (DTA and TGA in order to elucidate the main structural properties. Surface textural characteristics were investigated by means of nitrogen adsorption–desorption isotherms at −196 °C. Pore size distribution curves indicated the presence of mesopores (10–150 Å exhibiting maxima at 35 Å. The maxima were shifted toward higher values by increasing the alumina content. Thermodynamic parameters, ΔH, ΔG and ΔS, were determined by means of inverse gas chromatography using n-hexane as a probe. The untreated and thermally treated materials were tested as solid stationary phases in gas chromatography. The separation efficiency of various non polar and polar compounds was explained in terms of surface texture and thermodynamic parameters.

Sol-gel preparation of Ag-silica nanocomposite with high electrical conductivity

Science.gov (United States)

Ma, Zhijun; Jiang, Yuwei; Xiao, Huisi; Jiang, Bofan; Zhang, Hao; Peng, Mingying; Dong, Guoping; Yu, Xiang; Yang, Jian

2018-04-01

Sol-gel derived noble-metal-silica nanocomposites are very useful in many applications. Due to relatively low price, higher conductivity, and higher chemical stability of silver (Ag) compared with copper (Cu), Ag-silica has gained much more research interest. However, it remains a significant challenge to realize high loading of Ag content in sol-gel Ag-silica composite with high structural controllability and nanoparticles' dispersity. Different from previous works by using multifunctional silicon alkoxide to anchor metal ions, here we report the synthesis of Ag-silica nanocomposite with high loading of Ag nanoparticles by employing acetonitrile bi-functionally as solvent and metal ions stabilizer. The electrical conductivity of the Ag-silica nanocomposite reached higher than 6800 S/cm. In addition, the Ag-silica nanocomposite could simultaneously possess high electrical conductivity and positive conductivity-temperature coefficient by properly controlling the loading content of Ag. Such behavior is potentially advantageous for high-temperature devices (like phosphoric acid fuel cells) and inhibiting the thermal-induced increase of devices' internal resistance. The strategy proposed here is also compatible with block-copolymer directed self-assembly of mesoporous material, spin-coating of film and electrospinning of nanofiber, making it more charming in various practical applications.

Silica gel matrix immobilized Chlorophyta hydrodictyon africanum ...

African Journals Online (AJOL)

Aghomotsegin

2015-08-05

Aug 5, 2015 ... The algae-silica gel adsorbent was used for batch sorption studies of a cationic dye, ... traditional methods of treating industrial effluent, these ... Author(s) agree that this article remains permanently open access under the terms of the Creative ... sodium silicate solution (v/v) and 25 mL of distilled water. With.

Adsorption Characteristics of Water and Silica Gel System for Desalination Cycle

KAUST Repository

Cevallos, Oscar R.

2012-07-01

An adsorbent suitable for adsorption desalination cycles is essentially characterized by a hydrophilic and porous structure with high surface area where water molecules are adsorbed via hydrogen bonding mechanism. Silica gel type A++ possesses the highest surface area and exhibits the highest equilibrium uptake from all the silica gels available in the market, therefore being suitable for water desalination cycles; where adsorbent’s adsorption characteristics and water vapor uptake capacity are key parameters in the compactness of the system; translated as feasibility of water desalination through adsorption technologies. The adsorption characteristics of water vapor onto silica gel type A++ over a temperature range of 30 oC to 60 oC are investigated in this research. This is done using water vapor adsorption analyzer utilizing a constant volume and variable pressure method, namely the Hydrosorb-1000 instrument by Quantachrome. The experimental uptake data is studied using numerous isotherm models, i. e. the Langmuir, Tóth, generalized Dubinin-Astakhov (D-A), Dubinin-Astakhov based on pore size distribution (PSD) and Dubinin-Serpinski (D-Se) isotherm for the whole pressure range, and for a pressure range below 10 kPa, proper for desalination cycles; isotherms type V of the International Union of Pure and Applied Chemistry (IUPAC) classification were exhibited. It is observed that the D-A based on PSD and the D-Se isotherm models describe the best fitting of the experimental uptake data for desalination cycles within a regression error of 2% and 6% respectively. All isotherm models, except the D-A based on PSD, have failed to describe the obtained experimental uptake data; an empirical isotherm model is proposed by observing the behavior of Tóth and D-A isotherm models. The new empirical model describes the water adsorption onto silica gel type A++ within a regression error of 3%. This will aid to describe the advantages of silica gel type A++ for the design of

Nanostructural control of the release of macromolecules from silica sol–gels

Science.gov (United States)

Radin, Shula; Bhattacharyya, Sanjib; Ducheyne, Paul

2013-01-01

The therapeutic use of biological molecules such as growth factors and monoclonal antibodies is challenging in view of their limited half-life in vivo. This has elicited the interest in delivery materials that can protect these molecules until released over extended periods of time. Although previous studies have shown controlled release of biologically functional BMP-2 and TGF-β from silica sol–gels, more versatile release conditions are desirable. This study focuses on the relationship between room temperature processed silica sol–gel synthesis conditions and the nanopore size and size distribution of the sol–gels. Furthermore, the effect on release of large molecules with a size up to 70 kDa is determined. Dextran, a hydrophilic polysaccharide, was selected as a large model molecule at molecular sizes of 10, 40 and 70 kDa, as it enabled us to determine a size effect uniquely without possible confounding chemical effects arising from the various molecules used. Previously, acid catalysis was performed at a pH value of 1.8 below the isoelectric point of silica. Herein the silica synthesis was pursued using acid catalysis at either pH 1.8 or 3.05 first, followed by catalysis at higher values by adding base. This results in a mesoporous structure with an abundance of pores around 3.5 nm. The data show that all molecular sizes can be released in a controlled manner. The data also reveal a unique in vivo approach to enable release of large biological molecules: the use more labile sol–gel structures by acid catalyzing above the pH value of the isoelectric point of silica; upon immersion in a physiological fluid the pores expand to reach an average size of 3.5 nm, thereby facilitating molecular out-diffusion. PMID:23643607

Synthesis of zeolite from coal fly ashes with different silica-alumina composition

Energy Technology Data Exchange (ETDEWEB)

Miki Inada; Yukari Eguchi; Naoya Enomoto; Junichi Hojo [Kyushu University, Fukuoka (Japan). Department of Chemistry and Biochemistry, Graduate School of Engineering

2005-02-01

Coal fly ashes can be converted into zeolites by hydrothermal alkaline treatment. This study focuses on the effect of Si/Al molar ratio of the fly ash source on the type of formed zeolite, which also is affected by the alkaline condition. The fly ashes were mixed with an aqueous NaOH solution and hydrothermally treated at about 100{degree}C. Zeolite Na-P1 and/or hydroxy-sodalite appeared after the treatment. Zeolite Na-P1 predominantly formed from silica-rich fly ash at a low-NaOH concentration. The cation exchange capacity of the product with a large content of zeolite Na-P1 reached a value of 300 meq/100 g. The type of the product was controlled by addition of aerosil silica or alumina. It was found that silica addition effectively enhances the formation of zeolite Na-P1, even at a high-NaOH concentration. These results were discussed on the basis of a formation mechanism of zeolite from coal fly ash through dissolution-precipitation process. 10 refs., 6 figs., 1 tab.

Vapour-phase method in the synthesis of polymer-ibuprofen sodium-silica gel composites.

Science.gov (United States)

Kierys, Agnieszka; Krasucka, Patrycja; Grochowicz, Marta

2017-11-01

The study discusses the synthesis of polymer-silica composites comprising water soluble drug (ibuprofen sodium, IBS). The polymers selected for this study were poly(TRIM) and poly(HEMA- co -TRIM) produced in the form of permanently porous beads via the suspension-emulsion polymerization method. The acid and base set ternary composites were prepared by the saturation of the solid dispersions of drug (poly(TRIM)-IBS and/or poly(HEMA- co -TRIM)-IBS) with TEOS, and followed by their exposition to the vapour mixture of water and ammonia, or water and hydrochloric acid, at autogenous pressure. The conducted analyses reveal that the internal structure and total porosity of the resulting composites strongly depend on the catalyst which was used for silica precursor gelation. The parameters characterizing the porosity of both of the acid set composites are much lower than the parameters of the base set composites. Moreover, the basic catalyst supplied in the vapour phase does not affect the ibuprofen sodium molecules, whereas the acid one causes transformation of the ibuprofen sodium into the sodium chloride and a derivative of propanoic acid, which is poorly water soluble. The release profiles of ibuprofen sodium from composites demonstrate that there are differences in the rate and efficiency of drug desorption from them. They are mainly affected by the chemical character of the polymeric carrier but are also associated with the restricted swelling of the composites in the buffer solution after precipitation of silica gel.

Vapour-phase method in the synthesis of polymer-ibuprofen sodium-silica gel composites

Directory of Open Access Journals (Sweden)

Agnieszka Kierys

2017-11-01

Full Text Available The study discusses the synthesis of polymer-silica composites comprising water soluble drug (ibuprofen sodium, IBS. The polymers selected for this study were poly(TRIM and poly(HEMA-co-TRIM produced in the form of permanently porous beads via the suspension-emulsion polymerization method. The acid and base set ternary composites were prepared by the saturation of the solid dispersions of drug (poly(TRIM-IBS and/or poly(HEMA-co-TRIM-IBS with TEOS, and followed by their exposition to the vapour mixture of water and ammonia, or water and hydrochloric acid, at autogenous pressure. The conducted analyses reveal that the internal structure and total porosity of the resulting composites strongly depend on the catalyst which was used for silica precursor gelation. The parameters characterizing the porosity of both of the acid set composites are much lower than the parameters of the base set composites. Moreover, the basic catalyst supplied in the vapour phase does not affect the ibuprofen sodium molecules, whereas the acid one causes transformation of the ibuprofen sodium into the sodium chloride and a derivative of propanoic acid, which is poorly water soluble. The release profiles of ibuprofen sodium from composites demonstrate that there are differences in the rate and efficiency of drug desorption from them. They are mainly affected by the chemical character of the polymeric carrier but are also associated with the restricted swelling of the composites in the buffer solution after precipitation of silica gel.

Spectroscopic studies of Cu ions in sol–gel derived silica matrix

Indian Academy of Sciences (India)

Unknown

Abstract. The Cu2+ ion doped silica gel matrices in monolithic shape were prepared by hydrolysis and condensation of tetraethyl orthosilicate (TEOS). The absorption, transmittance and fluorescence spectra of the gel matrices heat treated at different temperatures were monitored. The loss of water and hydroxyl group from.

Characteristics of supported nano-TiO2/ZSM-5/silica gel (SNTZS): Photocatalytic degradation of phenol

International Nuclear Information System (INIS)

Zainudin, Nor Fauziah; Abdullah, Ahmad Zuhairi; Mohamed, Abdul Rahman

2010-01-01

Photocatalytic degradation of phenol was investigated using the supported nano-TiO 2 /ZSM-5/silica gel (SNTZS) as a photocatalyst in a batch reactor. The prepared photocatalyst was characterized using XRD, TEM, FT-IR and BET surface area analysis. The synthesized photocatalyst composition was developed using nano-TiO 2 as the photoactive component and zeolite (ZSM-5) as the adsorbents, all supported on silica gel using colloidal silica gel binder. The optimum formulation of SNTZS catalyst was observed to be (nano-TiO 2 :ZSM-5:silica gel:colloidal silica gel = 1:0.6:0.6:1) which giving about 90% degradation of 50 mg/L phenol solution in 180 min. The SNTZS exhibited higher photocatalytic activity than that of the commercial Degussa P25 which only gave 67% degradation. Its high photocatalytic activity was due to its large specific surface area (275.7 m 2 /g), small particle size (8.1 nm), high crystalline quality of the synthesized catalyst and low electron-hole pairs recombination rate as ZSM-5 adsorbent was used. The SNTZS photocatalyst synthesized in this study also has been proven to have an excellent adhesion and reusability.

The analysis of silica suspensions atomization

Energy Technology Data Exchange (ETDEWEB)

Ochowiak, M., E-mail: Marek.Ochowiak@put.poznan.pl [Poznan University of Technology, Faculty of Chemical Technology, Department of Chemical Engineering and Equipment, Poznan (Poland); Broniarz-Press, L.; Woziwodzki, S. [Poznan University of Technology, Faculty of Chemical Technology, Department of Chemical Engineering and Equipment, Poznan (Poland)

2011-12-15

Highlights: Black-Right-Pointing-Pointer The correlation equation for discharge coefficient has been proposed. Black-Right-Pointing-Pointer The spray angle increases with increase in GLR until a maximum value is attained at GLR value of 0.07. Black-Right-Pointing-Pointer The equation for SMD has been proposed. Black-Right-Pointing-Pointer The C{sub D} and SMD are decreasing rapidly as GLR is increased to around 0.07 and thereafter decreasing at a slower rate. - Abstract: The paper contains the results of experimental investigation of air-water and air-silica suspension atomization process in effervescent nozzles with internal mixing obtained by the use of the digital microphotography method. In experiments the different aqueous solutions of silica Aerosil 300 of different concentration have been used. The suspensions containing up to 0.04 (kg solid particles/kg solution) have Newtonian rheological properties. The observations were carried out at liquid flow rates changed from 0.0014 to 0.011 (kg/s) and gas flow rates from 0.00015 to 0.0065 (kg/s). It corresponded to gas to liquid mass ratios (GLR) values from 0.014 to 0.46. The analysis of photos shows that the droplets which have been formed during the liquid atomization have very different sizes. The differences between characteristics of effervescent atomization for water and suspensions used have not been observed. The present study confirmed the previous reports which suggested that the small particles added to solution do not change spray characteristics. The experimental results show that C{sub D} and SMD are non-linear functions of GLR. Their values are decreasing rapidly as GLR is increased from zero to around 0.07 and thereafter decreasing at a slower rate with further increase in GLR. In the same point (GLR = 0.07) the value of {alpha} is maximal. The first regime is characteristic for bubbly flow. The second is typical of annular flow regime. Boundary between bubbly and annular flow regime is observed

Development of new microporous silica membranes for gas separation

International Nuclear Information System (INIS)

Camelia Barboiu; Alejandro Mourgues; Beatrice Sala; Serge de Perthuis; Camelia Barboiu; Alejandro Mourgues; Beatrice Sala; Anne Julbe; Jose Sanchez

2006-01-01

This paper presents the synthesis and the application of molecular sieving ceramic membranes to purify hydrogen or helium from various gas mixtures. The membranes prepared in this work consist of an ultra-microporous silica-based separative layer produced via a sol-gel process. Ultra microporous silica containing boron is synthesized by the acid catalyzed hydrolysis and condensation of tetra-ethyl-ortho-silicate in ethanol. The layer is deposited inside a tubular asymmetric alumina support with a meso-porous y alumina inner layer. The thickness of the silica layers after treatment is about 200 nm, estimated from their cross-section SEM micrographs. Ultra-microporous membranes (with pore sizes less than 0.7 nm) are thus required to get high selectivity. Such membranes enable to carry out gas separation up to 500 deg C under a transmembrane pressure lower than 8 bars. He and H 2 permeance values close to 10 -7 mol.m -2 s -1 Pa -1 are obtained, associated with ideal selectivities α(He/CO 2 ) and α(H 2 /CO 2 ) between 10 and 20 at 300 deg C. (authors)

Development of fluorocarbon/silica composites via sol/gel process

International Nuclear Information System (INIS)

Ferreira, Max P.; Maria, Daniel A.; Gomes, Luiza M.F.

2009-01-01

Fluorocarbon/silica composites have interesting physical-chemical properties, combining the great resistance to chemical products, the electric insulation, and the thermal stability of fluorine polymers with the optical, magnetic, and dielectric properties of silica. Due to the unique mechanical, thermal, and dielectric properties of fluorocarbon and silica composites, there is interest in their application in the development of fuel cells, the production of integrated circuit boards (ICB), and packages for the transportation of integrated circuits. The sol-gel process is a chemical route to prepare ceramic materials with specific properties that are hard or impossible to obtain by conventional methods. Fluorocarbon/silica composites were obtained by the sol-gel method from tetramethoxysilane - TMOS and fluorinated hydrocarbons with low molecular weight and main chains with 10 - 20 carbon atoms previously obtained from PTFE scraps irradiated with a 60 Co γ source in oxygen atmosphere with a dose of 1 MGy. Syntheses were performed in 125-mL reaction flasks in basic medium at 35 deg C and in acid medium at 60 deg C with N-N dimethylformamide as a chemical additive for drying control. After synthesis, the material was thermally treated in an oven with electronic temperature control. The monoliths obtained were characterized by Fourier transform infrared spectroscopy (FTIR), electron microprobe and by a standard nitrogen adsorption-desorption technique. (author)

Characterization of silica particles prepared via urease-catalyzed urea hydrolysis and activity of urease in sol–gel silica matrix

International Nuclear Information System (INIS)

Kato, Katsuya; Nishida, Masakazu; Ito, Kimiyasu; Tomita, Masahiro

2012-01-01

Highlights: ► Silica precipitation occurred via urease-catalytic reactions. ► Higher urease activity for silica synthesis enables mesostructure of silica–urease composites. ► Urease encapsulating in silica matrix retained high activity. - Abstract: Urease templated precipitation of silica synthesized by sol–gel chemistry produces a composite material allowing high urease activity. This study investigates the structural properties of the composite material that allow for the retention of the urease hydrolysis activity. Scanning (SEM) and transmission (TEM) electron microscopy reveal that the composite has a mesoporous structure composed of closely packed spherical structures ∼20–50 nm in diameter. Brunauer–Emmett–Teller (BET) analysis revealed that the surface area and pore volume of the composite prepared under the conditions of 50 mM urea and 25 °C is relatively high (324 m 2 /g and 1.0 cm 3 /g). These values are equivalent to those of usual mesoporous silica materials synthesized from the self-assembly of triblock copolymers as organic templates. In addition, after encapsulating in a sol–gel silica matrix, urease retained high activity (∼90% of the activity compared with native urease). Our results suggest a new method for synthesizing mesoporous silica materials with highly tunable pore sizes and shapes under mild conditions.

Sedimentation in Particulate Aqueous Suspensions as studied by means of Dielectric Time Domain Spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Pettersen, Bjoernar Hauknes

1997-12-31

Many problems in offshore oil production and multiphase transport are related to surface and colloid chemistry. This thesis applies dielectric spectroscopy as an experimental technique to study the behaviour of particle suspensions in polar media. The thesis opens with an introduction to suspensions and time domain dielectric spectroscopy. It then investigates the dielectric properties of silica and alumina dispersed in polar solvents. It is found that theoretical models can be used to calculate the volume fraction disperse phase in the suspension and that the particle sedimentation depends on the wetting of the particles, charge on the particle surface and viscosity of the solvent, and that this dependency can be measured by time domain dielectric spectroscopy. When the surface properties of silica and alumina particles were modified by coating them with a non-ionic polymer and a non-ionic surfactant, then different degrees of packing in the sedimented phase at the bottom of the sedimentation vessel occurred. Chemometrical methods on the synthesis of monodisperse silica particles were used to investigate what factors influence the particle size. It turned out that it is insufficient to consider only main variables when discussing the results of the synthesis. By introducing interaction terms, the author could explain the variation in the size of particles synthesized. The difference in the sedimentation rate of monodisperse silica particles upon variation of volume fraction particles, pH, salinity, amount of silanol groups at the particle surface and temperature was studied. The cross interactions play an important role and a model explaining the variation in sedimentation is introduced. Finally, magnetic particles dispersed in water and in an external magnetic field were used to study the impact on the sedimentation due to the induced flocculation. 209 refs., 90 figs., 9 tabs.

Characterization of the Sol-Gel Transition for Zirconia-Toughened Alumina Precursors

Science.gov (United States)

Moeti, I.; Karikari, E.; Chen, J.

1998-01-01

High purity ZTA ceramic powders with and without yttria were produced using metal alkoxide precursors. ZTA ceramic powders with varying volume percents of zirconia were prepared (7, 15, and 22%). Aluminum tri-sec butoxide, zirconium propoxide, and yttrium isopropoxide were the reagents used. Synthesis conditions were varied to control the hydrolysis and the aging conditions for the sol to gel transition. FTIR analysis and theological characterization were used to follow the structural evolution during the sol to gel transition. The greater extent of hydrolysis and the build-up of structure measured from viscoelastic properties were consistent. Heat treatment was conducted to produce submicron grain fully crystalline ZTA ceramic powders. In all experimental cases a-alumina and tetragonal zirconia phases were confirmed even in the absence of yttria.

SAXS study of silica sols, gels and glasses obtained by the sol gel process

International Nuclear Information System (INIS)

Santos, D.I. dos; Aegerter, M.A.

1988-01-01

Systematic SAXS studies have been performed at the LURE Synchrotron, Orsay, using an intense beam of point like cross-section to obtain information about the sol -> humid gel -> dried gel -> silica glass transformation. The intensity curves have been analysed in term of power law in log-log plots, whose exponent is related to mass and surface fractal dimensions of the structure. It was found that almost all phases present fractal structures and for the case of basic gels, is of hierarchical nature. The aerogels are formed by a dense matrix, with a smooth surface and exhibit a very narrow auto-similarity range that gives a mass fractal dimension. (author) [pt

Low Concentration Fe-Doped Alumina Catalysts Using Sol-Gel and Impregnation Methods: The Synthesis, Characterization and Catalytic Performance during the Combustion of Trichloroethylene

Directory of Open Access Journals (Sweden)

Carolina Solis Maldonado

2014-03-01

Full Text Available The role of iron in two modes of integration into alumina catalysts was studied at 0.39 wt% Fe and tested in trichloroethylene combustion. One modified alumina was synthesized using the sol-gel method with Fe added in situ during hydrolysis; another modification was performed using calcined alumina, prepared using the sol-gel method and impregnated with Fe. Several characterization techniques were used to study the level of Fe modification in the γ-Al2O3 phase formed and to correlate the catalytic properties during trichloroethylene (TCE combustion. The introduction of Fe in situ during the sol-gel process influenced the crystallite size, and three iron species were generated, namely, magnetite, maghemite and hematite. The impregnated Fe-alumina formed hematite and maghemite, which were highly dispersed on the γ-Al2O3 surface. The X-ray photoelectron spectra (XPS, FT-IR and Mössbauer spectroscopy analyses revealed how Fe interacted with the γ-Al2O3 lattice in both catalysts. The impregnated Fe-catalyst showed the best catalytic performance compared to the catalyst that was Fe-doped in situ by the sol-gel method; both had better catalytic activity than pure alumina. This difference in activity was correlated with the accessibility of the reactants to the hematite iron species on the surface. The chlorine poisoning for all three catalysts was less than 1.8%.

Low Concentration Fe-Doped Alumina Catalysts Using Sol-Gel and Impregnation Methods: The Synthesis, Characterization and Catalytic Performance during the Combustion of Trichloroethylene.

Science.gov (United States)

Maldonado, Carolina Solis; De la Rosa, Javier Rivera; Lucio-Ortiz, Carlos J; Hernández-Ramírez, Aracely; Barraza, Felipe F Castillón; Valente, Jaime S

2014-03-12

The role of iron in two modes of integration into alumina catalysts was studied at 0.39 wt% Fe and tested in trichloroethylene combustion. One modified alumina was synthesized using the sol-gel method with Fe added in situ during hydrolysis; another modification was performed using calcined alumina, prepared using the sol-gel method and impregnated with Fe. Several characterization techniques were used to study the level of Fe modification in the γ-Al₂O₃ phase formed and to correlate the catalytic properties during trichloroethylene (TCE) combustion. The introduction of Fe in situ during the sol-gel process influenced the crystallite size, and three iron species were generated, namely, magnetite, maghemite and hematite. The impregnated Fe-alumina formed hematite and maghemite, which were highly dispersed on the γ-Al₂O 3 surface. The X-ray photoelectron spectra (XPS), FT-IR and Mössbauer spectroscopy analyses revealed how Fe interacted with the γ-Al₂O₃ lattice in both catalysts. The impregnated Fe-catalyst showed the best catalytic performance compared to the catalyst that was Fe-doped in situ by the sol-gel method; both had better catalytic activity than pure alumina. This difference in activity was correlated with the accessibility of the reactants to the hematite iron species on the surface. The chlorine poisoning for all three catalysts was less than 1.8%.

Porous Silica Sol-Gel Glasses Containing Reactive V2O5 Groups

Science.gov (United States)

Stiegman, Albert E.

1995-01-01

Porous silica sol-gel glasses into which reactive vanadium oxide functional groups incorporated exhibit number of unique characteristics. Because they bind molecules of some species both reversibly and selectively, useful as chemical sensors or indicators or as scrubbers to remove toxic or hazardous contaminants. Materials also oxidize methane gas photochemically: suggests they're useful as catalysts for conversion of methane to alcohol and for oxidation of hydrocarbons in general. By incorporating various amounts of other metals into silica sol-gel glasses, possible to synthesize new materials with broad range of new characteristics.

Immobilization of Beauveria bassiana Lipase on Silica Gel by Physical Adsorption

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Vanessa Hitomi Sugahara

2014-12-01

Full Text Available Extracellular lipase from Beauveria bassianastrain CG481 was immobilized by using thirteen different immobilization protocols. Silica gel was chosen as the most suitable adsorbent with 94.8% of activity yield. The adsorption on silica gel did not change the optimum pH (8.5 and temperature (45ºC values of the free lipase (FL for lipolytic activity, and it showed higher activities in extreme conditions (pH 9.0 to 10.5, 60ºC. The lipase immobilized on silica gel (ILS showed enhanced stability at pH 7.0 after 120 h incubation (69.0% when compared to FL (33.3%. The thermal stability was also enhanced by immobilization at 60ºC in aqueous (64.6% and organic medium (95.1%, while FL showed only 40.6% of residual activity in aqueous medium and exhibited no activity for esterification reaction in n-heptane. The treatment of ILS with 0.8 M NaCl prevented lipase desorption while Triton X-100 (0.1% resulted the enzyme leakage. The ILS was reused for four times for esterification reaction with 80.8% of initial activity.

Extrudate versus Powder Silica Alumina as Support for Re2O7 Catalyst in the Metathesis of Seed Oil-Derivatives – A Comparison

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Bassie B. Marvey

2009-01-01

Full Text Available Self- and cross-metathesis of fatty acid methyl esters (FAMEs was investigated using a silica alumina supported Re2O7 catalyst. Although a 3 wt% Re2O7/SiO2-Al2O3/SnBu4 is already active for the metathesis of unsaturated FAMEs, the results have shown that particle size of silica alumina support has a profound influence on its activity and selectivity. Consequently, high substrate conversions coupled with improved product yields (for mono- and diesters and reaction rates were obtained upon using powder, as opposed to extrudate silica alumina as the support material. Diesters are platform compounds for the synthesis of polymers and fragrances. In this paper a comparative outline of the influence of particle size of silica alumina (extrudate versus powder on catalytic performance of a 3 wt% Re2O7/SiO2-Al2O3/SnBu4 for self- and cross-metathesis of FAMEs is made. Low surface area and diffusion constraints associated with extrudates were identified as some of the factors leading to low catalytic activity and selectivity.

Structural and optical studies of nano-structure silica gel doped with different rare earth elements, prepared by two different sol -gel techniques

International Nuclear Information System (INIS)

Battisha, I.K.; El Beyally, A.; Seliman, S.I.; El Nahrawi, A.S.

2005-01-01

Structural and optical characteristics of pure silica gel (silica-xerogel, SiO 2 ) and doped with different concentrations ranging from 1 up to 6% of some rare earth (REEs) ions such as, praseodymium Pr +3 ,and Europium Eu +3 , Erbium Er +3 and Holmium Ho +3 , ions, in the form of thin film and monolith materials were prepared by sol - gel technique, Using tetra-ethoxysilane as precursor materials, which are of particular interest for sol-gel integrated optics applications. Some structural and optical features of sol-gel derived monolith and thin films are analyzed and compared, namely the structure of nano-particle monolith and thin film silica-gel samples, based on X-ray diffraction (XRD). The types of structural information obtainable are compared in detail. It is show that the XRD spectra of a-cristobalite are obtained for the two type materials and even by doping with the four REEs ions. Optical measurements of monolith and thin films were also studied and compared, the normal transmission and specular reflection were measured. The refractive index were calculated and discussed

Preparation and characterization of multilayer mesoporous γ-alumina membrane obtained via sol-gel using new precursors

Directory of Open Access Journals (Sweden)

Tafrishi R.

2015-12-01

Full Text Available In this paper, a mesoporous γ-alumina membrane coated on a macroporous α-alumina support via sol-gel method has been reported. A crack-free γ-alumina membrane was obtained by adding PVA to the alumina solution and optimum parameters of roughness, temperature and porosity were achieved. The support was dip-coated in different solutions using two new different solvents with different particle size distributions. Using these two solvents led to the uniform distribution of pore size in the final membrane. The alumina sols showed particle size distributions in the range of 20 to 55 nm which was measured by a DLS Zeta Sizer. X-ray diffraction technique, atomic force microscopy and scanning electron microscopy were used to characterize the membrane layer. XRD and DTA data for the γ-alumina membrane showed its thermal stability up to around 600 °C. The thickness of the mesoporous γ-alumina membrane was about 4 μm with 16 nm of surface roughness and 5 nm pore size. The resultant crack-free mesoporous membrane shows that the membrane preparation procedure was optimum. In this work, it has been investigated the performance of γ-alumina membranes for single gas permeation and separation of binary gas mixtures.

Styrene grafted natural rubber reinforced by in situ silica generated via sol–gel technique

Energy Technology Data Exchange (ETDEWEB)

Sittiphan, Torpong [Program of Petrochemistry and Polymer Sciences, Faculty of Science, Chulalongkorn University, Bangkok 10330 (Thailand); Prasassarakich, Pattarapan [Department of Chemical Technology, Faculty of Science, Chulalongkorn University, Bangkok 10330 (Thailand); Poompradub, Sirilux, E-mail: sirilux.p@chula.ac.th [Department of Chemical Technology, Faculty of Science, Chulalongkorn University, Bangkok 10330 (Thailand)

2014-02-15

Highlights: • Sol–gel reaction by NR latex was the absence of use of organic solvent and base catalyst. • Well dispersed in situ formed silica particles in the rubber matrix were obtained. • In situ silica was better to improve mechanical properties of rubber vulcanizates. -- Abstract: The filling of styrene graft natural rubber (ST-GNR) with in situ formed silica was performed using the sol–gel reaction via the latex solution method. The mechanical properties of ST-GNR/NR vulcanizate were improved when using the in situ formed silica to levels higher than those obtained with the commercial ex situ formed silica filled ST-GNR/NR vulcanizates at a comparable silica content of 12 parts by weight per hundred parts of rubber. Transmission electron microscopy analysis revealed that the in situ silica particles were small (∼40 nm diameter) and well dispersed, while the commercial silica particles were larger (∼60 nm diameter) and markedly agglomerated in the rubbery matrix. The mechanical properties of the composites prepared via both the solid rubber and latex solution methods were comparable.

Synthesis of all-silica zeolites from highly concentrated gels containing hexamethonium cations

KAUST Repository

Liu, Xiaolong; Ravon, Ugo; Tuel, Alain

2012-01-01

A pure and highly crystalline all-silica EU-1 zeolite has been obtained from the crystallization of gels containing very low water contents in the presence of hexamethonium cations. Decreasing the water content in the gel down to H 2O/Si < 1

The Influence of Surface Alumina and Silica on the Photocatalytic Degradation of Organic Pollutants

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Terry A. Egerton

2013-03-01

Full Text Available Practical photocatalysis for degradation of organic pollutants must take into account the influence of other chemicals. Significant Al deposition on titania can occur at naturally occurring concentrations of dissolved Al. This paper reviews the author’s work on the influence of deliberately deposited hydrous oxides of aluminium on the behavior of a ~130 m2 g−1 rutile TiO2, and then compares the behavior of deposited alumina with that of deposited silica. On rutile some adsorbed nitrogen is infrared-active. Alumina and silica deposited on the rutile reduce, and ultimately eliminate, this infrared-active species. They also reduce photocatalytic oxidation of both propan-2-ol and dichloroacetate ion and the photocatalytic reduction of diphenyl picryl hydrazine. The surface oxides suppress charge transfer and may also reduce reactant adsorption. Quantitative measurement of TiO2 photogreying shows that the adsorbed inorganics also reduce photogreying, attributed to the capture of photogenerated conduction band electrons by Ti4+ to form Ti3+. The influence of adsorbed phosphate on photocatalysis is briefly considered, since phosphate reduces photocatalytic disinfection. In the context of classical colloid studies, it is concluded that inorganic species in water can significantly reduce photoactivity from the levels that measured in pure water.

A Comparative Study of Solvothermal and Sol-Gel-Derived Nanocrystalline Alumina Catalysts for Ethanol Dehydration

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Mingkwan Wannaborworn

2015-01-01

Full Text Available The ethanol dehydration to ethylene over alumina catalysts prepared by solvothermal and sol-gel methods was investigated. Also, a commercial alumina was used for comparison purposes. The results showed that the catalytic activity depends on the properties of catalyst derived from different preparation methods and reaction temperature. The alumina synthesized by solvothermal method exhibited the highest activity. This can be attributed to the higher surface area and larger amount of acid site, especially the ratio of weak/strong acid strength as determined by N2 physisorption and NH3-TPD studies. The solvothermal-derived catalyst exhibited an excellent performance with complete ethanol conversion and 100% selectivity to ethylene at 350°C in comparison with other ones. In addition, we further studied the catalytic dehydration of alumina catalyst modified with Fe. The presence of 10 wt.% Fe decreased both conversion and ethylene selectivity. However, the acetaldehyde selectivity apparently increased. It was related to the dehydrogenation pathway that takes place on Fe species.

Epoxy-silica hybrids by nonaqueous sol-gel process

Czech Academy of Sciences Publication Activity Database

Ponyrko, Sergii; Kobera, Libor; Brus, Jiří; Matějka, Libor

2013-01-01

Roč. 54, č. 23 (2013), s. 6271-6282 ISSN 0032-3861 R&D Projects: GA ČR GAP108/12/1459 Grant - others:AV ČR(CZ) M200500903 Institutional support: RVO:61389013 Keywords : epoxy-silica hybrid * nonaqueous sol-gel process * gelation Subject RIV: CD - Macromolecular Chemistry Impact factor: 3.766, year: 2013

Characteristics of supported nano-TiO{sub 2}/ZSM-5/silica gel (SNTZS): Photocatalytic degradation of phenol

Energy Technology Data Exchange (ETDEWEB)

Zainudin, Nor Fauziah; Abdullah, Ahmad Zuhairi [School of Chemical Engineering, Engineering Campus, Universiti Sains Malaysia, Seri Ampangan, 14300 Nibong Tebal, Penang (Malaysia); Mohamed, Abdul Rahman, E-mail: chrahman@eng.usm.my [School of Chemical Engineering, Engineering Campus, Universiti Sains Malaysia, Seri Ampangan, 14300 Nibong Tebal, Penang (Malaysia)

2010-02-15

Photocatalytic degradation of phenol was investigated using the supported nano-TiO{sub 2}/ZSM-5/silica gel (SNTZS) as a photocatalyst in a batch reactor. The prepared photocatalyst was characterized using XRD, TEM, FT-IR and BET surface area analysis. The synthesized photocatalyst composition was developed using nano-TiO{sub 2} as the photoactive component and zeolite (ZSM-5) as the adsorbents, all supported on silica gel using colloidal silica gel binder. The optimum formulation of SNTZS catalyst was observed to be (nano-TiO{sub 2}:ZSM-5:silica gel:colloidal silica gel = 1:0.6:0.6:1) which giving about 90% degradation of 50 mg/L phenol solution in 180 min. The SNTZS exhibited higher photocatalytic activity than that of the commercial Degussa P25 which only gave 67% degradation. Its high photocatalytic activity was due to its large specific surface area (275.7 m{sup 2}/g), small particle size (8.1 nm), high crystalline quality of the synthesized catalyst and low electron-hole pairs recombination rate as ZSM-5 adsorbent was used. The SNTZS photocatalyst synthesized in this study also has been proven to have an excellent adhesion and reusability.

Reproducibility of measurement of the environmental carbon-14 samples prepared by the gel suspension method

International Nuclear Information System (INIS)

Ohura, Hirotaka; Wakabayashi, Genichiro; Nakamura, Kouji; Okai, Tomio; Matoba, Masaru; Kakiuchi, Hideki; Momoshima, Noriyuki; Kawamura, Hidehisa.

1997-01-01

Simple liquid scintillation counting technique for the assay of 14 C in the environment was developed. This technique was done by using gel suspension method, in which sample preparation is very simple and requires no special equipments. The reproducibility of this technique was considered and it was shown that the gel suspension method had enough reproducibility to monitor the environmental 14 C. (author)

Thermal and Mechanical Properties of Novolac-Silica Hybrid Aerogels Prepared by Sol-Gel Polymerization in Solvent-Saturated Vapor Atmosphere

Directory of Open Access Journals (Sweden)

Mohamad Mehdi Seraji1, Seraji

2015-05-01

Full Text Available Nowadays organic–inorganic hybrid aerogel materials have attracted increasing interests due to improved thermal and mechanical properties. In the present research, initially, novolac type phenolic resin-silica hybrid gels with different solid concentrations were synthesized using sol-gel polymerization in solvent-saturatedvapor atmosphere. The hybrid gels were dried at air atmosphere through ambient drying process. This method removed the need for costly and risky supercritical drying process. The yields of the obtained hybrid aerogels increased with less shrinkage in comparison with conventional sol-gel process. The precursor of silica phase in this study was tetraethoxysilane and inexpensive novolac resin was used as a reinforcing phase. The results of FTIR analysis confirmed the simultaneous formation of silica and novolac gels in the hybrid systems. The resultant hybrid aerogels showed a nanostructure hybrid network with high porosity (above 80% and low density (below 0.25 g/cm3. Nonetheless, higher content of silica resulted in more shrinkage in the hybrid aerogel structure due to the tendency of the silica network to shrink more during gelation and drying process. The SEM images of samples exhibited a continuous network of interconnected colloidal particles formed during sol-gel polymerization with mean particle size of less than 100 nanometers. Si mapping analysis showed good distribution of silica phase throughout the hybrid structure. The results demonstrated improvements in insulation properties and thermal stability of novolac-silica aerogel with increasing the silica content. The results of compressive strength showed that the mechanical properties of samples declined with increasing the silica content.

Characterization of a humic gel synthesized from an activated epoxy silica gel

International Nuclear Information System (INIS)

Barbot, C.; Pieri, J.; Durand, J.P.; Goudard, F.; Czerwinski, K.; Vial, M.; Buckau, G.; Kim, J.I.; Moulin, V.

2002-01-01

Purified humic acid has been covalently bound on activated epoxy silica gel particles. Determination of physical properties and chemical properties was conducted in order to characterize the material at different stages of the preparation. FTIR spectra and the PEC of the surface bound humic acid is very similar to that of humic acid starting material. This shows that the humic acid was not deteriorated during the surface binding process. This humic gel can be used as an analogue for sediment associated humic acid, with the advantage that covalently bound humic acid does not desorb, and thus allows for simple species separation between non-complexed and humic bound metal ions in batch and column experiments

Thermal stability of octadecylsilane hybrid silicas prepared by grafting and sol-gel methods

International Nuclear Information System (INIS)

Brambilla, Rodrigo; Santos, Joao H.Z. dos; Miranda, Marcia S.L.; Frost, Ray L.

2008-01-01

Hybrid silicas bearing octadecylsilane groups were prepared by grafting and sol-gel (SG) methods. The effect of the preparative route on the thermal stability was evaluated by means of thermal gravimetric analysis (TGA), infrared emission spectroscopy (IRES) and, complementary, by 13 C solid-state nuclear magnetic resonance ( 13 C NMR) and matrix assisted laser deionization time of flight mass spectroscopy (MALDI-TOF-MS). Silicas prepared by the grafting route seem to be slightly more stable than those produced by the sol-gel method. This behavior seems to be associated to the preparative route, since grafting affords a liquid-like conformation, while in the case of sol-gel a highly organized crystalline chain conformation was observed

Aqueous clay suspensions stabilized by alginate fluid gels for coal spontaneous combustion prevention and control.

Science.gov (United States)

Qin, Botao; Ma, Dong; Li, Fanglei; Li, Yong

2017-11-01

We have developed aqueous clay suspensions stabilized by alginate fluid gels (AFG) for coal spontaneous combustion prevention and control. Specially, this study aimed to characterize the effect of AFG on the microstructure, static and dynamic stability, and coal fire inhibition performances of the prepared AFG-stabilized clay suspensions. Compared with aqueous clay suspensions, the AFG-stabilized clay suspensions manifest high static and dynamic stability, which can be ascribed to the formation of a robust three-dimensional gel network by AFG. The coal acceleration oxidation experimental results show that the prepared AFG-stabilized clay suspensions can improve the coal thermal stability and effectively inhibit the coal spontaneous oxidation process by increasing crossing point temperature (CPT) and reducing CO emission. The prepared low-cost and nontoxic AFG-stabilized clay suspensions, exhibiting excellent coal fire extinguishing performances, indicate great application potentials in coal spontaneous combustion prevention and control.

Challenges and Strategies in the Synthesis of Mesoporous Alumina Powders and Hierarchical Alumina Monoliths

Directory of Open Access Journals (Sweden)

Anne Galarneau

2012-02-01

Full Text Available A new rapid, very simple and one-step sol-gel strategy for the large-scale preparation of highly porous γ-Al2O3 is presented. The resulting mesoporous alumina materials feature high surface areas (400 m2 g−1, large pore volumes (0.8 mL g−1 and the ��-Al2O3 phase is obtained at low temperature (500 °C. The main advantages and drawbacks of different preparations of mesoporous alumina materials exhibiting high specific surface areas and large pore volumes such as surfactant-nanostructured alumina, sol-gel methods and hierarchically macro-/mesoporous alumina monoliths have been analyzed and compared. The most reproducible synthesis of mesoporous alumina are given. Evaporation-Induced Self-Assembly (EISA is the sole method to lead to nanostructured mesoporous alumina by direct templating, but it is a difficult method to scale-up. Alumina featuring macro- and mesoporosity in monolithic shape is a very promising material for in flow applications; an optimized synthesis is described.

Preparation of an efficient humidity indicating silica gel from rice ...

Indian Academy of Sciences (India)

Administrator

Department of Ceramic Engineering, National Institute of Technology, Rourkela 769 008, ... An efficient humidity indicating silica gel was prepared using rice husk ash as a raw material via ... white or colourless and shows no changes of colour.

Chemical stability of soda-alumina-zirconia-silica glasses to Na, Na2S4, and S

International Nuclear Information System (INIS)

Bloom, S.I.; Bradley, J.; Nelson, P.A.; Roche, M.F.

1985-01-01

Twenty-two glasses with a broad range of compositions, spanning the quaternary soda-alumina-zirconia-silica system, have been prepared to allow characterization of the various properties of the system. The glasses were characterized by their resistivities, energies of activation for conduction, and glass transition temperatures. The glasses were screened for compositions of especially high chemical stability of static corrosion tests in Na, S, and Na 2 S 4 for 1000h at 400 0 C. Among the glasses tested, the high soda glasses showed the smallest weight change after exposure to the three media. The weight change observed was comparable to that seen in the Dow borate glass and beta'' alumina

Morphology and properties of silica/novolac hybrid xerogels synthesized using sol–gel polymerization at solvent vapor-saturated atmosphere

International Nuclear Information System (INIS)

Seraji, Mohamad Mehdi; Seifi, Azadeh; Bahramian, Ahmad Reza

2015-01-01

Highlights: • Sol–gel polymerization in vapor of solvent saturated atmosphere is developed. • Highly porous novolac–silica hybrid xerogels are successfully synthesized. • Novolac–silica hybrid gel was dried in ambient condition with low shrinkage. • Required time for preparation of gel reduced from 5 days to about 5 h. • By incorporation of silica into the novolac xerogel structure, the pore size decreases. - Abstract: Highly porous novolac–silica hybrid xerogels were successfully synthesized via the novel method of sol–gel polymerization in solvent vapor-saturated atmosphere. This method removes the need for supercritical drying and yields the hybrid xerogels with reduced shrinkage in comparison with conventional sol–gel process. Tetraethoxysilane (TEOS) was used as the precursor of silica-based inorganic phase. The chemical and structural characterization of the prepared hybrid xerogels were performed by Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM) analysis, respectively. Thermal and mechanical properties of the hybrid samples were investigated by differential scanning calorimetry (DSC), and compressive strength analysis. The resultant hybrid xerogels show a nanostructured colloidal hybrid network with high porosity (above 80%) and low density (below 0.25 g cm −3 ). Si mapping images shows the good distribution of silica phase throughout the hybrid structure

Fabrication of mesoporous silica nanoparticles by sol gel method followed various hydrothermal temperature

Science.gov (United States)

Purwaningsih, Hariyati; Pratiwi, Vania Mitha; Purwana, Siti Annisa Bani; Nurdiansyah, Haniffudin; Rahmawati, Yenny; Susanti, Diah

2018-04-01

Rice husk is an agricultural waste that is potentially used as natural silica resources. Natural silica claimed to be safe in handling, cheap and can be generate from cheap resource. In this study mesoporous silica was synthesized using sodium silicate extracted from rice husk ash. This research's aim are to study the optimization of silica extraction from rice husk, characterizing mesoporous silica from sol-gel method and surfactant templating from rice husk and the effect of hydrothermal temperature on mesoporous silica nanoparticle (MSNp) formation. In this research, rice husk was extracted with sol-gel method and was followed by hydrothermal treatment; several of hydrothermal temperatures were 85°C, 100°C, 115°C, 130°C and 145° for 24 hours. X-ray diffraction analysis was identified of α-SiO2 phase and NaCl compound impurities. Scherer's analysis method for crystallite size have resulted 6.27-40.3 nm. FTIR results of silica from extraction and MSNp indicated Si-O-Si bonds on the sample. SEM result showed the morphology of the sample that has spherical shape and smooth surface. TEM result showed particle size ranged between 69,69-84,42 nm. BET showed that the pore size classified as mesoporous with pore diameter size is 19,29 nm.

Simple analytical technique for liquid scintillation counting of environmental carbon-14 using gel suspension method

International Nuclear Information System (INIS)

Okai, Tomio; Wakabayashi, Genichiro; Nagao, Kenjiro; Matoba, Masaru; Ohura, Hirotaka; Momoshima, Noriyuki; Kawamura, Hidehisa

2000-01-01

A simple analytical technique for liquid scintillation counting of environmental 14 C was developed. Commercially available gelling agent, N-lauroyl-L -glutamic -α,γ-dibutylamide, was used for the gel-formation of the samples (gel suspension method) and for the subsequent liquid scintillation counting of 14 C in the form of CaCO 3 . Our procedure for sample preparation is much simpler than that of the conventional methods and requires no special equipment. Self absorption, stability and reproducibility of gel suspension samples were investigated in order to evaluate the characteristics of the gel suspension method for 14 C activity measurement. The self absorption factor is about 70% and slightly decrease as CaCO 3 weight increase. This is considered to be mainly due to the absorption of β-rays and scintillation light by the CaCO 3 sample itself. No change of the counting rate for the gel suspension sample was observed for more than 2 years after the sample preparation. Four samples were used for checking the reproducibility of the sample preparation method. The same values were obtained for the counting rate of 24 C activity within the counting error. No change of the counting rate was observed for the 're-gelated' sample. These results show that the gel suspension method is appropriate for the 14 C activity measurement by the liquid scintillation counting method and useful for a long-term preservation of the sample for repeated measurement. The above analytical technique was applied to actual environmental samples in Fukuoka prefecture, Japan. Results obtained were comparable with those by other researchers and appear to be reasonable. Therefore, the newly developed technique is useful for the routine monitoring of environmental 14 C. (author)

Visible-light-induced hydrogen production over Pt-Eosin Y catalysts with high surface area silica gel as matrix

Energy Technology Data Exchange (ETDEWEB)

Zhang, Xiaojie [State Key Laboratory for Oxo Synthesis and Selective Oxidation, Lanzhou Institute of Chemical Physics, The Chinese Academy of Sciences, Lanzhou 730000 (China); Graduate University of the Chinese Academy of Sciences, Beijing 100101 (China); Jin, Zhiliang; Li, Shuben; Lu, Gongxuan [State Key Laboratory for Oxo Synthesis and Selective Oxidation, Lanzhou Institute of Chemical Physics, The Chinese Academy of Sciences, Lanzhou 730000 (China); Li, Yuexiang [Department of Chemistry, Nanchang University, Nanjing Road 245, Nanchang, 330047 (China)

2007-03-30

A new system for the production of hydrogen, constructed using silica gel as a matrix, Eosin Y as a photosensitizer, and Pt as a cocatalyst, has been reported. It was found that the rate of photosensitized hydrogen evolution in the presence of silica gel is enhanced about 10-fold relative to the homogeneous phase, i.e. in the absence of silica gel. The pH value of the solution and the concentration of Eosin Y have remarkable effects on the rate of hydrogen evolution. The optimal pH and concentration of Eosin Y are 7 and 3.60 x 10{sup -4} mol dm{sup -3} (E/S = 1/3) to 7.24 x 10{sup -4} mol dm{sup -3} (E/S = 1/1), respectively. Triethanolamine (TEOA) as an electron donor, the rate of hydrogen evolution and the apparent quantum efficiency in the silica gel system under visible-light irradiation ({lambda} {>=} 420 nm) can reach about 43 {mu}mol h{sup -1} and 10.4%, respectively. In addition, the roles of silica gel, Pt and TEOA, respectively; and the probable mechanism of photosensitized hydrogen evolution have been discussed. (author)

Visible-light-induced hydrogen production over Pt-Eosin Y catalysts with high surface area silica gel as matrix

Science.gov (United States)

Zhang, Xiaojie; Jin, Zhiliang; Li, Yuexiang; Li, Shuben; Lu, Gongxuan

A new system for the production of hydrogen, constructed using silica gel as a matrix, Eosin Y as a photosensitizer, and Pt as a cocatalyst, has been reported. It was found that the rate of photosensitized hydrogen evolution in the presence of silica gel is enhanced about 10-fold relative to the homogeneous phase, i.e. in the absence of silica gel. The pH value of the solution and the concentration of Eosin Y have remarkable effects on the rate of hydrogen evolution. The optimal pH and concentration of Eosin Y are 7 and 3.60 × 10 -4 mol dm -3 (E/S = 1/3) to 7.24 × 10 -4 mol dm -3 (E/S = 1/1), respectively. Triethanolamine (TEOA) as an electron donor, the rate of hydrogen evolution and the apparent quantum efficiency in the silica gel system under visible-light irradiation (λ ≥ 420 nm) can reach about 43 μmol h -1 and 10.4%, respectively. In addition, the roles of silica gel, Pt and TEOA, respectively; and the probable mechanism of photosensitized hydrogen evolution have been discussed.

Characterization of alkali silica reaction gels using Raman spectroscopy

International Nuclear Information System (INIS)

Balachandran, C.; Muñoz, J.F.; Arnold, T.

2017-01-01

The ability of Raman spectroscopy to characterize amorphous materials makes this technique ideal to study alkali silica reaction (ASR) gels. The structure of several synthetic ASR gels was thoroughly characterized using Raman Spectroscopy. The results were validated with additional techniques such as Fourier transmission infrared spectroscopy, X-ray powder diffraction and thermogravimetric analysis. The Raman spectra were found to have two broad bands in the 800 to 1200 cm −1 range and the 400 to 700 cm −1 range indicating the amorphous nature of the gel. Important information regarding the silicate polymerization was deduced from both of these spectral regions. An increase in alkali content of the gels caused a depolymerization in the silicate framework which manifested in the Raman spectra as a gradual shift of predominant peaks in both regions. The trends in silicate depolymerization were in agreement with results from a NMR spectroscopy study on similar synthetic ASR gels.

Synergistic effect of plasmacatalyst and ozone in a pulsed corona discharge reactor on the decomposition of organic pollutants in water

Energy Technology Data Exchange (ETDEWEB)

Malik, Muhammad Arif [Applied Chemistry Laboratories, PINSTECH, PO Nilore, Islamabad (Pakistan)

2003-11-01

Plasmacatalytic effects of {alpha}-alumina, {gamma}-alumina, and silica gel in a pulsed corona discharge (PCD) reactor on the decomposition of aqueous methylene blue are described. Methylene blue concentration in the effluent was reduced to 23% of the inlet concentration by PCDs in water. Under the same experimental conditions, addition of {alpha}-alumina further reduced it to 8%, {gamma}-alumina to 4%, and silica gel to below the detection limits. PCDs with silica gel were run for >100 h in a continuous flow reactor and methylene blue in the effluent remained below the detection limit. A hybrid system of plasmacatalysis and ozonation is also described. Phenol concentration in the effluent was reduced to 84% of the inlet concentration by PCDs in water. Under the same experimental conditions, addition of either silica gel or ozone further reduced it to around 35%, and simultaneous addition of silica gel and ozone to 14% of inlet concentration. Decolourization of pre-adsorbed methylene blue on silica gel has been demonstrated. Adsorption and stabilization of the chemically active species on silica gel was indicated by experimental evidence. A significant improvement in the rate of decomposition of organic pollutants in water has been realized by hybridizing plasmacatalysis and ozonation in a PCD reactor.

Synergistic effect of plasmacatalyst and ozone in a pulsed corona discharge reactor on the decomposition of organic pollutants in water

International Nuclear Information System (INIS)

Malik, Muhammad Arif

2003-01-01

Plasmacatalytic effects of α-alumina, γ-alumina, and silica gel in a pulsed corona discharge (PCD) reactor on the decomposition of aqueous methylene blue are described. Methylene blue concentration in the effluent was reduced to 23% of the inlet concentration by PCDs in water. Under the same experimental conditions, addition of α-alumina further reduced it to 8%, γ-alumina to 4%, and silica gel to below the detection limits. PCDs with silica gel were run for >100 h in a continuous flow reactor and methylene blue in the effluent remained below the detection limit. A hybrid system of plasmacatalysis and ozonation is also described. Phenol concentration in the effluent was reduced to 84% of the inlet concentration by PCDs in water. Under the same experimental conditions, addition of either silica gel or ozone further reduced it to around 35%, and simultaneous addition of silica gel and ozone to 14% of inlet concentration. Decolourization of pre-adsorbed methylene blue on silica gel has been demonstrated. Adsorption and stabilization of the chemically active species on silica gel was indicated by experimental evidence. A significant improvement in the rate of decomposition of organic pollutants in water has been realized by hybridizing plasmacatalysis and ozonation in a PCD reactor

Preparation of Cylindrical Extrudates of Mesoporous Silica-alumina without Use of Binder and Their Activity in Cracking of Cumene.

Czech Academy of Sciences Publication Activity Database

Vít, Zdeněk

2016-01-01

Roč. 23, č. 4 (2016), s. 1125-1132 ISSN 1380-2224 R&D Projects: GA ČR GAP106/11/0902 Institutional support: RVO:67985858 Keywords : mesoporous * silica-alumina * binderless exstrusion Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 1.624, year: 2016

Ternary Phase-Separation Investigation of Sol-Gel Derived Silica from Ethyl Silicate 40

Science.gov (United States)

Wang, Shengnan; Wang, David K.; Smart, Simon; Diniz da Costa, João C.

2015-01-01

A ternary phase-separation investigation of the ethyl silicate 40 (ES40) sol-gel process was conducted using ethanol and water as the solvent and hydrolysing agent, respectively. This oligomeric silica precursor underwent various degrees of phase separation behaviour in solution during the sol-gel reactions as a function of temperature and H2O/Si ratios. The solution composition within the immiscible region of the ES40 phase-separated system shows that the hydrolysis and condensation reactions decreased with decreasing reaction temperature. A mesoporous structure was obtained at low temperature due to weak drying forces from slow solvent evaporation on one hand and formation of unreacted ES40 cages in the other, which reduced network shrinkage and produced larger pores. This was attributed to the concentration of the reactive sites around the phase-separated interface, which enhanced the condensation and crosslinking. Contrary to dense silica structures obtained from sol-gel reactions in the miscible region, higher microporosity was produced via a phase-separated sol-gel system by using high H2O/Si ratios. This tailoring process facilitated further condensation reactions and crosslinking of silica chains, which coupled with stiffening of the network, made it more resistant to compression and densification. PMID:26411484

Moisture sensor based on evanescent wave light scattering by porous sol-gel silica coating

Science.gov (United States)

Tao, Shiquan; Singh, Jagdish P.; Winstead, Christopher B.

2006-05-02

An optical fiber moisture sensor that can be used to sense moisture present in gas phase in a wide range of concentrations is provided, as well techniques for making the same. The present invention includes a method that utilizes the light scattering phenomenon which occurs in a porous sol-gel silica by coating an optical fiber core with such silica. Thus, a porous sol-gel silica polymer coated on an optical fiber core forms the transducer of an optical fiber moisture sensor according to an embodiment. The resulting optical fiber sensor of the present invention can be used in various applications, including to sense moisture content in indoor/outdoor air, soil, concrete, and low/high temperature gas streams.

Sol-gel processes and materials. November 1971-October 1989 (Citations from the US Patent data base). Report for November 1971-October 1989

International Nuclear Information System (INIS)

1990-01-01

This bibliography contains citations of selected patents concerning sol-gel processes and sol-gel derived materials and products. Selected patents include sol-gel compositions, ceramic and refractory materials, fabrication of silica glass, sol-gel thin films and coatings, transparent inorganic oxide glass, luminescent quartz glass, cataylsts and catalyst supports, nuclear fuels preparation, abrasives for grinding wheels, sol-gel production of microspheres, alumina composites, photographic materials, and dental materials. (This updated bibliography contains 120 citations, 12 of which are new entries to the previous edition.)

Sol-gel processes and materials. January 1970-August 1989 (Citations from the US Patent data base). Report for January 1970-August 1989

International Nuclear Information System (INIS)

1989-09-01

This bibliography contains citations of selected patents concerning Sol-Gel processes and Sol-Gel derived materials and products. Selected patents include Sol-Gel compositions, ceramic and refractory materials, fabrication of silica glass, Sol-Gel thin films and coatings, transparent inorganic oxide glass, luminescent quartz glass, cataylsts and catalyst supports, nuclear fuels preparation, abrasives for grinding wheels, Sol-Gel production of microspheres, alumina composites, photographic materials, and dental materials. (This updated bibliography contains 108 citations, 37 of which are new entries to the previous edition.)

Preparation and use of chemically modified MCM-41 and silica gel as selective adsorbents for Hg(II) ions

International Nuclear Information System (INIS)

Puanngam, Mahitti; Unob, Fuangfa

2008-01-01

Adsorbents for Hg(II) ion extraction were prepared using amorphous silica gel and ordered MCM-41. Grafting with 2-(3-(2-aminoethylthio)propylthio)ethanamine was used to functionalize the silica. The functionalized adsorbents were characterized by nitrogen adsorption, X-ray diffraction, 13 C MAS NMR spectroscopy and thermogravimetric analysis. The adsorption properties of the modified silica gel and MCM-41 were compared using batch method. The effect of pH, stirring time, ionic strength and foreign ions were studied. The extraction of Hg(II) ions occurred rapidly with the modified MCM-41 and the optimal pH range for the extraction by the modified materials was pH 4-7. Foreign ions, especially Cl - had some effect on the extraction efficiency of the modified silica gel and the modified MCM-41. The adsorption behavior of both adsorbents could be described by a Langmuir model at 298 K, and the maximum adsorption capacity of the modified silica gel and MCM-41 at pH 3 was 0.79 and 0.70 mmol g -1 , respectively. The modified MCM-41 showed a larger Langmuir constant than that of the modified silica gel, indicating a better ability for Hg(II) ion adsorption. The results indicate that the structure of the materials affects the adsorption behavior. These materials show a potential for the application as effective and selective adsorbents for Hg(II) removal from water

Fatigue Resistance of Filled NR with PMMA-Wrapped and Rare Earth-Doped Alumina-Siloxane Gel

Institute of Scientific and Technical Information of China (English)

无

2002-01-01

Poly (methyl methacrylate) (PMMA) was used to wrap alumina-siloxane sol which was produced by water glass, aluminum nitrate and α-methacrylic acid, and as a result, alumina-siloxane gel wrapped by PMMA was obtained. Meanwhile, rare earth ions were employed to dope in the course of reaction, and the formed rare earth doped PMMA microcapsule powder was filled into natural rubber (NR). It is found through the analysis of mechanical properties that Young′s modulus universally improves and a remarkable resistance to fatigue is displayed. Retention rate of tensile strength is twice that of the controlled sample after ten thousand times of extension fatigue.

Drying kinetics and characteristics of dried gambir leaves using solar heating and silica gel dessicant

Science.gov (United States)

Hasibuan, R.; Hidayati, J.; Sundari, R.; Wicaksono, A. S.

2018-02-01

A drying combination of solar heating and silica gel dessicant has been applied to dry gambir leaves. The solar energy is captured by a collector to heat the air and the hot air is used to dry gambir leaves in a drying chamber. An exhaust fan in drying chamber assists to draw water molecules from gambir leaves accelerated by silica gel dessicant. This study has investigated the drying kinetics and drying characteristics of gambir leaves drying. In drying operation the air velocity is tuned by a PWM (pulse width modulation) controller to adjust minimum and maximum level, which is based on the rotation speed of the exhaust fan. The results show that the air velocity influenced the drying kinetics and drying characteristics of gambir leaves using solar-dessicant drying at 40 cm distance between exhaust fan and silica gel dessicant.

Radiation hardness of Ce-doped sol-gel silica fibers for high energy physics applications.

Science.gov (United States)

Cova, Francesca; Moretti, Federico; Fasoli, Mauro; Chiodini, Norberto; Pauwels, Kristof; Auffray, Etiennette; Lucchini, Marco Toliman; Baccaro, Stefania; Cemmi, Alessia; Bártová, Hana; Vedda, Anna

2018-02-15

The results of irradiation tests on Ce-doped sol-gel silica using x- and γ-rays up to 10 kGy are reported in order to investigate the radiation hardness of this material for high-energy physics applications. Sol-gel silica fibers with Ce concentrations of 0.0125 and 0.05 mol. % are characterized by means of optical absorption and attenuation length measurements before and after irradiation. The two different techniques give comparable results, evidencing the formation of a main broad radiation-induced absorption band, peaking at about 2.2 eV, related to radiation-induced color centers. The results are compared with those obtained on bulk silica. This study reveals that an improvement of the radiation hardness of Ce-doped silica fibers can be achieved by reducing Ce content inside the fiber core, paving the way for further material development.

sup(60)Co hot atom chemistry of tris(acetylacetonato) cobalt(III) adsorbed on silica gel

International Nuclear Information System (INIS)

Nishioji, H.; Sakai, Y.; Tominaga, T.

1985-01-01

The sup(60)Co hot atom reactions were studied in tris(acetylacetonato)cobalt(III) adsorbed on silica gel surface. sup(57)Fe Moessbauer spectra of tris(acetylacetonato)iron(III) in the corresponding system were also measured in order to examine the state of dispersion of complex molecules on silica gel. The retention formation processes were discussed in terms of the dependence of sup(60)Co retention on the adsorbed amount (concentration) of cobalt(III) complexes. (author)

Mullite fibres preparation by aqueous sol-gel process and activation energy of mullitization

International Nuclear Information System (INIS)

Tan Hongbin; Ding Yaping; Yang Jianfeng

2010-01-01

Mullite fibres were prepared by sol-gel process using aluminum carboxylates (ACs) and silica sol. ACs was synthesized from dissolving aluminum powder in a mixture of formic acid and oxalic acid using aluminum chloride hexahydrate as catalyst. A molar ratio of 1:2:1 for aluminum, formic acid and oxalic acid was optimized to obtain clear solution and viscous ACs sol for fibres synthesis. Thermogravimetry-differential scanning calorimetry (TG-DSC), Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), and scanning electron microscopy (SEM) analysis were used to characterize the properties of the gel and ceramic fibres. The gel fibres completely transformed to mullite at 1200 o C, with a smooth surface and uniform diameter. The activation energy for mullite formation in precursor gel fibres was determined by means of differential thermal analysis. The value obtained, E a = 741.4 kJ/mol, was lower than most data reported in the literatures, which was attributed to the silica-alumina micro-phase separation when organic acids decomposed during gel fibres heating.

Comparison of the surface ion density of silica gel evaluated via spectral induced polarization versus acid-base titration

Science.gov (United States)

Hao, Na; Moysey, Stephen M. J.; Powell, Brian A.; Ntarlagiannis, Dimitrios

2016-12-01

Surface complexation models are widely used with batch adsorption experiments to characterize and predict surface geochemical processes in porous media. In contrast, the spectral induced polarization (SIP) method has recently been used to non-invasively monitor in situ subsurface chemical reactions in porous media, such as ion adsorption processes on mineral surfaces. Here we compare these tools for investigating surface site density changes during pH-dependent sodium adsorption on a silica gel. Continuous SIP measurements were conducted using a lab scale column packed with silica gel. A constant inflow of 0.05 M NaCl solution was introduced to the column while the influent pH was changed from 7.0 to 10.0 over the course of the experiment. The SIP measurements indicate that the pH change caused a 38.49 ± 0.30 μS cm- 1 increase in the imaginary conductivity of the silica gel. This increase is thought to result from deprotonation of silanol groups on the silica gel surface caused by the rise in pH, followed by sorption of Na+ cations. Fitting the SIP data using the mechanistic model of Leroy et al. (Leroyet al., 2008), which is based on the triple layer model of a mineral surface, we estimated an increase in the silica gel surface site density of 26.9 × 1016 sites m- 2. We independently used a potentiometric acid-base titration data for the silica gel to calibrate the triple layer model using the software FITEQL and observed a total increase in the surface site density for sodium sorption of 11.2 × 1016 sites m- 2, which is approximately 2.4 times smaller than the value estimated using the SIP model. By simulating the SIP response based on the calibrated surface complexation model, we found a moderate association between the measured and estimated imaginary conductivity (R2 = 0.65). These results suggest that the surface complexation model used here does not capture all mechanisms contributing to polarization of the silica gel captured by the SIP data.

SOL-GEL SILICA-BASED Ag–Ca–P COATINGS WITH AGRESSIVE PRETREATMENT OF TITANIUM SUBSTRATE

Directory of Open Access Journals (Sweden)

ELENA BORSHCHEVA

2011-12-01

Full Text Available The aim of the experiment was the obtaining of thin silica coatings on titanium by sol-gel method, using mechanical (SiC - paper No.180 and chemical (leaching in HF pretreatments of the titanium substrates. The solutions were based on TEOS. For the sol-gel dipping process 4 different solutions were prepared: silica, silica with AgNO3 and silica + AgNO3 with brushite (CaHPO4·2H2O or monetite (CaHPO4 powders. The solutions were aged for 7 and 14 days at laboratory temperature. After sol-gel dip-coating process the samples were dried and fired. The adhesion of fired coatings was measured by tape test according to ASTM procedure and the bioactivity of the coatings was tested using in vitro test. The surfaces of the samples after firing, tape test and in vitro test were observed with the optical and electron microscopes. The firing results showed that silica-silver coatings did not change, brushite sol-gel coatings have cracked and the monetite sol-gel coatings have cracked also, but less than brushite ones. In spite of coating´s crackings, the square’s frames made on the surfaces were without any breakdowns after tape tests and the adhesion of all coatings was very good, classified by the highest grade 5. The results of in vitro tests showed that all coatings interacted with simulated body fluid (SBF. After exposition in SBF the new layer formed on substrates. In case of 7 days aged coatings containing brushite the new layer was uniform and compact. In case of 7 days aged coatings containing monetite the new layer was formed by crystals aggregated tightly together. The monetite and brushite coatings prepared from 14 days aged sol were the same as previous ones, but they were thicker. X-ray analyses after in vitro test confirmed dellaite, titanate and hydroxyapatite phases.

Influence of kinetics on the determination of the surface reactivity of oxide suspensions by acid-base titration.

Science.gov (United States)

Duc, M; Adekola, F; Lefèvre, G; Fédoroff, M

2006-11-01

The effect of acid-base titration protocol and speed on pH measurement and surface charge calculation was studied on suspensions of gamma-alumina, hematite, goethite, and silica, whose size and porosity have been well characterized. The titration protocol has an important effect on surface charge calculation as well as on acid-base constants obtained by fitting of the titration curves. Variations of pH versus time after addition of acid or base to the suspension were interpreted as diffusion processes. Resulting apparent diffusion coefficients depend on the nature of the oxide and on its porosity.

Smectic liquid crystals in anisotropic colloidal silica gels

Energy Technology Data Exchange (ETDEWEB)

Liang, Dennis [Department of Physics and Astronomy, Johns Hopkins University, Baltimore, MD 21218 (United States); Borthwick, Matthew A [Department of Physics, Massachusetts Institute of Technology, Cambridge, MA 02139 (United States); Leheny, Robert L [Department of Physics and Astronomy, Johns Hopkins University, Baltimore, MD 21218 (United States)

2004-05-19

We report x-ray scattering studies of the smectic liquid crystal octylcyano-biphenol (8CB) confined by strained colloidal silica gels. The gels, comprised of aerosil particles, possess an anisotropic structure that stabilizes long-range nematic order in the liquid crystal while introducing random field effects that disrupt the smectic transition. The short-range smectic correlations that form within this environment are inconsistent with the presence of a topologically ordered state predicted for 3D random field XY systems and are quantitatively like the correlations of smectics confined by isotropic gels. Detailed analysis reveals that the quenched disorder suppresses the anisotropic scaling of the smectic correlation lengths observed in the pure liquid crystal. These results and additional measurements of the smectic-A to smectic-C transition in 4-n-pentylphenylthiol-4'-n-octyloxybenzoate (8barS5) indicate that the observed smectic behaviour is dictated by random fields coupling directly to the smectic order while fields coupling to the nematic director play a subordinate role.

Preparation of mesoporous silica microparticles by sol-gel/emulsion route for protein release.

Science.gov (United States)

Vlasenkova, Mariya I; Dolinina, Ekaterina S; Parfenyuk, Elena V

2018-04-06

Encapsulation of therapeutic proteins into particles from appropriate material can improve both stability and delivery of the drugs, and the obtained particles can serve as a platform for development of their new oral formulations. The main goal of this work was development of sol-gel/emulsion method for preparation of silica microcapsules capable of controlled release of encapsulated protein without loss of its native structure. For this purpose, the reported in literature direct sol-gel/W/O/W emulsion method of protein encapsulation was used with some modifications, because the original method did not allow to prepare silica microcapsules capable for protein release. The particles were synthesized using sodium silicate and tetraethoxysilane as silica precursors and different compositions of oil phase. In vitro kinetics of bovine serum albumin (BSA) release in buffer (pH 7.4) was studied by Fourier transform infrared (FTIR) and fluorescence spectrometry, respectively. Structural state of encapsulated BSA and after release was evaluated. It was found that the synthesis conditions influenced substantially the porous structure of the unloaded silica particles, release properties of the BSA-loaded silica particles and structural state of the encapsulated and released protein. The modified synthesis conditions made it possible to obtain the silica particles capable of controlled release of the protein during a week without loss of the protein native structure.

Effectiveness of silica based sol-gel microencapsulation method for odorants and flavors leading to sustainable environment.

Science.gov (United States)

Ashraf, Muhammad Aqeel; Khan, Aysha Masood; Ahmad, Mushtaq; Sarfraz, Maliha

2015-01-01

Microencapsulation has become a hot topic in chemical research. Technology mainly used for control release and protection purposes. The sol-gel micro encapsulation approach for fragrance and aroma in porous silica-based materials leads to sustainable odorant and flavored materials with novel and unique beneficial properties. Sol-gel encapsulation of silica based micro particles considered economically cheap as capital investment in manufacturing is very low and environmentally friendly. Amorphous sol-gel SiO2 is non-toxic and safe, whereas the sol-gel entrapment of delicate chemicals in its inner pores results in pronounced chemical and physical stabilization of the entrapped active agents, thereby broadening the practical utilization of chemically unstable essential oils (EOs). Reviewing progress in the fabrication of diverse odorant and flavored sol-gels, shows us how different synthetic strategies are appropriate for practical application with important health and environmental benefits.

Crystallization of mixed rare earth (didymium) molybdates in silica gel

Indian Academy of Sciences (India)

Experiments on the growth of mixed rare earth (didymium—a combination of La, Nd, Pr and Sm) molybdates in silica gel medium are reported. The optimum conditions conducive for the growth of these crystals are described and discussed. Concentration programming is reported to enhance the size of crystals by two-fold; ...

Effect of Support Pretreatment Temperature on the Performance of an Iron Fischer–Tropsch Catalyst Supported on Silica-Stabilized Alumina

Directory of Open Access Journals (Sweden)

Kamyar Keyvanloo

2018-02-01

Full Text Available The effect of support material pretreatment temperature, prior to adding the active phase and promoters, on Fischer–Tropsch activity and selectivity was explored. Four iron catalysts were prepared on silica-stabilized alumina (AlSi supports pretreated at 700 °C, 900 °C, 1100 °C or 1200 °C. Addition of 5% silica to alumina made the AlSi material hydrothermally stable, which enabled the unusually high support pretreatment temperatures (>900 °C to be studied. High-temperature dehydroxylation of the AlSi before impregnation greatly reduces FeO·Al2O3 surface spinel formation by removing most of the support-surface hydroxyl groups leading to more effectively carbided catalyst. The activity increases more than four-fold for the support calcined at elevated temperatures (1100–1200 °C compared with traditional support calcination temperatures of <900 °C. This unique pretreatment also facilitates the formation of ε′-Fe2.2C rather than χ-Fe2.5C on the AlSi support, which shows an excellent correlation with catalyst productivity.

Silica- and germania-based dual-ligand sol-gel organic-inorganic hybrid sorbents combining superhydrophobicity and π-π interaction. The role of inorganic substrate in sol-gel capillary microextraction.

Science.gov (United States)

Seyyal, Emre; Malik, Abdul

2017-04-29

Principles of sol-gel chemistry were utilized to create silica- and germania-based dual-ligand surface-bonded sol-gel coatings providing enhanced performance in capillary microextraction (CME) through a combination of ligand superhydrophobicity and π-π interaction. These organic-inorganic hybrid coatings were prepared using sol-gel precursors with bonded perfluorododecyl (PF-C 12 ) and phenethyl (PhE) ligands. Here, the ability of the PF-C 12 ligand to provide enhanced hydrophobic interaction was advantageously combined with π-π interaction capability of the PhE moiety to attain the desired sorbent performance in CME. The effect of the inorganic sorbent component on microextraction performance of was explored by comparing microextraction characteristics of silica- and germania-based sol-gel sorbents. The germania-based dual-ligand sol-gel sorbent demonstrated superior CME performance compared to its silica-based counterpart. Thermogravimetric analysis (TGA) of the created silica- and germania-based dual-ligand sol-gel sorbents suggested higher carbon loading on the germania-based sorbent. This might be indicative of more effective condensation of the organic ligand-bearing sol-gel-active chemical species to the germania-based sol-gel network (than to its silica-based counterpart) evolving in the sol solution. The type and concentration of the organic ligands were varied in the sol-gel sorbents to fine-tune extraction selectivity toward different classes of analytes. Specific extraction (SE) values were used for an objective comparison of the prepared sol-gel CME sorbents. The sorbents with higher content of PF-C 12 showed remarkable affinity for aliphatic hydrocarbons. Compared to their single-ligand sol-gel counterparts, the dual-ligand sol-gel coatings demonstrated significantly superior CME performance in the extraction of alkylbenzenes, providing up to ∼65.0% higher SE values. The prepared sol-gel CME coatings provided low ng L -1 limit of detections (LOD

Development of novel biocompatible hybrid nanocomposites based on polyurethane-silica prepared by sol gel process

Energy Technology Data Exchange (ETDEWEB)

Rashti, Ali [Department of Medical Nanotechnology, School of Advanced Technologies in Medicine, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Yahyaei, Hossein [Department of Polymer Engineering and Color Technology, Amirkabir University of Technology, Tehran (Iran, Islamic Republic of); Firoozi, Saman [Department of Tissue Engineering & Regenerative Medicine, Faculty of Advanced Technologies in Medicine, Iran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Ramezani, Sara [Department of Neuroscience, School of Advanced Technologies in Medicine, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Rahiminejad, Ali [Department of Medical Nanotechnology, School of Advanced Technologies in Medicine, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Karimi, Roya [Department of Tissue Engineering and Applied Cell Science, School of Advanced Technologies in Medicine, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Farzaneh, Khadijeh [Tehran Heart Center, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Mohseni, Mohsen [Department of Polymer Engineering and Color Technology, Amirkabir University of Technology, Tehran (Iran, Islamic Republic of); Ghanbari, Hossein, E-mail: hghanbari@tums.ac.ir [Department of Medical Nanotechnology, School of Advanced Technologies in Medicine, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Tehran Heart Center, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Medical Biomaterials Research Center, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of)

2016-12-01

Due to high biocompatibility, polyurethane has found many applications, particularly in development of biomedical devices. A new nanocomposite based on thermoset polyurethane and silica nanoparticles was synthesized using sol-gel method. Sol-gel process was fulfilled in two acidic and basic conditions by using tetraethylorthosilicate (TEOS) and trimethoxyisocyanatesilane as precursors. The hybrid films characterized for mechanical and surface properties using tensile strength, contact angle, ATR-FTIR and scanning electron microscopy. Biocompatibility and cytotoxicity of the hybrids were assessed using standard MTT, LDH and TUNEL assays. The results revealed that incorporation of silica nanoparticles was significantly improved tensile strength and mechanical properties of the hybrids. Based on the contact angle results, silica nanoparticles increased hydrophilicity of the hybrids. Biocompatibility by using human lung epithelial cell line (MRC-5) demonstrated that the hybrids were significantly less cytotoxic compared to pristine polymer as tested by MTT and LDH assays. TUNEL assay revealed no signs of apoptosis in all tested samples. The results of this study demonstrated that incorporation of silica nanoparticles into polyurethane lead to the enhancement of biocompatibility, indicating that these hybrids could potentially be used in biomedical field in particular as a new coating for medical implants. - Highlights: • Nanocomposites based on polyurethane and nanosilica prepared by sol-gel method fabricated • Addition of inorganic phase improved mechanical properties. • Nanosilica prepared by sol-gel method increased hydrophilicity. • By adding nanosilica to polyurethane biocompatibility increased significantly.

Separation of pharmacologically active nitrogen-containing compounds on silica gels modified with 6,10-ionene, dextran sulfate, and gold nanoparticles

Science.gov (United States)

Ioutsi, A. N.; Shapovalova, E. N.; Ioutsi, V. A.; Mazhuga, A. G.; Shpigun, O. A.

2017-12-01

New stationary phases for HPLC are obtained via layer-by-layer deposition of polyelectrolytes and studied: (1) silica gel modified layer-by-layer with 6,10-ionene and dextran sulfate (Sorbent 1); (2) silica gel twice subjected to the above modification (Sorbent 2); and (3) silica gel modified with 6,10-ionene, gold nanoparticles, and dextran sulfate (Sorbent 3). The effect the content of the organic solvent in the mobile phase and the concentration and pH of the buffer solution have on the chromatographic behavior of several pharmacologically active nitrogen-containing compounds is studied. The sorbents are stable during the process and allow the effective separation of beta-blockers, calcium channel blockers, alpha-agonists, and antihistamines. A mixture of caffeine, nadolol, tetrahydrozoline, pindolol, orphenadrine, doxylamine, carbinoxamine, and chlorphenamine is separated in 6.5 min on the silica gel modified with 6,10-ionene, gold nanoparticles, and dextran sulfate.

Solvent cleanup using base-treated silica gel solid adsorbent

International Nuclear Information System (INIS)

Tallent, O.K.; Mailen, J.C.; Pannell, K.D.

1984-06-01

A solvent cleanup method using silica gel columns treated with either sodium hydroxide (NaOH) or lithium hydroxide (LiOH) has been investigated. Its effectiveness compares favorably with that of traditional wash methods. After treatment with NaOH solution, the gels adsorb HNO 3 , dibutyl phosphate (DBP), UO 2 2+ , Pu 4+ , various metal-ion fission products, and other species from the solvent. Adsorption mechanisms include neutralization, hydrolysis, polymerization, and precipitation, depending on the species adsorbed. Sodium dibutyl phosphate, which partially distributes to the solvent from the gels, can be stripped with water; the stripping coefficient ranges from 280 to 540. Adsorption rates are diffusion controlled such that temperature effects are relatively small. Recycle of the gels is achieved either by an aqueous elution and recycle sequence or by a thermal treatment method, which may be preferable. Potential advantages of this solvent cleanup method are that (1) some operational problems are avoided and (2) the amount of NaNO 3 waste generated per metric ton of nuclear fuel reprocessed would be reduced significantly. 19 references, 6 figures, 12 tables

Relationship between sol-gel conditions and enzyme stability: a case study with β-galactosidase/silica biocatalyst for whey hydrolysis.

Science.gov (United States)

Escobar, Sindy; Bernal, Claudia; Mesa, Monica

2015-01-01

The sol-gel process has been very useful for preparing active and stable biocatalysts, with the possibility of being reused. Especially those based on silica are well known. However, the study of the enzyme behavior during this process is not well understood until now and more, if the surfactant is involved in the synthesis mixture. This work is devoted to the encapsulation of β-galactosidase from Bacillus circulans in silica by sol-gel process, assisted by non-ionic Triton X-100 surfactant. The correlation between enzyme activity results for the β-galactosidase in three different environments (soluble in buffered aqueous reference solution, in the silica sol, and entrapment on the silica matrix) explains the enzyme behavior under stress conditions offered by the silica sol composition and gelation conditions. A stable β-galactosidase/silica biocatalyst is obtained using sodium silicate, which is a cheap source of silica, in the presence of non-ionic Triton X-100, which avoids the enzyme deactivation, even at 40 °C. The obtained biocatalyst is used in the whey hydrolysis for obtaining high value products from this waste. The preservation of the enzyme stability, which is one of the most important challenges on the enzyme immobilization through the silica sol-gel, is achieved in this study.

Fluorescent silica hybrid materials containing benzimidazole dyes obtained by sol-gel method and high pressure processing

International Nuclear Information System (INIS)

Hoffmann, Helena Sofia; Stefani, Valter; Benvenutti, Edilson Valmir; Costa, Tania Maria Haas; Gallas, Marcia Russman

2011-01-01

Research highlights: → Sol-gel technique was used to obtain silica based hybrid materials containing benzimidazole dyes. → The sol-gel catalysts, HF and NaF, produce xerogels with different optical and textural characteristics. → High pressure technique (6.0 GPa) was used to produce fluorescent and transparent silica compacts with the dyes entrapped in closed pores, maintaining their optical properties. → The excited state intramolecular proton transfer (ESIPT) mechanism of benzimidazole dyes was studied by steady-state fluorescence spectroscopy for the monoliths, powders, and compacts. - Abstract: New silica hybrid materials were obtained by incorporation of two benzimidazole dyes in the silica network by sol-gel technique, using tetraethylorthosilicate (TEOS) as inorganic precursor. Several syntheses were performed with two catalysts (HF and NaF) producing powders and monoliths with different characteristics. The dye 2-(2'-hydroxy-5'-aminophenyl)benzimidazole was dispersed and physically adsorbed in the matrix, and the dye 2'(5'-N-(3-triethoxysilyl)propylurea-2'-hydroxyphenyl)benzimidazole was silylated, becoming chemically bonded to the silica network. High pressure technique was used to produce fluorescent and transparent silica compacts with the silylated and incorporated dye, at 6.0 GPa and room temperature. The excited state intramolecular proton transfer (ESIPT) mechanism of benzimidazole dyes was studied by steady-state fluorescence spectroscopy for the monoliths, powders, and compacts. The influence of the syntheses conditions was investigated by textural analysis using nitrogen adsorption isotherms.

Effectiveness of silica based sol-gel microencapsulation method for odorants and flavors leading to sustainable environment

Science.gov (United States)

Ashraf, Muhammad Aqeel; Khan, Aysha Masood; Ahmad, Mushtaq; Sarfraz, Maliha

2015-01-01

Microencapsulation has become a hot topic in chemical research. Technology mainly used for control release and protection purposes. The sol-gel micro encapsulation approach for fragrance and aroma in porous silica-based materials leads to sustainable odorant and flavored materials with novel and unique beneficial properties. Sol-gel encapsulation of silica based micro particles considered economically cheap as capital investment in manufacturing is very low and environmentally friendly. Amorphous sol-gel SiO2 is non-toxic and safe, whereas the sol-gel entrapment of delicate chemicals in its inner pores results in pronounced chemical and physical stabilization of the entrapped active agents, thereby broadening the practical utilization of chemically unstable essential oils (EOs). Reviewing progress in the fabrication of diverse odorant and flavored sol-gels, shows us how different synthetic strategies are appropriate for practical application with important health and environmental benefits. PMID:26322304

Effectiveness of silica based Sol-gel microencapsulation Method for odorants and flavours leading to sustainable Environment

Directory of Open Access Journals (Sweden)

Muhammad Aqeel eAshraf

2015-08-01

Full Text Available Microencapsulation has become a hot topic in chemical research. Technology mainly used for control release and protection purposes. The sol–gel micro encapsulation approach for fragrance and aroma in porous silica-based materials leads to sustainable odorant and flavored materials with novel and unique beneficial properties. Sol-gel encapsulation of silica based micro particles considered economically cheap as capital investment in manufacturing is very low and environmentally friendly. Amorphous sol–gel SiO2 is non-toxic and safe, whereas the sol–gel entrapment of delicate chemicals in its inner pores results in pronounced chemical and physical stabilization of the entrapped actives, thereby broadening the practical utilization of chemically unstable essential oils. Reviewing progress in the fabrication of diverse odorant and flavoured sol-gels, shows us how different synthetic strategies are appropriate for practical application with important health and environmental benefits.

Synthesis and surface characterization of alumina-silica-zirconia nanocomposite ceramic fibres on aluminium at room temperature

Energy Technology Data Exchange (ETDEWEB)

Mubarak Ali, M., E-mail: masterscience2003@yahoo.co.in [Advanced Materials Research Laboratory, Department of Chemistry, Periyar University, Omalur Main Road, Salem 636 011, Tamil Nadu (India); Raj, V., E-mail: alaguraj2@rediffmail.com [Advanced Materials Research Laboratory, Department of Chemistry, Periyar University, Omalur Main Road, Salem 636 011, Tamil Nadu (India)

2010-04-01

Alumina-silica-zirconia nanocomposite (ASZNC) ceramic fibres were synthesized by conventional anodization route. Scanning Electron Microscopy (SEM), Atomic Force microscopy (AFM), X-Ray Diffraction (XRD) and Energy Dispersive X-Ray spectroscopy (EDAX) were used to characterize the morphology and crystalloid structure of ASZNC fibres. Current density (DC) is one of the important parameters to get the alumina-silica-zirconia nanocomposite (ASZNC) ceramic fibres by this route. Annealing of the films exhibited a drastic change in the properties due to improved crystallinity. The root mean square roughness of the sample observed from atomic force microscopic analysis is about 71.5 nm which is comparable to the average grain size of the coatings which is about 72 nm obtained from X-Ray diffraction. The results indicate that, the ASZNC fibres are arranged well in the nanostructure. The thickness of the coating increased with the anodizing time, but the coatings turned rougher and more porous. At the initial stage the growth of ceramic coating increases inwards to the metal substrate and outwards to the coating surface simultaneously. Subsequently, it mainly grows towards the metal substrate and the density of the ceramic coating increases gradually, which results in the decrease of the total thickness as anodizing time increases. This new approach of preparing ASZNC ceramic fibres may be important in applications ranging from gas sensors to various engineering materials.

Sol-gel derived flexible silica aerogel as selective adsorbent for water decontamination from crude oil.

Science.gov (United States)

Abolghasemi Mahani, A; Motahari, S; Mohebbi, A

2018-04-01

Oil spills are the most important threat to the sea ecosystem. The present study is an attempt to investigate the effects of sol-gel parameters on seawater decontamination from crude oil by use of flexible silica aerogel. To this goal, methyltrimethoxysilane (MTMS) based silica aerogels were prepared by two-step acid-base catalyzed sol-gel process, involving ambient pressure drying (APD) method. To investigate the effects of sol-gel parameters, the aerogels were prepared under two different acidic and basic pH values (i.e. 4 and 8) and varied ethanol/MTMS molar ratios from 5 to 15. The adsorption capacity of the prepared aerogels was evaluated for two heavy and light commercial crude oils under multiple adsorption-desorption cycles. To reduce process time, desorption cycles were carried out by using roll milling for the first time. At optimum condition, silica aerogels are able to uptake heavy and light crude oils with the order of 16.7 and 13.7, respectively. Copyright © 2017 Elsevier Ltd. All rights reserved.

Adsorption Characteristics of Water and Silica Gel System for Desalination Cycle

KAUST Repository

Cevallos, Oscar R.

2012-01-01

(D-Se) isotherm for the whole pressure range, and for a pressure range below 10 kPa, proper for desalination cycles; isotherms type V of the International Union of Pure and Applied Chemistry (IUPAC) classification were exhibited. It is observed that the D-A based on PSD and the D-Se isotherm models describe the best fitting of the experimental uptake data for desalination cycles within a regression error of 2% and 6% respectively. All isotherm models, except the D-A based on PSD, have failed to describe the obtained experimental uptake data; an empirical isotherm model is proposed by observing the behavior of Tóth and D-A isotherm models. The new empirical model describes the water adsorption onto silica gel type A++ within a regression error of 3%. This will aid to describe the advantages of silica gel type A++ for the design of adsorption desalination processes where reducing capital cost and footprint area are highly important parameters to take into account.

Seeding technique for lowering temperature during synthesis of α-alumina

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Yoshio Kobayashi

2015-03-01

Full Text Available This paper reports a method for producing α-Al2O3 at low temperature using a seeding technique. A white product obtained by hydrolyzing aluminum isopropoxide in water at 80 °C was peptized using acetic acid at 80 °C, which transformed the white product to a transparent alumina sol. α-Al2O3 particles were added to the alumina sol as seed material; the sol containing α-Al2O3 particles was then transformed to an α-Al2O3-seeded alumina gel by drying the sol at room temperature. The non-seeded alumina gel remained boehmite after annealing at 300 °C and crystallized into γ-Al2O3 and α-Al2O3 at temperatures between 300 and 500 °C and between 900 and 1100 °C, respectively. The α-Al2O3 seeding promoted crystallization of the alumina gel into α-Al2O3. The promotion of crystallization was significant with an increase in α-Al2O3 particle content by weight in the final seeded alumina gel. With an α-Al2O3 particle content of 5%, the seeded alumina gel was partially crystallized into α-Al2O3 by annealing at a temperature as low as 900 °C.

The influence of the matrix structure on the oxidation of aniline in a silica sol-gel composite

International Nuclear Information System (INIS)

Widera, J.; Kijak, A.M.; Ca, D.V.; Pacey, G.E.; Taylor, R.T.; Perfect, H.; Cox, J.A.

2005-01-01

Mesoporous and microporous silica matrices were formed on indium tin oxide electrodes for liquid-phase voltammetry and as monoliths for solid-state voltammetry of aniline. The pore structure, which was verified by scanning probe microscopy and by surface area measurement, was directed by either control of pH during sol-gel processing or by inclusion of a templating agent. Whether aniline was included as a dopant in the sol-gel or as a component of the contacting liquid, the pore size influenced the coupling of the product of its electrochemical oxidation. With microporous silica, the dominant products were dimers and related short-chain products whereas with mesoporous silica, polymerization was suggested. As a step toward the formation of polyaniline (PANI) that is covalently anchored to the sol-gel, the electrochemistry of aniline was investigated using composites prepared from sols comprising tetraethyl orthosilicate (TEOS), 3-aminophenyl-[3-triethoxylsilyl)-propyl] urea (ormosil), and aniline in various ratios. Combinatorial chemistry identified that the optimum combination of silica precursors in terms of obtaining PANI was a 1:12 mole ratio of ormosil:TEOS

In vitro⿿in vivo performance of bare and drug loaded silica gel synthesized via optimized process parameters

Science.gov (United States)

Chakraborty, Suparna; Biswas, Supratim

2016-01-01

Silica xerogel as a potential drug carrier system for the in vivo as well as in vitro delivery of andrographolide was tested. The present study aims to optimize the effective experimental parameters; volume of ethanol, volume of water and drying temperature by applying response surface methodology coupled with Box⿿Behnken experimental design. The in vitro drug release in simulated body fluid at 37 οC from the selected formulation was significantly highest (44.83 ± 0.9%) among rest of the formulations. Results indicate that sol⿿gel method is useful for entrapping andrographolide in the silica gel and for releasing the same via diffusion through the porous matrix under the in vitro/in vivo conditions. Silica gel exhibited slow matrix degradation as well as sustained release of andrographolide within the experimental time frame of 168 h. In vivo study was performed with three increasing doses [2 mg (S1), 8 mg (S2), and 16 mg (S3)] of silica. Histological fates of different organs were executed with those doses.

Preparation of Nano Activated γ-Alumina ( with Surfactant and Surface Characterization

Directory of Open Access Journals (Sweden)

Enas Sameer AL-Khawaja

2016-09-01

Full Text Available This paper deals with the preparation of Alumina by sol-gel technique through the hydrolysis of aluminum ion mixed with the glucose as a surfactant and converting it to gel by ammonium hydroxide in aqueous media. The resulting sol composed of particle is draying to become a transparent gel. The freshly prepared gel is heated at 700°C for 2hrs to obtain alumina ( particles. The obtained particles are found to be γ-alumina particles with high porosity, Their characteristics are determined by LPSA, XRD, SEM, TEM and BET techniques. The results show that the particles are pure alumina, nano-sized=20nm, spherical shape, high surface area=210 /gm.

Adsorption isotope effects of water on mesoporous silica and alumina with implications for the land-vegetation-atmosphere system

Science.gov (United States)

Lin, Ying; Horita, Juske; Abe, Osamu

2018-02-01

Soil water dynamics within a vadose (unsaturated) zone is a key component in the hydrologic cycle, especially in arid regions. In applying the Craig-Gordon evaporation model to obtain isotopic compositions of soil water and the evaporated vapor in land-surface models (LSMs), it has been assumed that the equilibrium isotope fractionation factors between soil water and water vapor, α(2H) and α(18O), are identical to those between liquid and vapor of bulk water. Isotope effects in water condensation arise from intermolecular hydrogen bonding in the condensed phase and the appearance of hindered rotation/translation. Hydrogen bonding between water molecules and pore surface hydroxyl groups influences adsorption isotope effects. To test whether equilibrium fractionation factors between soil water and water vapor are identical to those between liquid and vapor of bulk water and to evaluate the influence of pore size and chemical composition upon adsorption isotope effects, we extended our previous experiments of a mesoporous silica (15 nm) to two other mesoporous materials, a silica (6 nm) and an alumina (5.8 nm). Our results demonstrated that α(2H) and α(18O) between adsorbed water and water vapor are 1.057 and 1.0086 for silica (6 nm) and 1.041 and 1.0063 for alumina (5.8 nm), respectively, at saturation pressure (po), which are smaller than 1.075 and 1.0089, respectively, between liquid and vapor phases of free water at 30 °C and that the differences exaggerate at low water contents. However, the profiles of α values with relative pressures (p/po) for these three materials differ due to the differences in chemical compositions and pore sizes. Empirical formula relating α(2H) and α(18O) values to the proportions of filled pores (f) are developed for potential applications to natural soils. Our results from triple oxygen isotope analyses demonstrated that the isotope fractionation does not follow a canonical law. For the silica (15 nm), fractionation exponents

Highly fluorescent silver nanoclusters in alumina-silica composite optical fiber

Energy Technology Data Exchange (ETDEWEB)

Halder, A.; Chattopadhyay, R.; Majumder, S.; Paul, M. C.; Das, S.; Bhadra, S. K., E-mail: skbhadra@cgcri.res.in [Fiber Optics and Photonics Division, CSIR-Central Glass and Ceramic Research Institute, 196, Raja S. C. Mullick Road, Kolkata 700032 (India); Bysakh, S.; Unnikrishnan, M. [Material Characterization Division, CSIR-Central Glass and Ceramic Research Institute, 196, Raja S. C. Mullick Road, Kolkata 700032 (India)

2015-01-05

An efficient visible fluorescent optical fiber embedded with silver nanoclusters (Ag-NCs) having size ∼1 nm, uniformly distributed in alumina-silica composite core glass, is reported. Fibers are fabricated in a repetitive controlled way through modified chemical vapour deposition process associated with solution doping technique. Fibers are drawn from the transparent preforms by conventional fiber drawing process. Structural characteristics of the doped fibers are studied using transmission electron microscopy and electron probe micro analysis. The oxidation state of Ag within Ag-NCs is investigated by X-ray photo electron spectroscopy. The observed significant fluorescence of the metal clusters in fabricated fibers is correlated with electronic model. The experimentally observed size dependent absorption of the metal clusters in fabricated fibers is explained with the help of reported results calculated by ab-initio density functional theory. These optical fibers may open up an opportunity of realizing tunable wavelength fiber laser without the help of rare earth elements.

Thermal and Hydrothermal Treatment of Silica Gels as Solid Stationary Phases in Gas Chromatography

Directory of Open Access Journals (Sweden)

Ashraf Yehia El-Naggar

2013-01-01

Full Text Available Silica gel was prepared and treated thermally and hydrothermally and was characterized as solid stationary phase in gas chromatography. The characteristics have been evaluated in terms of polarity, selectivity, and separation efficiencies. These parameters were used to assess the outer silica surface contributions and the degree of surface deactivation brought about by different treatment techniques. The parent silica elutes the paraffinic hydrocarbons with high efficiency of separation and elutes aromatic hydrocarbons with nearly good separation and has bad separation of alcohols. The calcined silica at 500°C and 1000°C has a pronounced effect on the separation of aromatic hydrocarbons compared with the parent silica and hydrothermal treatment of silica. With respect to alcohols separation, the obtained bad separations using treated and untreated silica reflect the little effect of the thermal and hydrothermal treatment on the silica surface deactivation.

Silica Gel Behavior Under Different EGS Chemical And Thermal Conditions: An Experimental Study

International Nuclear Information System (INIS)

Hunt, J.D.; Ezzedine, S.M.; Bourcier, W.; Roberts, S.

2012-01-01

Fractures and fracture networks are the principal pathways for migration of water and contaminants in groundwater systems, fluids in enhanced geothermal systems (EGS), oil and gas in petroleum reservoirs, carbon dioxide leakage from geological carbon sequestration, and radioactive and toxic industrial wastes from underground storage repositories. When dealing with EGS fracture networks, there are several major issues to consider, e.g., the minimization of hydraulic short circuits and losses of injected geothermal fluid to the surrounding formation, which in turn maximize heat extraction and economic production. Gel deployments to direct and control fluid flow have been extensively and successfully used in the oil industry for enhanced oil recovery. However, to the best of our knowledge, gels have not been applied to EGS to enhance heat extraction. In-situ gelling systems can either be organic or inorganic. Organic polymer gels are generally not thermostable to the typical temperatures of EGS systems. Inorganic gels, such as colloidal silica gels, however, may be ideal blocking agents for EGS systems if suitable gelation times can be achieved. In the current study, we explore colloidal silica gelation times and rheology as a function of SiO 2 concentration, pH, salt concentration, and temperature, with preliminary results in the two-phase field above 100 C. Results at 25 C show that it may be possible to choose formulations that will gel in a reasonable and predictable amount of time at the temperatures of EGS systems.

Potentiometric detection of silver (I) ion based on carbon paste electrode modified with diazo-thiophenol-functionalized nanoporous silica gel

International Nuclear Information System (INIS)

Zhang Ting; Chai Yaqin; Yuan Ruo; Guo Junxiang

2012-01-01

For the first time, triazene compound functionalized silica gel was incorporated into carbon paste electrode for the potentiometric detection of silver (I) ion. A novel diazo-thiophenol-functionalized silica gel (DTPSG) was synthesized, and the presence of DTPSG acted as not only a paste binder, but also a reactive material. The electrode with optimum composition, exhibited an excellent Nernstian response to Ag + ion ranging from 1.0 × 10 −6 to 1.0 × 10 −1 M with a detection limit of 9.5 × 10 −7 M and a slope of 60.4 ± 0.2 mV dec −1 over a wide pH range (4.0–9.0) with a fast response time (50 s) at 25 °C. The electrode also showed a long-time stability, high selectivity and reproducibility. The response mechanism of the proposed electrode was investigated by using AC impedance. Moreover, the electrode was successfully applied for the determination of silver ions in radiology films, and for potentiometric titration of the mixture solution of Cl − and Br − ions. - Highlights: ► Functionalized silica gels have become promising materials. ► This work is the first attempt to apply triazene functionalized silica gel. ► The Functionalized silica gels were used to detect silver. ► The response of the previously reported papers are compared with this work. ► The result indicates the proposed electrode is better than reported Ag + electrodes.

Fabrication of Meso-Porous Gamma-Alumina Films by Sol-Gel and Gel Casting Processes for Making Moisture Sensors

Directory of Open Access Journals (Sweden)

Kalyan Kumar Mistry

2007-04-01

Full Text Available Meso-porous g-Al2O3 film may be used as a highly sensitive trace moisture sensor. The crack-free alumina film was developed using a combination of sol-gel and tape casting processes, which produce high porosity, high surface area and small pore dimensions in the range of few nano-meter at uniform distribution. Sol-gel processes are well known in nano-technology and nano-material preparation, but it is difficult to make crack-free thick or thin films using this method. Tape cast methods are used for the fabrication of flexible crack-free thick ceramic sheets. Our objective was to develop nano-structured, crack-free, transparent Al2O3 film a few microns thick, has a highly porous and stable crystallographic nature. A metallic paste was printed by screen printing on both side of the film surface for electrodes to form a sensitive element. A silver wire (dia j=0.1mm lead was connected to a grid structure electrode using a silver paste spot for fine joining. Alumina is absorbs moisture molecules into its meso-porous layer and changes its electrical characteristics according to the moisture content, its dielectric constant increase as moisture increase. Moisture molecules can be conceived of as dipoles in random state before the application of an electric field. When the dipole orientation was changed from random to an equilibrium state under the application of external field, a large change in dielectric constant was observed. The number of water molecules absorbed determines the electrical impedance of the capacitor, which in turn is proportional to water vapor pressure.

Enhancement of aromatic and saturated hydrocarbon by modified ...

African Journals Online (AJOL)

Three sediment samples collected from the Qua Iboe River System and eighteen different column packing ratios of silica gel and alumina were used in this investigation. The variation of the composition of the stationary phase (silica gel and alumina, SA) gave different yields of aromatic and saturated hydrocarbons. In all the ...

Phase equilibria and thermodynamic modeling of ethane and propane hydrates in porous silica gels.

Science.gov (United States)

Seo, Yongwon; Lee, Seungmin; Cha, Inuk; Lee, Ju Dong; Lee, Huen

2009-04-23

In the present study, we examined the active role of porous silica gels when used as natural gas storage and transportation media. We adopted the dispersed water in silica gel pores to substantially enhance active surface for contacting and encaging gas molecules. We measured the three-phase hydrate (H)-water-rich liquid (L(W))-vapor (V) equilibria of C(2)H(6) and C(3)H(8) hydrates in 6.0, 15.0, 30.0, and 100.0 nm silica gel pores to investigate the effect of geometrical constraints on gas hydrate phase equilibria. At specified temperatures, the hydrate stability region is shifted to a higher pressure region depending on pore size when compared with those of bulk hydrates. Through application of the Gibbs-Thomson relationship to the experimental data, we determined the values for the C(2)H(6) hydrate-water and C(3)H(8) hydrate-water interfacial tensions to be 39 +/- 2 and 45 +/- 1 mJ/m(2), respectively. By using these values, the calculation values were in good agreement with the experimental ones. The overall results given in this study could also be quite useful in various fields, such as exploitation of natural gas hydrate in marine sediments and sequestration of carbon dioxide into the deep ocean.

Surface Behavior of Rhodamin and Tartrazine on Silica-Cellulose Sol-Gel Surfaces by Thin Layer Elution

Directory of Open Access Journals (Sweden)

Surjani Wonorahardjo

2016-05-01

Full Text Available Physical and chemical interactions are the principles for different types of separation systems as the equillibrium dynamics on surface plays a key-role. Surface modification is a way for selective separation at interfaces. Moreover, synthesis of gel silica by a sol-gel method is preferred due to the homogeneity and surface feature easily controlled. Cellulose can be added in situ to modified the silica features during the process. Further application for to study interaction of rhodamin and tartrazine in its surface and their solubilities in mobile phase explains the possibility for their separation. This paper devoted to evaluate the surface behavior in term of adsorption and desorption of tartrazine and rhodamin on silica-cellulose thin layer in different mobile phase. Some carrier liquids applied such as methanol, acetone, n-hexane and chloroform. The result proves tartrazine and rhodamin is separated and have different behavior in different mobile phase. The retardation factors (Rf of the mixtures suggest complexity behavior on silica-cellulose surface.

Sol-gel-derived mesoporous silica films with low dielectric constants

Energy Technology Data Exchange (ETDEWEB)

Seraji, S.; Wu, Yun; Forbess, M.; Limmer, S.J.; Chou, T.; Cao, Guozhong [Washington Univ., Seattle, WA (United States). Dept. of Materials Science and Engineering

2000-11-16

Mesoporous silica films with low dielectric constants and possibly closed pores have been achieved with a multiple step sol-gel processing technique. Crack-free films with approximately 50% porosity and 0.9 {mu}m thicknesses were obtained, a tape-test revealing good adhesion between films and substrates or metal electrodes. Dielectric constants remained virtually unchanged after aging at room temperature at 56% humidity over 6 days. (orig.)

Thickness controlled sol-gel silica films for plasmonic bio-sensing devices

Energy Technology Data Exchange (ETDEWEB)

Figus, Cristiana, E-mail: cristiana.figus@dsf.unica.it; Quochi, Francesco, E-mail: cristiana.figus@dsf.unica.it; Artizzu, Flavia, E-mail: cristiana.figus@dsf.unica.it; Saba, Michele, E-mail: cristiana.figus@dsf.unica.it; Marongiu, Daniela, E-mail: cristiana.figus@dsf.unica.it; Mura, Andrea; Bongiovanni, Giovanni [Dipartimento di Fisica - University of Cagliari, S.P. Km 0.7, I-09042 Monserrato (Canada) (Italy); Floris, Francesco; Marabelli, Franco; Patrini, Maddalena; Fornasari, Lucia [Dipartimento di Fisica - University of Pavia, Via Agostino Bassi 6, I-27100 Pavia (PV) (Italy); Pellacani, Paola; Valsesia, Andrea [Plasmore S.r.l. -Via Grazia Deledda 4, I-21020 Ranco (Vatican City State, Holy See) (Italy)

2014-10-21

Plasmonics has recently received considerable interest due to its potentiality in many fields as well as in nanobio-technology applications. In this regard, various strategies are required for modifying the surfaces of plasmonic nanostructures and to control their optical properties in view of interesting application such as bio-sensing, We report a simple method for depositing silica layers of controlled thickness on planar plasmonic structures. Tetraethoxysilane (TEOS) was used as silica precursor. The control of the silica layer thickness was obtained by optimizing the sol-gel method and dip-coating technique, in particular by properly tuning different parameters such as pH, solvent concentration, and withdrawal speed. The resulting films were characterized via atomic force microscopy (AFM), Fourier-transform (FT) spectroscopy, and spectroscopic ellipsometry (SE). Furthermore, by performing the analysis of surface plasmon resonances before and after the coating of the nanostructures, it was observed that the position of the resonance structures could be properly shifted by finely controlling the silica layer thickness. The effect of silica coating was assessed also in view of sensing applications, due to important advantages, such as surface protection of the plasmonic structure.

Adjustable rheology of fumed silica dispersion in urethane prepolymers: Composition-dependent sol and gel behaviors and energy-mediated shear responses

Energy Technology Data Exchange (ETDEWEB)

Zheng, Zhong, E-mail: 11329038@zju.edu.cn; Song, Yihu, E-mail: s-yh0411@zju.edu.cn; Wang, Xiang, E-mail: 11229036@zju.edu.cn; Zheng, Qiang, E-mail: zhengqiang@zju.edu.cn [MOE Key Laboratory of Macromolecule Synthesis and Functionalization, Department of Polymer Science and Engineering, Zhejiang University, Hangzhou 310027 (China)

2015-07-15

Variation of colloidal and interfacial interactions leads to a microstructural diversity in fumed silica dispersions exhibiting absolutely different sol- or gel-like rheological responses. In this study, fumed silicas with different surface areas (200–400 m{sup 2}/g) and surface characteristics (hydrophilic or hydrophobic) are dispersed into moisture-cured polyurethane. The microstructures investigated using transmission electron microscope are associated perfectly with three different rheological behaviors: (i) Sols with well-dispersed silica aggregates, (ii) weak gels with agglomerate-linked networks, and (iii) strong gels with concentrated networks of large agglomerates. Though sols and gels are well distinguished by shear thickening or sustained thinning response through steady shear flow test, it is interesting that the sols and weak gels exhibit a uniform modulus plateau-softening-hardening-softening response with increasing dynamic strain at frequency 10 rad s{sup −1} while the strong gels show a sustained softening beyond the linear regime. Furthermore, the onset of softening and hardening can be normalized: The two softening are isoenergetic at mechanical energies of 0.3 J m{sup −3} and 10 kJ m{sup −3}. On the other hand, the hardening is initiated by a critical strain of 60%. The mechanisms involved in the generation of the sol- and the gel-like dispersions and their structural evolutions during shear are thoroughly clarified in relation to the polyols, the characteristic and content of silica and the curing catalysts.

Potentiometric detection of silver (I) ion based on carbon paste electrode modified with diazo-thiophenol-functionalized nanoporous silica gel

Energy Technology Data Exchange (ETDEWEB)

Zhang Ting; Chai Yaqin, E-mail: yqchai@swu.edu.cn; Yuan Ruo; Guo Junxiang

2012-07-01

For the first time, triazene compound functionalized silica gel was incorporated into carbon paste electrode for the potentiometric detection of silver (I) ion. A novel diazo-thiophenol-functionalized silica gel (DTPSG) was synthesized, and the presence of DTPSG acted as not only a paste binder, but also a reactive material. The electrode with optimum composition, exhibited an excellent Nernstian response to Ag{sup +} ion ranging from 1.0 Multiplication-Sign 10{sup -6} to 1.0 Multiplication-Sign 10{sup -1} M with a detection limit of 9.5 Multiplication-Sign 10{sup -7} M and a slope of 60.4 {+-} 0.2 mV dec{sup -1} over a wide pH range (4.0-9.0) with a fast response time (50 s) at 25 Degree-Sign C. The electrode also showed a long-time stability, high selectivity and reproducibility. The response mechanism of the proposed electrode was investigated by using AC impedance. Moreover, the electrode was successfully applied for the determination of silver ions in radiology films, and for potentiometric titration of the mixture solution of Cl{sup -} and Br{sup -} ions. - Highlights: Black-Right-Pointing-Pointer Functionalized silica gels have become promising materials. Black-Right-Pointing-Pointer This work is the first attempt to apply triazene functionalized silica gel. Black-Right-Pointing-Pointer The Functionalized silica gels were used to detect silver. Black-Right-Pointing-Pointer The response of the previously reported papers are compared with this work. Black-Right-Pointing-Pointer The result indicates the proposed electrode is better than reported Ag{sup +} electrodes.

Silica doped with lanthanum sol–gel thin films for corrosion protection

International Nuclear Information System (INIS)

Abuín, M.; Serrano, A.; Llopis, J.; García, M.A.; Carmona, N.

2012-01-01

We present here anticorrosive silica coatings doped with lanthanum ions for the protection of metallic surfaces as an alternative to chromate (VI)-based conversion coatings. The coatings were synthesized by the sol–gel method starting from silicon alkoxides and two different lanthanum precursors: La (III) acetate hydrate and La (III) isopropoxide. Artificial corrosion tests in acid and alkaline media showed their effectiveness for the corrosion protection of AA2024 aluminum alloy sheets for coating prepared with both precursors. The X-ray absorption Near Edge Structure and X-ray Absorption Fine Structure analysis of the coatings confirmed the key role of lanthanum in the structural properties of the coating determining its anticorrosive properties. - Highlights: ► Silica sol–gel films doped with lanthanum ions were synthesized. ► Films from lanthanum-acetate and La-alkoxide were prepared for comparison purposes. ► La-acetate is an affordable chemical reactive preferred for the industry. ► Films properties were explored by scanning electron microscopy and X-Ray absorption spectroscopy. ► An alternative to anticorrosive pre-treatments for metallic surfaces is suggested.

Designing robust alumina nanowires-on-nanopores structures: superhydrophobic surfaces with slippery or sticky water adhesion.

Science.gov (United States)

Peng, Shan; Tian, Dong; Miao, Xinrui; Yang, Xiaojun; Deng, Wenli

2013-11-01

Hierarchical alumina surfaces with different morphologies were fabricated by a simple one-step anodization method. These alumina films were fabricated by a new raw material: silica gel plate (aluminum foil with a low purity of 97.17%). The modulation of anodizing time enabled the formation of nanowires-on-nanopores hybrid nanostructures having controllable nanowires topographies through a self-assembly process. The resultant structures were demonstrated to be able to achieve superhydrophobicity without any hydrophobic coating layer. More interestingly, it is found that the as-prepared superhydrophobic alumina surfaces exhibited high contrast water adhesion. Hierarchical alumina film with nanowire bunches-on-nanopores (WBOP) morphology presents extremely slippery property which can obtain a sliding angle (SA) as low as 1°, nanowire pyramids-on-nanopores (WPOP) structure shows strongly sticky water adhesion with the adhesive ability to support 15 μL inverted water droplet at most. The obtained superhydrophobic alumina surfaces show remarkable mechanical durability even treated by crimping or pressing without impact on the water-repellent performance. Moreover, the created surfaces also show excellent resistivity to ice water, boiling water, high temperature, organic solvent and oil contamination, which could expand their usefulness and efficacy in harsh conditions. Copyright © 2013 Elsevier Inc. All rights reserved.

A BIDISPERSE MODEL TO STUDY THE HYDROLYSIS OF MALTOSE USING GLUCOAMYLASE IMMOBILIZED IN SILICA AND WRAPPED IN PECTIN GEL

Directory of Open Access Journals (Sweden)

L.R.B. Gonçalves

1997-12-01

Full Text Available In this work, a bidisperse model is built to represent the hydrolysis of maltose using immobilized glucoamylase. The experimental set is a mixed-batch reactor, maintained at 30ºC, with pectin gel spherical particles that contain enzyme immobilized in macroporous silica. The possibility of substrate adsorption on the pectin gel is also studied because this phenomenon may result in smaller values of diffusivity. Equilibrium assays are then performed for different substrates (maltose, lactose and glucose at different temperatures and pHs. These assays show that adsorption on the pectin gel is not important for the three dextrins analysed. The bidisperse model presents a good fit with the experimental data, when using previously-estimated kinetic and mass transfer parameters (Gonçalves et al., 1997. This result shows that the methodology used (wrapping the silica in pectin gel is appropriate for experimental studies with silica, since it allows a higher degree of agitation without causing shearing

Effect of silica fiber on the mechanical and chemical behavior of alumina-based ceramic core material

OpenAIRE

Weiguo Jiang; Kaiwen Li; Jiuhan Xiao; Langhong Lou

2017-01-01

In order to improve the chemical leachability, the alumina-based ceramic core material with the silica fiber was injected and sintered at 1100 °C/4 h, 1200 °C/4 h, 1300 °C/4 h and 1400 °C/4 h, respectively. The micrographs of ceramic core materials at sintered and leached state were characterized by scanning electron microscopy (SEM). The phase composition of ceramic core material after sintering and the leaching product after leaching were detected by X-ray diffraction (XRD). The porosity, r...

Fabrication of silica ceramic membrane via sol-gel dip-coating method at different nitric acid amount

Science.gov (United States)

Kahlib, N. A. Z.; Daud, F. D. M.; Mel, M.; Hairin, A. L. N.; Azhar, A. Z. A.; Hassan, N. A.

2018-01-01

Fabrication of silica ceramics via the sol-gel method has offered more advantages over other methods in the fabrication of ceramic membrane, such as simple operation, high purity homogeneous, well defined-structure and complex shapes of end products. This work presents the fabrication of silica ceramic membrane via sol-gel dip-coating methods by varying nitric acid amount. The nitric acid plays an important role as catalyst in fabrication reaction which involved hydrolysis and condensation process. The tubular ceramic support, used as the substrate, was dipped into the sol of Tetrethylorthosilicate (TEOS), distilled water and ethanol with the addition of nitric acid. The fabricated silica membrane was then characterized by (Field Emission Scanning Electron Microscope) FESEM and (Fourier transform infrared spectroscopy) FTIR to determine structural and chemical properties at different amount of acids. From the XRD analysis, the fabricated silica ceramic membrane showed the existence of silicate hydrate in the final product. FESEM images indicated that the silica ceramic membrane has been deposited on the tubular ceramic support as a substrate and penetrate into the pore walls. The intensity peak of FTIR decreased with increasing of amount of acids. Hence, the 8 ml of acid has demonstrated the appropriate amount of catalyst in fabricating good physical and chemical characteristic of silica ceramic membrane.

Comparison of optical properties of Eu3+ ions in the silica gel glasses obtained by different preparation techniques

International Nuclear Information System (INIS)

Legendziewicz, J.; Sokolnicki, J.; Keller, B.; Borzechowska, M.; Strek, W.

1996-01-01

Silica-gel glasses doped with Eu 3+ ions were obtained by different preparation techniques. The absorption, emission and excitation spectra of the obtained glasses were measured in the range of 77-300 K. The energy levels diagrams of Eu 3+ ions were derived. An intensity analysis of f-f transitions was performed. In particular, polymeric structure behaviour of europium compounds entrapped in silica gel glasses was temperature controlled during the preparation of glasses. Their optical properties were investigated. (author)

Iodine, krypton and xenon retention efficiencies of silver impregnated silica gel media with different silver loadings and under different test conditions

International Nuclear Information System (INIS)

Motes, B.G.; Fernandez, S.J.; Tkachyk, J.W.

1983-02-01

The purpose of an independent study conducted by Exxon Nuclear Idaho, Co. (ENICO) was to evaluate a silver impregnated silica gel adsorption medium associated with a radioiodine air sampler developed at Brookhaven National Laboratory (BNL). Specifically, ENICO's responsibility was to evaluate the iodine and noble gas retention efficiencies of the adsorption medium. The evaluation was comprised of a four-phase program: 1) test assemblies capable of challenging the silver silica gel filled adsorber canister with radioiodine species or noble gases at flow rates up to 10 scfm and relative humidities up to 83% were constructed; 2) more than 45 kgs of the 4 and 8% silver impregnated silica gel were prepared and characterized for particle size distribution, bulk silver content, bulk density, and silver content by particle size; 3) iodine species retention efficiencies of the silver silica gel were determined; and 4 krypton and xenon retention efficiencies were measured. The iodine species retention efficiencies were greater than 90% under most conditions. A combination of flow rates >5 scfm and 4% silver loaded silica gel reduced the methyl iodide retention efficiency to less than 90%. The retention efficiencies for both krypton and xenon were on the order of 8 x 10 -2 % and were not affected greatly by any test variable except test duration. A reduced retention efficiency with increased test durations indicates adsorption equilibrium may be established within five minutes. (author)

Synthesis of Titania-Silica Materials by Sol-Gel

Directory of Open Access Journals (Sweden)

Rubia F. S. Lenza

2002-10-01

Full Text Available In this work TiO2-SiO2 glasses containing as much as 20 mol % of TiO2 were prepared via sol-gel process using titanium and silicon alkoxides, in the presence of chlorine, in the form of titanium tetrachloride or HCl. The gels were heat-treated until 800 °C. X-ray diffraction and Fourier transform infrared spectroscopy were used to understand the structural properties of TiO2-SiO2 oxides calcined at different temperatures and to evaluate the homogeneity of these materials. The degree of the compactness of the silica network is inferred from the frequency of the asymmetric stretching vibrations of Si-O-Si bonds. Formation of Si-O-Ti bridges, as monitored by the intensity of characteristic 945 cm-1 ¾ 960 cm-1 vibration, is particularly prominent if the method of basic two-step prehydrolysis of silicon alkoxide, addition of titanium alkoxide and completion of hydrolysis was used.

Damping and tuning of the fibre violin modes in monolithic silica suspensions

International Nuclear Information System (INIS)

Gossler, S; Cagnoli, G; Crooks, D R M; Lueck, H; Rowan, S; Smith, J R; Strain, K A; Hough, J; Danzmann, K

2004-01-01

High Q mirror suspensions are a key element of the advanced interferometric gravitational-wave detectors. In December 2002 the last of the final interferometer optics of GEO 600 were monolithically suspended, using fused silica fibres. The violin modes of the suspension fibres can have Q greater than 10 8 and can therefore interfere with the interferometer length control servo. Hence, the violin modes need to be damped, without degrading the pendulum Q itself. Furthermore, the frequency spread of the fibres used has to be small to allow for high Q notch filtering in the length control servo. The requirements for the violin modes of the two GEO 600 inboard suspensions are Q 6 for the fundamental and Q 6 for the first harmonic mode, respectively. The frequency spread should not exceed 10% within one mode. To accomplish that, two sections of the fibres were coated with amorphous Teflon. By applying the coating, the Q of the relevant modes can be degraded to the desired values and furthermore, the frequencies of these modes can be tuned almost independently with a good accuracy over a wide range. After welding the fibres in the monolithic suspension, a corrective coating was applied to some fibres, to compensate for the frequency spread due to the tension spread of the four fibres within a suspension. We present the method and the results achieved

Reinforcement of LENRA film by in-situ generated silica produced by sol gel process

International Nuclear Information System (INIS)

Mahathir Mohamed; Eda Yuhana Ariffin; Dahlan Mohd; Ibrahim Abdullah

2008-08-01

Liquid epoxidised natural rubber acrylate (LENRA) film was reinforced with silica-siloxane structures formed in-situ via sol gel process. Combination of these two components produces organic-inorganic composites. Tetraethylorthosilicate (TEOS) was used as precursor material for silica generation. Sol gel reaction was carried out at different concentrations of TEOS i.e. between 10 and 50 phr. Instrumental analysis was carried out by dynamic mechanical analysis (DMA), thermogravimetry analysis (TGA) and FTIR. It was found that miscibility between organic and inorganic components improved with the presence of silanol groups (Si-OH) and polar solvent i.e. THF, via hydrogen bonding formation between siloxane and LENRA. In this work, the effects of TEOS composition on mechanical properties and interaction that occurs between fillers and matrix have also been studied. It was observed that increasing the concentration of TEOS improved the scratch and stress properties of the film. Morphology study by the scanning electron microscopy (SEM) showed in-situ generated silica particles were homogenous and well dispersed at low concentrations of TEOS. (Author)

Synthesis of palladium-doped silica nanofibers by sol-gel reaction and electrospinning process

Energy Technology Data Exchange (ETDEWEB)

San, Thiam Hui; Daud, Wan Ramli Wan; Kadhum, Abdul Amir Hassan; Mohamad, Abu Bakar; Kamarudin, Siti Kartom; Shyuan, Loh Kee; Majlan, Edy Herianto [Fuel Cell Institute, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor (Malaysia); Fuel Cell Institute, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor, Malaysia and Department of Chemical and Process Engineering, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor (Malaysia); Fuel Cell Institute, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor (Malaysia)

2012-06-29

Nanofiber is drawing great attention nowadays with their high surface area per volume and flexibility in surface functionalities that make them favorable as a proton exchange membrane in fuel cell application. In this study, incorporation of palladium nanoparticles in silica nanofibers was prepared by combination of a tetraorthosilane (TEOS) sol-gel reaction with electrospinning process. This method can prevent the nanoparticles from aggregation by direct mixing of palladium nanoparticles in silica sol. The as-produced electrospun fibers were thermally treated to remove poly(vinyl pyrrolidone) (PVP) and condensation of silanol in silica framework. PVP is chosen as fiber shaping agent because of its insulting and capping properties for various metal nanoparticles. Scanning electron microscopy (SEM), energy dispersive spectrometer (EDS) and Fourier transform infrared spectroscopy (FTIR) were used to characterize the silica fibers and Pd nanoparticles on the fibers. Spun fibers with average diameter ranged from 100nm to 400nm were obtained at optimum operating condition and distribution of Pd nanoparticles on silica fibers was investigated.

D. C. plasma-sprayed coatings of nano-structured alumina-titania-silica

CERN Document Server

Jiang Xian Liang

2002-01-01

nano-crystalline powders of omega(Al sub 2 O sub 3) = 95%, omega(TiO sub 2) = 3%, and omega(SiO sub 2) = 2%, were reprocessed into agglomerated particles for plasma spraying, by using consecutive steps of ball milling, slurry forming, spray drying, and heat treatment. D.C. plasma was used to spray the agglomerated nano-crystalline powders, and resultant coatings were deposited on the substrate of stainless steel. Scanning electron microscopy (SEM) was used to examine the morphology of the agglomerated powders and the cross section of the alumina-titania-silica coatings. Experimental results show that the agglomerated nano-crystalline particles are spherical, with a size from (10-90) mu m. The flow ability of the nano-crystalline powders is greatly improved after the reprocessing. The coatings deposited by the plasma spraying are mainly of nano-structure. Unlike conventional plasma-sprayed coatings, no laminar layer could be found in the nano-structured coatings. Although the nano-structured coatings have a lo...

Sol-gel synthesized of nanocomposite palladium-alumina ceramic membrane for H{sub 2} permeability: Preparation and characterization

Energy Technology Data Exchange (ETDEWEB)

Ahmad, A.L.; Mustafa, N.N.N. [School of Chemical Engineering, Engineering Campus, Universiti Sains Malaysia, Seri Ampangan, 14300 Nibong Tebal, Penang (Malaysia)

2007-08-15

Palladium-alumina membrane with mesopore and narrow pore size distribution was prepared by the sol-gel method. Effect of the finely dispersed metal on the microstructure and the characteristic properties of the palladium-alumina membrane were investigated. Observations were made on membrane weight loss, morphology, pore structure, pore size, surface area, pore surface fractal and membrane's crystal structure. Autosorb analysis, X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM) and Fourier Transform Infrared (FTIR) analysis were employed in the membrane characterization. Autosorb analysis found that, BET surface area decreased and pore size of the membrane increased with the increasing of calcinations temperature (500-1100{sup o}C) and with the increasing of palladium amount in the membrane. FTIR and TG/DTA analysis show that the suitable temperature for calcinations of palladium-alumina membrane is at 700{sup o}C. Palladium metals are highly dispersed at calcinations temperature of 700{sup o}C as observed by TEM analysis. The fine crystallinity of the palladium and {gamma}-alumina phase was obtained after calcined at 700{sup o}C. The SEM morphology shows a smooth and free crack layer of palladium-alumina membrane after repeating the process of dipping, drying and calcinations at temperature of 700{sup o}C. The membrane also successfully coated with a good adhesion on support. The thickness of the final membrane layer was estimated as 9{mu} m. (author)

Electrochemical redox reactions in solvated silica sol-gel glass

International Nuclear Information System (INIS)

Opallo, M.

2002-01-01

The studies of electrochemical redox reactions in solvated silica sol-gel glass were reviewed. The methodology of the experiments with emphasis on the direct preparation of the solid electrolyte and the application ultra microelectrodes was described. Generally, the level of the electrochemical signal is not much below that observed in liquid electrolyte. The current depends on time elapsed after gelation, namely the longer time, the smaller current. The differences between electrochemical behaviour of the redox couples in monoliths and thin layers were described. (author)

A pure silica ytterbium-doped sol–gel-based fiber laser

International Nuclear Information System (INIS)

Baz, Assaad; El Hamzaoui, Hicham; Fsaifes, Ihsan; Bouwmans, Géraud; Bouazaoui, Mohamed; Bigot, Laurent

2013-01-01

In this letter it is demonstrated that the sol–gel route combined with fiber fabrication by the stack and draw method can be used to realize efficient fiber lasers. More precisely, a pure silica ytterbium-doped photonic crystal fiber with a core obtained by the sol–gel polymeric technique is studied, and a laser efficiency of more than 73% is achieved for a laser emission around 1034 nm. The optical and spectroscopic properties of the monolith and fiber are investigated, together with the sensitivity of the fiber to photodarkening. The dimensions of the ytterbium-doped monolith combined with the uniform doping and refractive index that are reported make this technique particularly interesting for the realization of large-mode area fibers. (letter)

STUDY OF HYDRODYNAMICS IN FIXED BED OF COMPOSITE GRANULAR MATERIALS

Directory of Open Access Journals (Sweden)

Stelian Petrescu

2010-12-01

Full Text Available This study aims at the experimental determination of pressure drop and friction factor at gas flow through fixed beds of granular silica gel, alumina and activated carbon, and establishment of an equation containing a modified friction factor Fm to calculate pressure drop. In order to calculate the modified friction factor, an equation was suggested.The experimental values for pressure drop and friction factor were determined using spherical grains of silica gel, cylindrical grains of alumina and silica gel, alumina and activated carbon impregnated with calcium chloride. By means of the suggested equation, the values of pressure drop in fixed bed were calculated and compared with the experimental values. A good agreement between the predicted and experimental data is noticed.

Iodine, krypton and xenon retention efficiencies of silver impregnated silica gel media with different silver loadings and under different test conditions

Energy Technology Data Exchange (ETDEWEB)

Motes, B G; Fernandez, S J; Tkachyk, J W

1983-02-01

The purpose of an independent study conducted by Exxon Nuclear Idaho, Co. (ENICO) was to evaluate a silver impregnated silica gel adsorption medium associated with a radioiodine air sampler developed at Brookhaven National Laboratory (BNL). Specifically, ENICO's responsibility was to evaluate the iodine and noble gas retention efficiencies of the adsorption medium. The evaluation was comprised of a four-phase program: 1) test assemblies capable of challenging the silver silica gel filled adsorber canister with radioiodine species or noble gases at flow rates up to 10 scfm and relative humidities up to 83% were constructed; 2) more than 45 kgs of the 4 and 8% silver impregnated silica gel were prepared and characterized for particle size distribution, bulk silver content, bulk density, and silver content by particle size; 3) iodine species retention efficiencies of the silver silica gel were determined; and 4 krypton and xenon retention efficiencies were measured. The iodine species retention efficiencies were greater than 90% under most conditions. A combination of flow rates >5 scfm and 4% silver loaded silica gel reduced the methyl iodide retention efficiency to less than 90%. The retention efficiencies for both krypton and xenon were on the order of 8 x 10{sup -2}% and were not affected greatly by any test variable except test duration. A reduced retention efficiency with increased test durations indicates adsorption equilibrium may be established within five minutes. (author)

Synthesis and characterization of uniform silica nanoparticles on nickel substrate by spin coating and sol-gel method

Science.gov (United States)

Ngoc Thi Le, Hien; Jeong, Hae Kyung

2014-01-01

Spin coating and sol-gel methods are proposed for the preparation of silica nanoparticles on a nickel substrate using silicon tetrachloride, 2-methoxyethanol, and four different types of alkaline solutions. The effects of the type of alkaline solution, concentration of silica solution, and speed of spin coating on the properties of silica nanoparticles are investigated systematically. Uniform spherical shape of silica nanoparticles on Ni with the smallest size are obtained with sodium carbonate among the alkaline solutions after stirring at 70 °C for 6 h and spin-coating at 7000 rpm. Physical and electrochemical properties of the silica particles are investigated.

Silica doped with lanthanum sol-gel thin films for corrosion protection

Energy Technology Data Exchange (ETDEWEB)

Abuin, M. [Department of Materials Physics, Complutense University at Madrid, Avda. Complutense sn, 28004 Madrid (Spain); Serrano, A. [Glass and Ceramic Institute, CSIC, C. Kelsen 5, 28049 Madrid (Spain); Llopis, J. [Department of Materials Physics, Complutense University at Madrid, Avda. Complutense sn, 28004 Madrid (Spain); Garcia, M.A. [Glass and Ceramic Institute, CSIC, C. Kelsen 5, 28049 Madrid (Spain); IMDEA Nanoscience, Fco. Tomas y Valiente 7, 28049 Madrid (Spain); Carmona, N., E-mail: n.carmona@fis.ucm.es [Department of Materials Physics, Complutense University at Madrid, Avda. Complutense sn, 28004 Madrid (Spain)

2012-06-01

We present here anticorrosive silica coatings doped with lanthanum ions for the protection of metallic surfaces as an alternative to chromate (VI)-based conversion coatings. The coatings were synthesized by the sol-gel method starting from silicon alkoxides and two different lanthanum precursors: La (III) acetate hydrate and La (III) isopropoxide. Artificial corrosion tests in acid and alkaline media showed their effectiveness for the corrosion protection of AA2024 aluminum alloy sheets for coating prepared with both precursors. The X-ray absorption Near Edge Structure and X-ray Absorption Fine Structure analysis of the coatings confirmed the key role of lanthanum in the structural properties of the coating determining its anticorrosive properties. - Highlights: Black-Right-Pointing-Pointer Silica sol-gel films doped with lanthanum ions were synthesized. Black-Right-Pointing-Pointer Films from lanthanum-acetate and La-alkoxide were prepared for comparison purposes. Black-Right-Pointing-Pointer La-acetate is an affordable chemical reactive preferred for the industry. Black-Right-Pointing-Pointer Films properties were explored by scanning electron microscopy and X-Ray absorption spectroscopy. Black-Right-Pointing-Pointer An alternative to anticorrosive pre-treatments for metallic surfaces is suggested.

Synthesis of biocompatible hydrophobic silica-gelatin nano-hybrid by sol-gel process.

Science.gov (United States)

Smitha, S; Shajesh, P; Mukundan, P; Nair, T D R; Warrier, K G K

2007-03-15

Silica-biopolymer hybrid has been synthesised using colloidal silica as the precursor for silica and gelatin as the biopolymer counterpart. The surface modification of the hybrid material has been done with methyltrimethoxysilane leading to the formation of biocompatible hydrophobic silica-gelatin hybrid. Here we are reporting hydrophobic silica-gelatin hybrid and coating precursor for the first time. The hybrid gel has been evaluated for chemical modification, thermal degradation, hydrophobicity, particle size, transparency under the UV-visible region and morphology. FTIR spectroscopy has been used to verify the presence of CH(3) groups which introduce hydrophobicity to the SiO2-MTMS-gelatin hybrids. The hydrophobic property has also been tailored by varying the concentration of methyltrimethoxysilane. Contact angle by Wilhelmy plate method of transparent hydrophobic silica-gelatin coatings has been found to be as high as approximately 95 degrees . Oxidation of the organic group which induces the hydrophobic character occurs at 530 degrees C which indicates that the surface hydrophobicity is retained up to that temperature. Optical transmittance of SiO2-MTMS-gelatin hybrid coatings on glass substrates has been found to be close to 100% which will enable the hybrid for possible optical applications and also for preparation of transparent biocompatible hydrophobic coatings on biological substrates such as leather.

Aging time on the aluminum basic acetate gel and its influence on the membrane permeability

International Nuclear Information System (INIS)

Clar, C; Scian, A. N; Aglietti, E.F

2003-01-01

Alumina ceramic membranes are new materials with important applications in separation processes with low energy requirements, high selectivity and ability to work at high and low temperatures.The preparation of alumina ceramic membranes from hydrates or aluminum salts as precursors implies obtaining a system of controlled porosity with a suitable mechanical resistance as well as the densification of the material thanks to the stable phases remaining after the thermal treatment.The metal carboxylates are potential precursors for the deposition and the subsequent formation of oxides at low temperatures.Aluminum basic acetate gel was synthesised in this work from commercial pseudobohemite. The influence of the aging time on the composition, crystalline structure and transition temperatures of the phases on the carboxylate was studied by XRD and DTA-TG.From suspensions of this aged gel at different times alumina ceramic membranes were prepared by dipcoating on different α-Al 2 O 3 supports and the influence of aging on the permeability of those membranes face to N 2 was also studied. It was observed that this is a parameter to be considered as it determines the thickness, permeability and integrity of the membranes

Al2O3 - TiO2-A simple sol-gel strategy to the synthesis of low temperature sintered alumina-aluminium titanate composites through a core-shell approach

International Nuclear Information System (INIS)

Jayasankar, M.; Ananthakumar, S.; Mukundan, P.; Wunderlich, W.; Warrier, K.G.K.

2008-01-01

A simple sol-gel based core-shell approach for the synthesis of alumina-aluminium titanate composite is reported. Alumina is the core and titania is the shell. The coating of titania has been performed in aqueous medium on alumina particle by means of heterocoagulation of titanyl chloride. Further heat treatment results in low temperature formation of aluminium titanate as well as low temperature sintering of alumina-aluminium titanate composites. The lowering of the reaction temperature can be attributed to the maximisation of the contact surface between the reactants due to the core-shell approach involving nanoparticles. The mechanism of formation of aluminium titanate and the observations on densification features in the present process are compared with that of mixture of oxides under identical conditions. The sintered alumina-aluminium titanate composite has an average grain size of 2 μm. - Graphical abstract: The article presents a simple sol-gel process through core-shell approach to the synthesis of low temperature sintered alumina-aluminium titanate. The lowering of the reaction temperature can be attributed to the maximisation of the contact surface between the reactant due to the core-shell approach. This material showed the better microstructure control compared to the standard solid-state mixing route

In situ immobilization on the silica gel surface and adsorption capacity of polymer-based azobenzene on toxic metal ions

Science.gov (United States)

Savchenko, Irina; Yanovska, Elina; Sternik, Dariusz; Kychkyruk, Olga; Ol'khovik, Lidiya; Polonska, Yana

2018-03-01

In situ immobilization of poly[(4-methacryloyloxy-(4'-carboxy)azobenzene] on silica gel surface has been performed by radical polymerization of monomer. The fact of polymer immobilization is confirmed by IR spectroscopy. TG and DSC-MS analysis showed that the mass of the immobilized polymer was 10.61%. The SEM-microphotograph-synthesized composite analysis showed that the immobilized polymer on the silica gel surface is placed in the form of fibers. It has been found that the synthesized composite exhibits the sorption ability in terms of microquantities of Cu(II), Cd(II), Pb(II), Mn(II) and Fe(III) ions in a neutral aqueous medium. The quantitative sorption of microquantities of Pb(II) and Fe(III) ions has been recorded. It has been found that immobilization of the silica gel surface leads to an increase in its sorption capacitance for Fe(III), Cu(II) and Pb(II) ions by half.

Damping and tuning of the fibre violin modes in monolithic silica suspensions

Energy Technology Data Exchange (ETDEWEB)

Gossler, S [Max-Planck-Institute for Gravitational Physics (Albert-Einstein-Institute) and University of Hannover, Callinstr 38, D-30167 Hannover (Germany); Cagnoli, G [Department of Physics and Astronomy, Institute for Gravitational Research, University of Glasgow, Glasgow G12 8QQ (United Kingdom); Crooks, D R M [Department of Physics and Astronomy, Institute for Gravitational Research, University of Glasgow, Glasgow G12 8QQ (United Kingdom); Lueck, H [Max-Planck-Institute for Gravitational Physics (Albert-Einstein-Institute) and University of Hannover, Callinstr 38, D-30167 Hannover (Germany); Rowan, S [Department of Physics and Astronomy, Institute for Gravitational Research, University of Glasgow, Glasgow G12 8QQ (United Kingdom); Smith, J R [Max-Planck-Institute for Gravitational Physics (Albert-Einstein-Institute) and University of Hannover, Callinstr 38, D-30167 Hannover (Germany); Strain, K A [Department of Physics and Astronomy, Institute for Gravitational Research, University of Glasgow, Glasgow G12 8QQ (United Kingdom); Hough, J [Department of Physics and Astronomy, Institute for Gravitational Research, University of Glasgow, Glasgow G12 8QQ (United Kingdom); Danzmann, K [Max-Planck-Institute for Gravitational Physics (Albert-Einstein-Institute) and University of Hannover, Callinstr 38, D-30167 Hannover (Germany)

2004-03-07

High Q mirror suspensions are a key element of the advanced interferometric gravitational-wave detectors. In December 2002 the last of the final interferometer optics of GEO 600 were monolithically suspended, using fused silica fibres. The violin modes of the suspension fibres can have Q greater than 10{sup 8} and can therefore interfere with the interferometer length control servo. Hence, the violin modes need to be damped, without degrading the pendulum Q itself. Furthermore, the frequency spread of the fibres used has to be small to allow for high Q notch filtering in the length control servo. The requirements for the violin modes of the two GEO 600 inboard suspensions are Q < 3 x 10{sup 6} for the fundamental and Q < 2 x 10{sup 6} for the first harmonic mode, respectively. The frequency spread should not exceed 10% within one mode. To accomplish that, two sections of the fibres were coated with amorphous Teflon. By applying the coating, the Q of the relevant modes can be degraded to the desired values and furthermore, the frequencies of these modes can be tuned almost independently with a good accuracy over a wide range. After welding the fibres in the monolithic suspension, a corrective coating was applied to some fibres, to compensate for the frequency spread due to the tension spread of the four fibres within a suspension. We present the method and the results achieved.

Rheological properties of ceramic nanopowders in aqueous and nonaqueous suspensions

International Nuclear Information System (INIS)

Tomaszewski, H.; Loiko, E.M.

2003-01-01

The potential for ceramic nanocomposites to offer significantly enhanced mechanical properties is generally known since the first work of Niihara published in 1991. However achieving these properties needs carefully done colloidal processing, because ceramic nanopowders are naturally prone to agglomeration. The work presented here is concerned with the processing of zirconia/alumina nanocomposites via aqueous and alumina silicon carbide nanocomposites via nonaqueous colloidal route. The effect of pH of aqueous alumina and zirconia suspensions on properties of suspension and centrifuged green bodies was studied. A correlation between surface electric charge of grains (zeta potential)and agglomerate size, viscosity of suspension and porosity of green compacts was found. In the case of nonaqueous route alumina and silicon carbide suspensions in iso-propanol were investigated. Electrostatic surface charge of grains was changed by addition of chloroacetic acid and determined indirectly by the mass of powder deposited on electrode during electrophoresis. Different behaviour of SiC nanopowder than of alumina was observed and mechanism of charge creation is proposed on the base of DLVO theory. The effect of grain charge on preventing agglomeration on the silicon carbide powder is presented on micrographs of sintered nanocomposites. (author)

Stability of inorganic mercury and methylmercury on yeast-silica gel microcolumns: field sampling capabilities

Energy Technology Data Exchange (ETDEWEB)

Perez-Corona, M. [Universidad Complutense de Madrid (Spain). Dept. de Quimica Analitica

2000-11-01

The stability of methylmercury and inorganic mercury retained on yeast-silica gel microcolumns was established and compared with the stability of these species in solution. Yeast-silica gel columns with the retained analytes were stored for two months at three different temperatures: -20 C, 4 C and room temperature. At regular time intervals, both mercury species were eluted and quantified by cold vapor atomic absorption spectrometry (CVAAS). Methylmercury was found stable in the columns over the two-month period at the three different temperatures tested while the concentration of inorganic mercury decreased after one week's storage even at -20 C. These results are of great interest since the use of these microcolumns allows the preconcentration and storage of mercury species until analysis, thus saving laboratory space and avoiding the problems associated with maintaining species integrity in aqueous solution. (orig.)

Modeling the supercritical desorption of orange essential oil from a silica-gel bed

Directory of Open Access Journals (Sweden)

Silva E.A.

2000-01-01

Full Text Available One of the most important byproducts of the orange juice industry is the oil phase. This is a mixture of terpenes, alcohols, and aldehydes, dissolved in approximately 96% limonene. To satisfactorily use oil phase as an ingredient in the food and cosmetics industries separation of the limonene is required. One possibility is to use a fixed bed of silica gel to remove the light or aroma compounds from the limonene. The aroma substances are then extracted from the bed of silica gel using supercritical carbon dioxide. This work deals with the modeling of the desorption step of the process using mass balance equations coupled with the Langmuir equilibrium isotherm. Data taken from the literature for the overall extraction curves were used together with empirical correlations to calculate the concentration profile of solute in the supercritical phase at the bed outlet. The system of equations was solved by the finite volume technique. The overall extraction curves calculated were in good agreement with the experimental ones.

Ionic liquids as dynamic templating agents for sol-gel silica systems: synergistic anion and cation effect on the silica structured growth

Czech Academy of Sciences Publication Activity Database

Donato, K. Z.; Donato, Ricardo Keitel; Lavorgna, M.; Ambrosio, L.; Matějka, Libor; Mauler, R. S.; Schrekker, H. S.

2015-01-01

Roč. 76, č. 2 (2015), s. 414-427 ISSN 0928-0707 R&D Projects: GA ČR GAP108/12/1459 Institutional support: RVO:61389013 Keywords : silica * imidazolium ionic liquid * sol-gel Subject RIV: CD - Macromolecular Chemistry Impact factor: 1.473, year: 2015

Synthesis and nonlinear optical properties of zirconia-protected gold nanoparticles embedded in sol-gel derived silica glass

Science.gov (United States)

Le Rouge, A.; El Hamzaoui, H.; Capoen, B.; Bernard, R.; Cristini-Robbe, O.; Martinelli, G.; Cassagne, C.; Boudebs, G.; Bouazaoui, M.; Bigot, L.

2015-05-01

A new approach to dope a silica glass with gold nanoparticles (GNPs) is presented. It consisted in embedding zirconia-coated GNPs in a silica sol to form a doped silica gel. Then, the sol-doped nanoporous silica xerogel is densified leading to the formation of a glass monolith. The spectral position and shape of the surface plasmon resonance (SPR) reported around 520 nm remain compatible with small spherical GNPs in a silica matrix. The saturable absorption behavior of this gold/zirconia-doped silica glass has been evidenced by Z-scan technique. A second-order nonlinear absorption coefficient β of about -13.7 cm GW-1 has been obtained at a wavelength near the SPR of the GNPs.

Synthesis of α-Alumina (Corundum) and its Application

International Nuclear Information System (INIS)

Nay Thwe Kyi; Kyaw Myo Naing; Tin Tin Aye; Nyunt Wynn

2005-09-01

This paper described the preparation of aluminium isopropoxide from aluminium sheet at different heating times.Aluminium sheet is found to have a reaction with absolute isopropyl alcohol and mercury (II) chloride as a catalyst under nitrogen atmosphere. Aluminium isopropoxide was characterized by NMR, XRD and IR. Aluminium isopropoxide serves as a molecular precursor to derive pure alumina gel by hydrolysis under both homogeneous and heterogeneous conditions. Pyrolysis to this alumina gel transforms it into -aluminia (corundum) at 1200'C. The phase transformation during pyrolysis was characterized by XRD, SEM and TEM. The alumina (corundum) has porous crystalline nature with high surface aera, which may be used as efficient adsorbent packing material in coloumn chromatography for the seperation of vitamin A from the leaves. -alumina can be also used in catalysis

Synthesis and characterization of nanocomposite powders of calcium phosphate/silica-gel; Sintese e caracterizacao de pos nanoestruturados de fosfato de calcio/silica-gel

Energy Technology Data Exchange (ETDEWEB)

Muller, D.T.; Delima, S.A. [Universidade do Estado de Santa Catarina (UDESC), Joinville, SC (Brazil). Dept. de Engenharia Mecanica; Santos, R.B.M.; Camargo, N.H.A., E-mail: dem2nhac@joinville.udesc.b [Universidade do Estado de Santa Catarina (UDESC), Joinville, SC (Brazil). Programa de Pos Graduacao em Ciencia e Engenharia de Materiais

2009-07-01

In the recent years ceramics of calcium phosphate are pointed out as an outstanding material in substitution and regeneration in defects from osseous tissue, in reason of their similar mineralogical characteristics of apatite of bone structure. However, the challenge with phosphate calcium ceramics find out about the mechanical properties and the development of biomaterials similar of the bone structure, what sometimes is not so easy, about fragile materials. The aim of this work focused in synthesis and characterization nanocomposites powders of calcium phosphate/silica-gel with percentages 1, 2, 3 e 5% of nanometric silica. The method synthesis used for the compositions elaboration was dissolution-precipitation. The presented results are related with the optimization to method elaboration of nanostructured powders, the mineralogical characterization with X-ray diffraction, thermal behavior with thermal differential analysis, differential scanning calorimetry here is ADT and dilatometer. The scanning electronic microscopy was used to help of morphological characterization the nanostructured powders and the surfaces from body test recovered from the mechanical test. (author)

Permeability optimization and performance evaluation of hot aerosol filters made using foam incorporated alumina suspension.

Science.gov (United States)

Innocentini, Murilo D M; Rodrigues, Vanessa P; Romano, Roberto C O; Pileggi, Rafael G; Silva, Gracinda M C; Coury, José R

2009-02-15

Porous ceramic samples were prepared from aqueous foam incorporated alumina suspension for application as hot aerosol filtering membrane. The procedure for establishment of membrane features required to maintain a desired flow condition was theoretically described and experimental work was designed to prepare ceramic membranes to meet the predicted criteria. Two best membranes, thus prepared, were selected for permeability tests up to 700 degrees C and their total and fractional collection efficiencies were experimentally evaluated. Reasonably good performance was achieved at room temperature, while at 700 degrees C, increased permeability was obtained with significant reduction in collection efficiency, which was explained by a combination of thermal expansion of the structure and changes in the gas properties.

Dose uniformity of loteprednol etabonate ophthalmic gel (0.5%) compared with branded and generic prednisolone acetate ophthalmic suspension (1%).

Science.gov (United States)

Marlowe, Zora T; Davio, Stephen R

2014-01-01

Loteprednol etabonate (LE) ophthalmic gel 0.5% (Lotemax®) is a new polycarbophil-based, nonsettling topical ophthalmic formulation. The formulation is a semisolid gel at rest and a shear thinning fluid when expressed through a dropper tip. The present study was undertaken to determine how the nonsettling character of LE ophthalmic gel affects dose uniformity. Prednisolone acetate ophthalmic suspension 1% (Pred Forte®) and a generic prednisolone acetate suspension 1% were used as comparators. Drug concentrations of LE ophthalmic gel, Pred Forte, and a generic prednisolone acetate suspension were determined following simulated dosing - consisting of 2 drops, expressed four times daily for 2 weeks, with bottles that were shaken or not shaken immediately prior to expressing the drops. Drug concentrations were determined using a reverse-phase high-performance liquid chromatography (HPLC) method and reported as a percentage of the declared (labeled) concentration. Comparative kinetics of drug particle sedimentation were also determined for each formulation, using dispersion analysis under gravity. Mean drug concentrations in drops of all three formulations were within a few percentage points of the declared concentration when the bottles were shaken for 5 seconds prior to dispensing. Only LE ophthalmic gel showed consistent and on-target concentrations when the bottles were unshaken prior to dispensing, with a mean (standard deviation [SD]) percent declared concentration of 102% (1.92%) over the 2-week dosing regimen. Drug concentrations for the branded and generic prednisolone acetate suspensions following expression from unshaken bottles were highly variable (overall relative SDs of 16.8% and 20.3%, respectively), with mean concentrations for both falling significantly below the declared concentration for drops expressed at the beginning of the 2-week dosing regimen and significantly above the declared concentration for drops expressed near the end of the dosing

Stability and reproducibility of gel-suspension samples for the liquid scintillation counting of 14C using N-lauroyl-L-glutamic-α,γ-dibutylamide

International Nuclear Information System (INIS)

Wakabayashi, G.; Ohura, H.; Okai, T.; Matoba, M.

1999-01-01

Stability and reproducibility of gel-suspension method for 14 C activity measurement. Commercially available gelling agent, N-lauroyl-L-glutamic-α,γ-dibutylamide, was used for the gel-formation of the samples. No change of the counting rate for the gel-suspension sample was observed for more than 2 years after the sample preparation. Four samples used for checking the reproducibility of the sample preparation method. The same values were obtained for the counting rate of 14 C activity within the counting error. No change of the counting rate was observed for the 're-gelated' sample. These results show that the gel-suspension method is appropriate for the 14 C activity measurement by the liquid scintillation method and is useful for a long-term preservation of the sample for repeated measurement. (author)

Evaluation of technological properties of alumina refractory systems-zirconia and zirconia-silica-alumina; Avaliacao das propriedades tecnologicas de refratarios dos sistemas alumina-zirconia e alumina-zirconia-silica

Energy Technology Data Exchange (ETDEWEB)

Marinho, A.R.O.; Carvalho, T.U.S.; Fagury Neto, E.; Rabelo, A.A., E-mail: adriano@unifesspa.edu.br [Universidade Federal do Sul e Sudeste do Para (UFSSPA), Maraba, PA (Brazil)

2014-07-01

Alumina-zirconia refractories are noted for being products of excellent cost-effective, however, zirconia may limit its use due to decreasing resistance to thermal shock. This study aims to evaluate these refractories with the addition of microsilica, which can greatly improve their properties. Were used the following starting materials: calcined alumina, zirconia (stabilized and monoclinic) in amounts of 2%, 4% and 6% by weight, plus microsilica (5%w.). The powders were milled together with binder and lubricant for conformation bodies by uniaxial pressing. The samples were dried, calcined and sintered at 1400 °C/2h were characterized using the methods of Archimedes, and scanning electron microscopy (SEM), chemical analysis using energy dispersive X-ray (EDS), and mechanical flexural strength tests at room temperature. Formulations with the presence of microsilica showed satisfactory results and optimized properties. (author)

Strong visible-light emission of ZnS nanocrystals embedded in sol-gel silica xerogel

International Nuclear Information System (INIS)

Yang Ping; Lue, M.-K.; Song, C.-F.; Zhou, G.-J.; Ai, Z.-P.; Xu Dong; Yuan, D.-R.; Cheng, X.-F.

2003-01-01

ZnS nanoparticles embedded in novel porous phosphor silica xerogel have been synthesized by sol-gel processing. Their fluorescence properties have been evaluated and compared with those of the Na + -doped and un-doped silica xerogels. Stable and strong visible-light emission of the doped samples has been observed. The relative fluorescence intensities of the samples doped with ZnS nanoparticles (S 2- ions have been obtained by the water solution of NaS) are the highest among all of the doped samples. Its relative fluorescence intensity is about 7.5 times of that of the un-doped silica xerogel and about 300 times of that of pure ZnS nanoparticles. The emission wavelength of the ZnS-doped and Na + -doped samples is the same as that of the un-doped silica xerogel and ZnS nanoparticles (λ em =440-450 nm). This high efficiency luminescence of the doped silica xerogels has been assigned to the luminescence centers of ZnS nanoparticles and Na + in the porous phosphorescence silica xerogel

Transition metal-free oxidation of benzylic alcohols to carbonyl compounds by hydrogen peroxide in the presence of acidic silica gel

Directory of Open Access Journals (Sweden)

Hossein Ghafuri

2015-01-01

Full Text Available Oxidation of alcohols to carbonyl compounds has become an important issue in the process industry as well as many other applications. In this method, various benzylic alcohols were successfully converted to corresponding aldehydes and ketones under transition metal-free condition using hydrogen peroxide in the presence of some amount of catalytic acidic silica gel. Silica gel is inexpensive and available. One of the most important features of this method is its short reaction time.

D. C. plasma-sprayed coatings of nano-structured alumina-titania-silica

International Nuclear Information System (INIS)

Jiang Xianliang

2002-01-01

nano-crystalline powders of ω(Al 2 O 3 ) = 95%, ω(TiO 2 ) = 3%, and ω(SiO 2 ) = 2%, were reprocessed into agglomerated particles for plasma spraying, by using consecutive steps of ball milling, slurry forming, spray drying, and heat treatment. D.C. plasma was used to spray the agglomerated nano-crystalline powders, and resultant coatings were deposited on the substrate of stainless steel. Scanning electron microscopy (SEM) was used to examine the morphology of the agglomerated powders and the cross section of the alumina-titania-silica coatings. Experimental results show that the agglomerated nano-crystalline particles are spherical, with a size from (10-90) μm. The flow ability of the nano-crystalline powders is greatly improved after the reprocessing. The coatings deposited by the plasma spraying are mainly of nano-structure. Unlike conventional plasma-sprayed coatings, no laminar layer could be found in the nano-structured coatings. Although the nano-structured coatings have a lower microhardness than conventional microstructured coatings, the toughness of the nano-structured ceramic coatings is significantly improved

Tetragonal zirconia quantum dots in silica matrix prepared by a modified sol-gel protocol

Science.gov (United States)

Verma, Surbhi; Rani, Saruchi; Kumar, Sushil

2018-05-01

Tetragonal zirconia quantum dots (t-ZrO2 QDs) in silica matrix with different compositions ( x)ZrO2-(100 - x)SiO2 were fabricated by a modified sol-gel protocol. Acetylacetone was added as a chelating agent to zirconium propoxide to avoid precipitation. The powders as well as thin films were given thermal treatment at 650, 875 and 1100 °C for 4 h. The silica matrix remained amorphous after thermal treatment and acted as an inert support for zirconia quantum dots. The tetragonal zirconia embedded in silica matrix transformed into monoclinic form due to thermal treatment ≥ 1100 °C. The stability of tetragonal phase of zirconia is found to enhance with increase in silica content. A homogenous dispersion of t-ZrO2 QDs in silica matrix was indicated by the mapping of Zr, Si and O elements obtained from scanning electron microscope with energy dispersive X-ray analyser. The transmission electron images confirmed the formation of tetragonal zirconia quantum dots embedded in silica. The optical band gap of zirconia QDs (3.65-5.58 eV) was found to increase with increase in zirconia content in silica. The red shift of PL emission has been exhibited with increase in zirconia content in silica.

Effect of Plasma Spheroidization Process on the Microstructure and Crystallographic Phases of Silica, Alumina and Nickel Particles

International Nuclear Information System (INIS)

Hu Peng; Yan Shikai; Yuan Fangli; Bai Liuyang; Li Jinlin; Chen Yunfa

2007-01-01

During the plasma spheroidization process powders undergo different changes in their microstructures and crystal phases. In this paper, simple calculation of heat transfer between the plasma and a suspended particle was performed based on three hypotheses for the purpose of guiding experiments. Experimental investigation of the crystal phases and microstructural changes during the plasma processing was made using silica, alumina and nickel powders as starting materials. It has been revealed from the experimental results that these materials undergo different changes in crystal phases and microstructures, and these changes are essentially determined by the structures, properties and aggregate states of the starting materials

[A treatment to serious esophageal cicatrices stenosi by metal and silica gel dilator].

Science.gov (United States)

Li, J; Chen, X; Sun, C; Liu, H

1999-12-01

To find an effective method of treating the esophageal cicatricial stenosis. Six cases with esophageal cicatricial stenosis were treated by mental and silica gel dilator. The effects in all six cases were satisfactory and no any complications were finded. The method is safe, effective and of no complications, the treatment time is shorter also.

Dose uniformity of loteprednol etabonate ophthalmic gel (0.5% compared with branded and generic prednisolone acetate ophthalmic suspension (1%

Directory of Open Access Journals (Sweden)

Marlowe ZT

2013-12-01

Full Text Available Zora T Marlowe, Stephen R DavioPharmaceutical Product Development, Global Pharmaceutical Research and Development, Bausch and Lomb, Inc, Rochester, NY, USAIntroduction: Loteprednol etabonate (LE ophthalmic gel 0.5% (Lotemax® is a new polycarbophil-based, nonsettling topical ophthalmic formulation. The formulation is a semisolid gel at rest and a shear thinning fluid when expressed through a dropper tip. The present study was undertaken to determine how the nonsettling character of LE ophthalmic gel affects dose uniformity. Prednisolone acetate ophthalmic suspension 1% (Pred Forte® and a generic prednisolone acetate suspension 1% were used as comparators.Methods: Drug concentrations of LE ophthalmic gel, Pred Forte, and a generic prednisolone acetate suspension were determined following simulated dosing – consisting of 2 drops, expressed four times daily for 2 weeks, with bottles that were shaken or not shaken immediately prior to expressing the drops. Drug concentrations were determined using a reverse-phase high-performance liquid chromatography (HPLC method and reported as a percentage of the declared (labeled concentration. Comparative kinetics of drug particle sedimentation were also determined for each formulation, using dispersion analysis under gravity.Results: Mean drug concentrations in drops of all three formulations were within a few percentage points of the declared concentration when the bottles were shaken for 5 seconds prior to dispensing. Only LE ophthalmic gel showed consistent and on-target concentrations when the bottles were unshaken prior to dispensing, with a mean (standard deviation [SD] percent declared concentration of 102% (1.92% over the 2-week dosing regimen. Drug concentrations for the branded and generic prednisolone acetate suspensions following expression from unshaken bottles were highly variable (overall relative SDs of 16.8% and 20.3%, respectively, with mean concentrations for both falling significantly

Effect of Shear History on Rheology of Time-Dependent Colloidal Silica Gels

Directory of Open Access Journals (Sweden)

Paulo H. S. Santos

2017-11-01

Full Text Available This paper presents a rheological study describing the effects of shear on the flow curves of colloidal gels prepared with different concentrations of fumed silica (4%, 5%, 6%, and 7% and a hydrophobic solvent (Hydrocarbon fuel, JP-8. Viscosity measurements as a function of time were carried out at different shear rates (10, 50, 100, 500, and 1000 s−1, and based on this data, a new structural kinetics model was used to describe the system. Previous work has based the analysis of time dependent fluids on the viscosity of the intact material, i.e., before it is sheared, which is a condition very difficult to achieve when weak gels are tested. The simple action of loading the gel in the rheometer affects its structure and rheology, and the reproducibility of the measurements is thus seriously compromised. Changes in viscosity and viscoelastic properties of the sheared material are indicative of microstructural changes in the gel that need to be accounted for. Therefore, a more realistic method is presented in this work. In addition, microscopical images (Cryo-SEM were obtained to show how the structure of the gel is affected upon application of shear.

Silica Gel-Mediated Organic Reactions under Organic Solvent-Free Conditions

Directory of Open Access Journals (Sweden)

Satoaki Onitsuka

2012-09-01

Full Text Available Silica gel was found to be an excellent medium for some useful organic transformations under organic solvent-free conditions, such as (1 the Friedel-Crafts-type nitration of arenes using commercial aqueous 69% nitric acid alone at room temperature, (2 one-pot Wittig-type olefination of aldehydes with activated organic halides in the presence of tributyl- or triphenylphosphine and Hunig’s base, and (3 the Morita-Baylis-Hillman reaction of aldehydes with methyl acrylate. After the reactions, the desired products were easily obtained in good to excellent yields through simple manipulation.

Sol-Gel processing of silica nanoparticles and their applications.

Science.gov (United States)

Singh, Lok P; Bhattacharyya, Sriman K; Kumar, Rahul; Mishra, Geetika; Sharma, Usha; Singh, Garima; Ahalawat, Saurabh

2014-11-06

Recently, silica nanoparticles (SNPs) have drawn widespread attention due to their applications in many emerging areas because of their tailorable morphology. During the last decade, remarkable efforts have been made on the investigations for novel processing methodologies to prepare SNPs, resulting in better control of the size, shape, porosity and significant improvements in the physio-chemical properties. A number of techniques available for preparing SNPs namely, flame spray pyrolysis, chemical vapour deposition, micro-emulsion, ball milling, sol-gel etc. have resulted, a number of publications. Among these, preparation by sol-gel has been the focus of research as the synthesis is straightforward, scalable and controllable. Therefore, this review focuses on the recent progress in the field of synthesis of SNPs exhibiting ordered mesoporous structure, their distribution pattern, morphological attributes and applications. The mesoporous silica nanoparticles (MSNPs) with good dispersion, varying morphology, narrow size distribution and homogeneous porous structure have been successfully prepared using organic and inorganic templates. The soft template assisted synthesis using surfactants for obtaining desirable shapes, pores, morphology and mechanisms proposed has been reviewed. Apart from single template, double and mixed surfactants, electrolytes, polymers etc. as templates have also been intensively discussed. The influence of reaction conditions such as temperature, pH, concentration of reagents, drying techniques, solvents, precursor, aging time etc. have also been deliberated. These MSNPs are suitable for a variety of applications viz., in the drug delivery systems, high performance liquid chromatography (HPLC), biosensors, cosmetics as well as construction materials. The applications of these SNPs have also been briefly summarized. Copyright © 2014 Elsevier B.V. All rights reserved.

Sol-gel synthesis of iron catalysers supported on silica and titanium for selectively oxidising methane to formaldehyde

OpenAIRE

Carlos Alberto Guerrero Fajardo; Francisco José Sánchez Castellanos; Anne Cécile Roger; Claire Courson

2010-01-01

Iron materials supported on silica were prepared by the sol-gel method for evaluating catalytic activity in selective o-xidation of methane to formaldehyde. Four catalysts were prepared, one corresponding to the silica support (catalyst 1S), another to the titanium support (catalyst 1T) and two more having 0.5% weight iron loads, one for the silica su-pport (catalyst 2FS) and the last one the titanium support (catalyst 2FT). The higher BET areas were 659 and 850 m2/g for catalysts 1S and 2FS,...

Immobilization of Chlorosulfonyl-Calix[4]arene onto the surface of silica gel through the directly estrification

Science.gov (United States)

Taghvaei-Ganjali, Saeed; Zadmard, Reza; Saber-Tehrani, Mandana

2012-06-01

For the first time Chlorosulfonyl-Calix[4]arene has been chemically bonded to silica gel through the directly estrification without silane coupling agent to prepare Chlorosulfonyl-Calix[4]arene-bonded silica gel. Sample characterization was performed by various techniques such as elemental analysis, Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDAX), powder X-ray diffraction (XRD), N2 adsorption-desorption, thermal gravimetric analysis (TGA), 29Si CP/MAS spectroscopy and acid-base titration. All data approve the successful incorporation of organic group via covalent bond. From the comparison between sulfur content determined by elemental analysis and the number of H+ determined by acid-base titration, it was shown that two ester units took place onto the new synthesized sample and two acidic sites exist on the surface.

Characterization of selenium doped silica glasses synthesized by sol-gel method

International Nuclear Information System (INIS)

Kobayashi, R.A.; Toffoli, S.M.

2012-01-01

Selenium is a rare element in nature. It is used in the food, pharmaceutical, and glass industries. In commercial glasses, selenium is the element responsible for most of the pink or light red color, but its effect is primarily dependent on the oxidation state of the element in the glassy matrix. Besides, selenium is highly volatile, and as high as 80 wt% may be lost in the furnace during the industrial glass elaboration. The sol– gel method yields synthesized materials of high purity and homogeneity, and uses low processing temperatures. Samples of silica glass were obtained by sol-gel method, incorporating precursors of selenium, with the main objective of reducing selenium losses during its heating. The results of optical absorption, XRD and thermal analysis (TGA, DSC) of the glasses are presented and discussed. (author)

Direct measurement of the interaction energy between solids and gases--3. Comparison of the calorimetric titration method with the amine titration method for the determination of acid strength distribution of the silica-alumina surface

Energy Technology Data Exchange (ETDEWEB)

Taniguchi, H.; Masuda, T.; Tsutsumi, K.; Takahashi, H.

1978-07-01

Comparison of the calorimetric titration method with the amine titration method for the determination of acid strength distribution of the silica-alumina surface was carried out for a catalyst containing 13% by wt alumina and evacuated at 400/sup 0/C at 0.00001 mm Hg for five hours. The heats of adsorption of ammonia on silica-alumina poisoned with Hammett indicators of 8.2 to 3.3 pK/sub a/ were also measured to obtain the relation between the dissociation constant of the acid (pK/sub a/) and the heat of adsorption. At pK/sub a/ values of -5.6 and +3.3, the differential heats of adsorption were 76.1 and 55.1 kj/mole, respectively. The number of acid sites calculated from the heat vs. adsorbed-amount curve was about twice as large as that determined by amine titration. The discrepancy is discussed.

NMR of mercury in porous coal and silica gel

International Nuclear Information System (INIS)

Kasperovich, V.S.; Charnaya, E.V.; Tien, C.; Wur, C.S.

2003-01-01

Temperature dependences of the integral intensity and NMR signals Knight shift in 199 Hg nuclei are measured for liquid and solid mercury introduced into the porous coal and silica gel. The decrease in the crystallization completion temperature and small temperature hysteresis (from 4 up to 9 K) between melting and crystallization are identified. Mercury melting temperature in pores coincided with melting temperature of the bulk mercury. NMR signal from crystalline mercury under conditions of limited geometry was observed for the first time. It is ascertained that Knight shift for mercury in the pores both in liquid and crystalline phases is lesser than for the bulk mercury [ru

MECHANISMS CONTROLLING Ca ION RELEASE FROM SOL-GEL DERIVED IN SITU APATITE-SILICA NANOCOMPOSITE POWDER

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Seyed Mohsen Latifi

2015-03-01

Full Text Available Ca ion release from bioactive biomaterials could play an important role in their bioactivity and osteoconductivity properties. In order to improve hydroxyapatite (HA dissolution rate, in situ apatite-silica nanocomposite powders with various silica contents were synthesized via sol-gel method and mechanisms controlling the Ca ion release from them were investigated. Obtained powders were characterized by X-ray diffraction (XRD and transmission electron spectroscopy (TEM techniques, acid dissolution test, and spectroscopy by atomic absorption spectrometer (AAS. Results indicated the possible incorporation of (SiO44- into the HA structure and tendency of amorphous silica to cover the surface of HA particles. However, 20 wt. % silica was the lowest amount that fully covered HA particles. All of the nanocomposite powders showed more Ca ion release compared with pure HA, and HA - 10 wt. % silica had the highest Ca ion release. The crystallinity, the crystallite size, and the content of HA, along with the integrity, thickness, and ion diffusion possibility through the amorphous silica layer on the surface of HA, were factors that varied due to changes in the silica content and were affected the Ca ion release from nanocomposite powders.

Surface-enhanced Raman scattering of amorphous silica gel adsorbed on gold substrates for optical fiber sensors

Science.gov (United States)

Degioanni, S.; Jurdyc, A. M.; Cheap, A.; Champagnon, B.; Bessueille, F.; Coulm, J.; Bois, L.; Vouagner, D.

2015-10-01

Two kinds of gold substrates are used to produce surface-enhanced Raman scattering (SERS) of amorphous silica obtained via the sol-gel route using tetraethoxysilane Si(OC2H5)4 (TEOS) solution. The first substrate consists of a gold nanometric film elaborated on a glass slide by sputter deposition, controlling the desired gold thickness and sputtering current intensity. The second substrate consists of an array of micrometer-sized gold inverted pyramidal pits able to confine surface plasmon (SP) enhancing electric field, which results in a distribution of electromagnetic energy inside the cavities. These substrates are optically characterized to observe SPR with, respectively, extinction and reflectance spectrometries. Once coated with thin layers of amorphous silica (SiO2) gel, these samples show Raman amplification of amorphous SiO2 bands. This enhancement can occur in SERS sensors using amorphous SiO2 gel as shells, spacers, protective coatings, or waveguides, and represents particularly a potential interest in the field of Raman distributed sensors, which use the amorphous SiO2 core of optical fibers as a transducer to make temperature measurements.

Silica sol as grouting material: a physio-chemical analysis.

Science.gov (United States)

Sögaard, Christian; Funehag, Johan; Abbas, Zareen

2018-01-01

At present there is a pressing need to find an environmentally friendly grouting material for the construction of tunnels. Silica nanoparticles hold great potential of replacing the organic molecule based grouting materials currently used for this purpose. Chemically, silica nanoparticles are similar to natural silicates which are essential components of rocks and soil. Moreover, suspensions of silica nanoparticles of different sizes and desired reactivity are commercially available. However, the use of silica nanoparticles as grouting material is at an early stage of its technological development. There are some critical parameters such as long term stability and functionality of grouted silica that need to be investigated in detail before silica nanoparticles can be considered as a reliable grouting material. In this review article we present the state of the art regarding the chemical properties of silica nanoparticles commercially available, as well as experience gained from the use of silica as grouting material. We give a detailed description of the mechanisms underlying the gelling of silica by different salt solutions such as NaCl and KCl and how factors such as particle size, pH, and temperature affect the gelling and gel strength development. Our focus in this review is on linking the chemical properties of silica nanoparticles to the mechanical properties to better understand their functionality and stability as grouting material. Along the way we point out areas which need further research.

Investigating the property profile of polyamide-alumina nanocomposite materials

International Nuclear Information System (INIS)

Sarwar, Muhammad Ilyas; Zulfiqar, Sonia; Ahmad, Zahoor

2009-01-01

Transparent sol-gel-derived nanocomposites were prepared by incorporating an alumina network into a polyamide matrix. Different amounts of aluminum butoxide were hydrolyzed and condensed to produce the alumina network. Thin composite films were characterized in terms of their optical, morphological, mechanical and thermomechanical properties. Tensile modulus, stress at both yield and break points, improved for alumina loadings of 5-10 wt.%. The glass transition temperature increased to 140 o C for nanocomposites containing 15 wt.% alumina. Scanning electron microscopy investigations indicated a uniform distribution of alumina in the polyamide matrix.

Gamma ray irradiation induced optical band gap variations in silica sol-gel doped sucrose

International Nuclear Information System (INIS)

Marzouki, F.; Farah, K.; Hamzaoui, A.H; Ben Ouada, H

2015-01-01

The silica xerogels doped sucrose was prepared via sol-gel process and exposed at room temperature to different doses of high energy ("6"0Co) gamma irradiation. Changes in the UV-visible and FTIR spectra of pristine and irradiated xerogels with varying of gamma doses rays show variation in the gap energy. It was found that energy gap of the investigated silica xerogels decreases with increasing the gamma irradiation doses. Thereby the irradiated samples reveal behaviour changes, from an insulator (Eg ∼5,8 eV) towards a semiconductor with (Eg ∼ 3.5 eV).

Role of pluronics on rheological, drying and crack initiation of 'suckable' gels of decontamination

International Nuclear Information System (INIS)

Bousquet, C.

2007-12-01

The aim of this work was to understand the role of an addition of pluronics on the rheological behaviour, the drying and the fracturing of 'suckable' gels used for nuclear decontamination. The system studied was an aqueous suspension of silica (100 g/L of Aerosil 380) in a strong acidic medium (HNO 3 /H 3 PO 4 1.5 mol/L/1.5 mol/L) in presence of pluronics. Pluronics are amphiphilic tri-blocks copolymers composed of ethylene poly-oxide blocks and of propylene poly-oxide. The first part of this study deals with the characterization of the rheological properties of the gels. From viscosity retaking measurements, flow rheo-grams analysis and the viscoelastic properties of the gels, have been determined an improvement of the rheological properties of the gels significant from the addition of 5 g/L of copolymer. In a second part, the determination of adsorption isotherms coupled to small angles neutrons diffusion measurements has revealed that copolymers are adsorbed flat on silica in bridging the aggregates between them and that the improvement of the rheological behaviour of the gels is due to the increase of the bonds density of the gelled lattice. Moreover, beyond 10 g/L, the adsorption saturation of copolymers at the surface of the silica prevents the bridging of the aggregates which induces the gel destabilization. The last part of this work deals with the characterization of characteristic values of drying and of crack initiation of gels. Then is revealed a relation between the drying kinetics and the formation of cracks in the gel layer. Moreover, the study of the evolution of stresses in the gel layer during time allows to reveal that the addition of pluronics to the formulation of gels allows to improve the gel resistance to the crack initiation and to the delamination. (O.M.)

Does Uniformity of Topical Corticosteroid Ophthalmic Medications: Flourometholone Acetate 0.1 Suspension and Loteprednol Etabonate 0.5 gel

Science.gov (United States)

2017-01-03

following ocular surgery.1 They are available in different forms including emulsions , ointments, solutions, gels, and suspensions. The choice of...study done by Stringer and Bryant compared dose uniformity of difluprednate ophthalmic emulsion (Durezol®) with prednisolone acetate (brand name...topical ophthalmic corticosteroid suspensions. Am J Ophthalmol. 1979;87(2): 210- 214. 5 Flarex® [ package insert]. Fort Worth, TX: Alcon Laboratories Inc

Role of alkyl alcohol on viscosity of silica-based chemical gels for decontamination of highly radioactive nuclear facilities

International Nuclear Information System (INIS)

Choi, B. S.; Yoon, S. B.; Jung, C. H.; Lee, K. W.; Moon, J. K.

2012-01-01

Silica-based chemical gel for the decontamination of nuclear facilities was prepared by using fumed silica as a viscosifier, a 0.5 M Ce (IV) solution dissolved in concentrated nitric acid as a chemical decontamination agent, and tripropylene glycol butyl ether (TPGBE) as a co-viscosifier. A new effective strategy for the preparation of the chemical gel was investigated by introducing the alkyl alcohols as organic solvents to effectively dissolve the co-viscosifier. The mixture solution of the co-viscosifier and alkyl alcohols was more effective in the control of viscosity than that of the co-viscosifier only in gel. Here, the alkyl alcohols played a key role as an effective dissolution solvent for the co-viscosifier in the preparation of the chemical gel, resulting in a reducing of the amount of the co-viscosifier and gel time compared with that of the chemical gel prepared without the alkyl alcohols. It was considered that the alkyl alcohols contributed to the effective dissolution of the co-viscosifier as well as the homogeneous mixing in the formation of the gel, while the co-viscosifier in an aqueous media of the chemical decontamination agent solution showed a lower solubility. The decontamination efficiency of the chemical gels prepared in this work using a multi-channel analyzer (MCA) showed a high decontamination efficiency of over ca. 94% and ca. 92% for Co-60 and Cs-137 contaminated on surface of the stainless steel 304, respectively. (authors)

Influence of a sol–gel alumina coating on oxidation of X20CrMoV12-1 in air up to 650 °C

International Nuclear Information System (INIS)

Schulz, W.; Feigl, M.; Dörfel, I.; Nofz, M.; Kranzmann, A.

2013-01-01

The need for a more efficient coal power plant generation (e.g. oxyfuel technology) results in modified process parameters and enhanced corrosion. To reach the necessary service life of high temperature parts protective coatings may be a sufficient technical solution. A modified Yoldas sol (Al 2 O 3 based) was used to coat X20CrMoV12-1 by spin coating. After appropriate heat treatments transition alumina coatings being about 400 nm thick were obtained. Oxidation studies were carried out in laboratory air at temperatures up to 650 °C for up to 500 h exposure time. In case of the uncoated sample a rough oxide layer formed on the surface and a remarkable weight gain (2.62 mg/cm 2 ) were detected. The sol–gel alumina layer (mainly δ-Al 2 O 3 ) demonstrated a high protection, i.e. a very low weight gain (0.05 mg/cm 2 ). Diffusion of alloying elements into the coating was observed. No indication of spallation of the coating occurred. Local defects (2 μm–30 μm) in the coating led to the formation of iron-oxide islands. - Highlights: • Power plant steel X20 was coated with alumina by sol–gel method. • A 400 nm alumina layer provides good protection up to 650 °C. • Cr and Mn diffusion into Al 2 O 3 supports coating adhesion and protective ability. • Improvement of the coating process must be directed to avoidance of local defects

Retention behaviour of some estradiol derivatives on alumina in normal phase chromatography

Directory of Open Access Journals (Sweden)

MARIJANA M. ACANSKI

2003-03-01

Full Text Available The retention constants of variously substituted estradiol derivatives were measured as a function of the composition of various binary mobile phases in order to study the relationship between chemical structure and retention behaviour in TLC on alumina. The slopes and intercepts of the linear relationships between the retention constant RM and the logarithm of the volume fraction of the polar mobile phase component were calculated and are discussed in relation to the characteristics of the solute and mobile phase. The RFvalues and relative retention DRM of the compounds depend largely on the retention behaviour of their substituents. The results obtained in this investigation are compared with the results of the same derivatives obtained in previous investigations on silica gel.

Preparation of Bragg mirrors on silica optical fibers and inner walls of silica capillaries by employing the sol-gel method, and titanium and silicon alkoxides

Czech Academy of Sciences Publication Activity Database

Bartoň, Ivo; Matějec, Vlastimil; Mrázek, Jan; Podrazký, Ondřej; Matoušek, J.

2017-01-01

Roč. 81, č. 3 (2017), s. 867-879 ISSN 0928-0707 R&D Projects: GA ČR GA16-10019S Grant - others:AV ČR(CZ) SAV-16-17 Program:Bilaterální spolupráce Institutional support: RVO:67985882 Keywords : Multilayered coatings * Silica and titania layersSilica and titania layers * Alkoxide sol–gel method Subject RIV: JA - Electronics ; Optoelectronics, Electrical Engineering OBOR OECD: Electrical and electronic engineering Impact factor: 1.575, year: 2016

A new approach to the silica gel surface : characterization of different surface regions by 29Si magic angle spinning NMR relaxation parameters and consequences for quantification of silica gels by NMR: characterization of different surface regions by silicon-29 magic angle spinning NMR relaxation parameters and consequences for quantification of silica gels by NMR

NARCIS (Netherlands)

Pfleiderer, B.; Albert, K.; Bayer, E.; Ven, van de L.J.M.; Haan, de J.W.; Cramers, C.A.M.G.

1990-01-01

Native and some monofunctionally derivatized silica gels have been investigated by 29Si CP MAS NMR spectroscopy with pulse and with cross-polarization (CP) excitation. Contact time variation experiments for some native materials yield results for the siloxane (Q4)g roups which cannot be described

Immobilization of Chlorosulfonyl-Calix[4]arene onto the surface of silica gel through the directly estrification

Energy Technology Data Exchange (ETDEWEB)

Taghvaei-Ganjali, Saeed, E-mail: S-taghvaei@IAU-tnb.ac.ir [Chemistry Department, Islamic Azad University, North Tehran Branch, Postal Code: 1913674711, Tehran (Iran, Islamic Republic of); Zadmard, Reza [Chemistry and Chemical Engineering Research Center of Iran, Postal Code: 1496813151, Tehran (Iran, Islamic Republic of); Saber-Tehrani, Mandana [Chemistry Department, Islamic Azad University, North Tehran Branch, Postal Code: 1913674711, Tehran (Iran, Islamic Republic of)

2012-06-01

For the first time Chlorosulfonyl-Calix[4]arene has been chemically bonded to silica gel through the directly estrification without silane coupling agent to prepare Chlorosulfonyl-Calix[4]arene-bonded silica gel. Sample characterization was performed by various techniques such as elemental analysis, Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDAX), powder X-ray diffraction (XRD), N{sub 2} adsorption-desorption, thermal gravimetric analysis (TGA), {sup 29}Si CP/MAS spectroscopy and acid-base titration. All data approve the successful incorporation of organic group via covalent bond. From the comparison between sulfur content determined by elemental analysis and the number of H{sup +} determined by acid-base titration, it was shown that two ester units took place onto the new synthesized sample and two acidic sites exist on the surface.

Characterization and sintering of niobium-ATR alumina

International Nuclear Information System (INIS)

Sibuya, N.H.; Iwasaki, H.; Suzuki, C.K.; Pinatti, D.G.

1987-01-01

In the niobium aluminothermy a slag is produced, composed mostly of alumina and other compounds such as niobium oxide and silica. The phase composition of this ATR alumina was characterized by X-ray powder diffractometry, and afterwards this alumina was subjected to leaching processes. It was noticed that the original content of 70% α-alumina in slag rose to 95% after the calcination. ATR alumina (leached and calcined, and without any treatment) was used to make pressed bodies which were fired in air at 1200 to 1400 0 C for 1 to 10,5 hours; and in vacuum at 1550 to 1800$0C for 2 hours. Characterization was done by density measurements, X-ray diffractometry and ultrasonic analysis. Ultrasonic analysis of some vacuum fired bodies showed londitudinal velocities close to the value found in literature. Correlation of several techniques measurements disclosed the niobium oxide interference in sintering. (Author) [pt

Studies on silica sol-clay particle interactions by small-angle neutron scattering

International Nuclear Information System (INIS)

Moini, A.; Pinnavaia, T.J.; Michigan State Univ., East Lansing; Thiyagarajan, P.; White, J.W.

1988-01-01

SANS data were collected on a series of hydrolyzed silica and silica-clay complexes prepared from a 40 A silica sol and aqueous suspensions of Na + montmorillonite. The hydrolyzed silica product showed a peak centered at Q=0.0856 A -1 corresponding to a distance of 73 A between the sol particles. For such an evaporated gel in which the particles are in close contact, this distance is expected to be very close to the particle diameter indicating partial aggregation of the original spheres. A similar feature was observed in the SANS data for silica-clay products indicating the presence of some unintercalated silica. The intensity of this scattering was found to be dependent on the silica:clay ratio and the reaction time. The SANS data in the region from Q=0.006 to 0.025 A -1 were characteristic of clay scattering and exhibited a power-law behavior. The change in the slope of this curve upon reaction of the clay with the silica sol was interpreted in terms of a separation of clay platelets caused by a binding interaction with the sol particles. (orig.)

Solid-phase microextraction Ni-Ti fibers coated with functionalised silica particles immobilized in a sol-gel matrix.

Science.gov (United States)

Azenha, Manuel; Ornelas, Mariana; Fernando Silva, A

2009-03-20

One of the possible approaches for the development of novel solid-phase microextraction (SPME) fibers is the physical deposition of porous materials onto a support using high-temperature epoxy glue. However, a major drawback arises from decomposition of epoxy glue at temperatures below 300 degrees C and instability in some organic solvents. This limitation motivated us to explore the possibility of replacing the epoxy glue with a sol-gel film, thermally more stable and resistant to organic solvents. We found that functionalised silica particles could be successfully attached to a robust Ni-Ti wire by using a UV-curable sol-gel film. The particles were found to be more important than the sol-gel layer during the microextraction process, as shown by competitive extraction trials and by the different extraction profiles observed with differently functionalised particles. If a quality control microscopic-check aiming at the rejection of fibers exhibiting unacceptably low particle load was conducted, acceptable (6-14%) reproducibility of preparation of C(18)-silica fibers was observed, and a strong indication of the durability of the fibers was also obtained. A cyclohexyldiol-silica fiber was used, as a simple example of applicability, for the successful determination of benzaldehyde, acetophenone and dimethylphenol at trace level in spiked tap water. Recoveries: 95-109%; limits of detection: 2-7 microg/L; no competition effects within the studied range (

ANALISA DAYA SERAP SILIKA GEL BERBAHAN DASAR ABU SEKAM PADI

Directory of Open Access Journals (Sweden)

Hendriwan Fahmi

2016-08-01

Full Text Available Rice husk ash Silica Gel is aproduct which call be used in preventing the humidity by absorbing the water ion on the water andonthe air. This absorbing isbased onthe size, the composition and the total amount ofpolluter which contained on the Silica Gel. The purpose of making this silica gel is to seehow much thiskind of Silica Gel can absorb and compare it to the synthetic one,and also processing rise husk ashto be something useful, Ion water can be absorbed much more by using this natural silica gel if it is compared to the synthetic silica gel. This is because of its capable inabsorbing more –OHand O from water and air. Afterdoing a research with column method, silica gel was beingput in 50 ml water. Fromthis research, natural silica can absorb much more water (0.0010 gr/ml, 0.285 % water level ofweigh in comparing with synthetic one (0.008gr/ml with 0.248 %water level ofweight andsintering (0,007 gr/ml 0.253%water level and non-sintering silica gel contains 39.22 % weight of silica, 30.93 %weight of sintering silica gel, and 33.40 % of the synthetic. More silica and water level, means more total amount of absorbing. This silica gel application is considered with capability ofabsorbing andthe level of the water.

Bio sorption process for uranium (VI) by using algae-yeast-silica gel composite adsorbent

International Nuclear Information System (INIS)

Turkozu, D. A.; Aytas, S.

2006-01-01

Many yeast, algae, bacteria and various aquatic flora are known to be capable of concentrating metal species from dilute aqueous solution. Many researcher have found that non-living biomaterials can be used to accumulate metal ions from environment. In recent studies, mainly two process are used in biosorption experiments. These are the use of free cells and the use of immobilized cells on a solid support. A variety of inert supports have been used to immobilize biomaterials either by adsorption or physical entrapment. This uptake is often considerable and frequently selective, and occurs via a variety of mechanisms including active transport, ion exchange or complexation, and adsorption or inorganic precipitation. Biosorbent may be used as an ion exchange material. Adsorption occurs through interaction of the metal ions with functional groups that are found in the cell wall biopolymers of either living or dead organisms. In this study, the algae-yeast-silica gel composite adsorbent was tested for its ability to recover U(VI) from diluted aqueous solutions. Macro marine algae (Jania rubens.), yeast (Saccharomyces cerevisiae) and silica gel were used to prepare composite adsorbent. The ability of the composite biosorbent to adsorb uranium (VI) from aqueous solution has been studied at different optimized conditions of pH, concentration of U(VI), temperature, contact time and matrix ion effect was also investigated. The adsorption patterns of uranium on the composite biosorbent were investigated by the Langmuir, Freundlich and Dubinin-Radushkhevic isotherms. The thermodynamic parameters such as variation of enthalpy ΔH, variation of entropy ΔS and variation of Gibbs free energy ΔG were calculated. The results suggested that the macro algae-yeast-silica gel composite sorbent is suitable as a new biosorbent material for removal of uranium ions from aqueous solutions

Aspectos da Reologia e da Estabilidade de Suspensões Cerâmicas. Parte III: Mecanismo de Estabilização Eletroestérica de Suspensões com Alumina Aspects of Rheology and Stability of Ceramic Suspensions. Part III: Electrosteric Stabilization Mechanism of Alumina Suspensions

Directory of Open Access Journals (Sweden)

F. S. Ortega

1997-08-01

Full Text Available Esta terceira e última parte da revisão sobre os aspectos reológicos e de estabilização de suspensões com pós cerâmicos vem reunir a aplicação dos conhecimentos adquiridos nas primeiras duas partes publicadas anteriormente. Aqui, os fenômenos eletrostático devido à dupla camada elétrica, e estérico, relacionado à adsorção de moléculas poliméricas, são combinados para explicar o mecanismo eletroestérico de estabilização de suspensões cerâmicas. Os defloculantes que atuam através desse mecanismo abrangem uma classe específica de polímero denominada polieletrólitos, a qual é constituída por macromoléculas ionizáveis quando em solução. O estudo da forma com que os polieletrólitos atuam justifica-se devido à larga utilização desta classe de polímeros na indústria cerâmica. Os ácidos poliacrílico (PAA e polimetacrílico (PMAA são exemplos de polieletrólitos amplamente utilizados no processo de materiais à base de alumina. Dá-se destaque à influência do pH do meio e da presença de íons, sendo novamente aqui importante o conceito de força iônica da suspensão. Como aplicação prática, apresenta-se a estabilidade do sistema alumina-PMAA, reportando-se sobre o comportamento da viscosidade e da efetiva defloculação da suspensão. Este estudo é concluído apresentando resultados do efeito do peso molecular sobre a viscosidade, chamando atenção para o fato de que não basta definir apenas a classe de polímero a ser usada, sendo também fundamental especificar o peso molecular médio do polímero selecionado.The third and last part of this review about stabilization and rheological aspects of ceramic suspension gathers the knowledge in the two parts previously published. Here, the electrostatic and steric phenomena, related to the electrical double layer and polymeric molecules adsorption, respectively, are combined to explain the electrosteric stabilization mechanism of ceramic suspensions. The

Role of pluronics on rheological, drying and crack initiation of 'suckable' gels of decontamination; Role des pluronics sur les proprietes rheologiques, de sechage et de fracturation des gels 'aspirables' de decontamination

Energy Technology Data Exchange (ETDEWEB)

Bousquet, C

2007-12-15

The aim of this work was to understand the role of an addition of pluronics on the rheological behaviour, the drying and the fracturing of 'suckable' gels used for nuclear decontamination. The system studied was an aqueous suspension of silica (100 g/L of Aerosil 380) in a strong acidic medium (HNO{sub 3}/H{sub 3}PO{sub 4} 1.5 mol/L/1.5 mol/L) in presence of pluronics. Pluronics are amphiphilic tri-blocks copolymers composed of ethylene poly-oxide blocks and of propylene poly-oxide. The first part of this study deals with the characterization of the rheological properties of the gels. From viscosity retaking measurements, flow rheo-grams analysis and the viscoelastic properties of the gels, have been determined an improvement of the rheological properties of the gels significant from the addition of 5 g/L of copolymer. In a second part, the determination of adsorption isotherms coupled to small angles neutrons diffusion measurements has revealed that copolymers are adsorbed flat on silica in bridging the aggregates between them and that the improvement of the rheological behaviour of the gels is due to the increase of the bonds density of the gelled lattice. Moreover, beyond 10 g/L, the adsorption saturation of copolymers at the surface of the silica prevents the bridging of the aggregates which induces the gel destabilization. The last part of this work deals with the characterization of characteristic values of drying and of crack initiation of gels. Then is revealed a relation between the drying kinetics and the formation of cracks in the gel layer. Moreover, the study of the evolution of stresses in the gel layer during time allows to reveal that the addition of pluronics to the formulation of gels allows to improve the gel resistance to the crack initiation and to the delamination. (O.M.)

Determination of arsenate in water by anion selective membrane electrode using polyurethane–silica gel fibrous anion exchanger composite

Energy Technology Data Exchange (ETDEWEB)

Khan, Asif Ali, E-mail: asifkhan42003@yahoo.com; Shaheen, Shakeeba, E-mail: shakeebashaheen@ymail.com

2014-01-15

Highlights: • PU–Si gel is new anion exchanger material synthesized and characterized. • This material used as anion exchange membrane is applied for electroanalytical studies. • The method for detection and determination of AsO{sub 4}{sup 3−} in traces amounts discussed. • The results are also verified from arsenic analyzer. -- Abstract: Polyurethane (PU)–silica (Si gel) based fibrous anion exchanger composites were prepared by solid–gel polymerization of polyurethane in the presence of different amounts of silica gel. The formation of PU–Si gel fibrous anion exchanger composite was characterized by Fourier transform infra-red spectroscopy (FTIR), X-ray diffraction (XRD), thermogravimetric analysis (TGA-DTA), scanning electron microscopy (SEM) and elemental analysis. The membrane having a composition of 5:3 (PU:Si gel) shows best results for water content, porosity, thickness and swelling. Our studies show that the present ion selective membrane electrode is selective for arsenic, having detection limit (1 × 10{sup −8} M to 1 × 10{sup −1} M), response time (45 s) and working pH range (5–8). The selectivity coefficient values for interfering ions indicate good selectivity for arsenate (AsO{sub 4}{sup 3−}) over interfering anions. The accuracy of the detection limit results was compared by PCA-Arsenomat.

Synthesis of mesoporous silica nanoparticles by sol–gel as nanocontainer for future drug delivery applications

Energy Technology Data Exchange (ETDEWEB)

Vazquez, N.I.; Gonzalez, Z.; Ferrari, B.; Castro, Y.

2017-07-01

Development of mesoporous silica nanoparticles as carriers for drug delivery systems has increased exponentially during the last decade. The present work is focused on the synthesis of silica carriers by sol–gel from tetraethyl orthosilicate (TEOS) as precursor of silica and cetyltrimethylammonium bromide (CTAB) as pore generating agent. The synthesis conditions were modified varying the molar ratio of water/TEOS, NH3/TEOS and amount of CTAB. The silica particles were characterized by scan electron microscopy techniques (FESEM), high resolution transmission electron microscopy (HR-TEM), N2 adsorption–desorption isotherms, Zeta-potential and Dynamic Light Scattering (DLS). The results show that the specific surface area and the porosity of silica particles were strongly affected by the addition of CTAB and the amount of H2O. The dispersion and stability of silica mesoporous particles is achieved in spite of the high surface reactivity. The synthesis formulation affects considerably to the particle morphology, which changes from spheres to rods when the molar ratio of H2O increases. A maximum specific surface area of 1480m2/g was obtained with pore sizes ranging 2.5–2.8nm. (Author)

Silica-gel Catalyzed Facile Synthesis of 3,4-Dihydropyrimidinones

International Nuclear Information System (INIS)

Agarwal, Sameer; Aware, Umesh; Patil, Amit; Rohera, Vinita; Jain, Mukul; Patel, Pankaj; Ghate, Manjunath

2012-01-01

We have developed a mild and highly effective procedure for the one-pot synthesis of substituted dihydropyrimidinones in high yields using silica gel as a green, highly efficient and recyclable heterogeneous catalyst. Our approach can be applied to the preparation of a wide range of synthetic analogues for structure-activity studies. Investigations in this direction are ongoing. The pyrimidinone ring is a basic substructure of numerous biologically active alkaloids and pharmaceutical products. These cores are regarded as one of the most important groups of drug-like scaffolds. 3,4-dihydropyrimidinones above are known to exhibit variety of pharmacological activity such as calcium channel modulation, mitotic kinesin Eg5 inhibition, antiviral, anti-inflammatory, antibacterial activity, etc

Silica-gel Catalyzed Facile Synthesis of 3,4-Dihydropyrimidinones

Energy Technology Data Exchange (ETDEWEB)

Agarwal, Sameer; Aware, Umesh; Patil, Amit; Rohera, Vinita; Jain, Mukul; Patel, Pankaj [Zydus Research Centre, Sarkhej-Bavla N.H., Ahmedabad (India); Ghate, Manjunath [Nirma University, Ahmedabad (India)

2012-02-15

We have developed a mild and highly effective procedure for the one-pot synthesis of substituted dihydropyrimidinones in high yields using silica gel as a green, highly efficient and recyclable heterogeneous catalyst. Our approach can be applied to the preparation of a wide range of synthetic analogues for structure-activity studies. Investigations in this direction are ongoing. The pyrimidinone ring is a basic substructure of numerous biologically active alkaloids and pharmaceutical products. These cores are regarded as one of the most important groups of drug-like scaffolds. 3,4-dihydropyrimidinones above are known to exhibit variety of pharmacological activity such as calcium channel modulation, mitotic kinesin Eg5 inhibition, antiviral, anti-inflammatory, antibacterial activity, etc.

An identification of the soft polyelectrolyte gel-like layer on silica colloids using atomic force and electron microscopy.

Science.gov (United States)

Škvarla, Jiří; Škvarla, Juraj

2017-10-01

A procedure is introduced for measuring the radius of spherical colloid particles from the curvature of upper parts of their central cross-sectional profiles obtained by atomic force microscopy (AFM). To minimize the possible compression and displacement of the spheres, AFM is operated in a mode rendering a constant ultralow pN force on the tip. The procedure allows us to evaluate the mean radius of nearly monodisperse submicrometer spheres of silica in their natively hydrated state in aqueous electrolyte solutions, irrespective of whether they are coagulated or not. A variation in the volume (swelling degree) of layers delimited by the AFM mean radii of these spheres in KCl solutions and their invariable mean radius in vacuum is obtained that follows a scaling power law derived in polymer physics for swellable polyelectrolyte gels and deduced previously by us from coagulation tests. This supports our former suggestion about the existence of soft polyelectrolyte gel-like layer developed spontaneously around silica surfaces and colloids. We discuss this finding in the context of recent knowledge about the structure of the silica/water interface obtained from direct surface force measurements between macroscopic silica surfaces and from particle size measurements of silica colloids and highlight its importance for colloid chemistry and condensed mattter physics. Copyright © 2017 Elsevier B.V. All rights reserved.

Synthesis of nanocrystalline LaF3 doped silica glasses by hydrofluoric acid catalyzed sol–gel process

International Nuclear Information System (INIS)

Nagayama, Shuhei; Kajihara, Koichi; Kanamura, Kiyoshi

2012-01-01

Highlights: ► Silica glasses doped by LaF 3 nanocrystals are obtained by HF-catalyzed sol–gel method. ► The processing time (∼1 week) is much shorter than that of previous studies. ► The uptake of SiF groups in the glass matrix greatly reduces the SiOH concentration. ► Effects of sintering conditions and properties of Er 3+ -doped samples are presented. - Abstract: Silica glasses doped with LaF 3 nanocrystals were prepared by HF-catalyzed sol–gel method. HF was used both as fluorine source and as catalyst of the sol–gel reaction, making it possible to shorten the processing time with reducing the concentration of SiOH groups to ∼10 18 cm −3 . The resultant glasses are transparent at visible spectral range, and the optical loss at the ultraviolet absorption edge is dominated by the Rayleigh scattering from LaF 3 crystallites. The size of LaF 3 crystallites increases with an increase in the sintering temperature and time, and is smaller than ∼40 nm in samples showing good visible transparency. Green upconversion photoluminescence is observed in an Er 3+ -doped sample under excitation at 980 nm.

Influence of a sol–gel alumina coating on oxidation of X20CrMoV12-1 in air up to 650 °C

Energy Technology Data Exchange (ETDEWEB)

Schulz, W., E-mail: wencke.schulz@bam.de [BAM Federal Institute for Materials Research and Testing, Unter den Eichen 87, 12205 Berlin (Germany); Feigl, M. [BAM Federal Institute for Materials Research and Testing, Unter den Eichen 87, 12205 Berlin (Germany); Fügetechnik Berlin-Brandenburg GmbH, Kupferhammerweg 14-18, 16227 Eberswalde (Germany); Dörfel, I.; Nofz, M.; Kranzmann, A. [BAM Federal Institute for Materials Research and Testing, Unter den Eichen 87, 12205 Berlin (Germany)

2013-07-31

The need for a more efficient coal power plant generation (e.g. oxyfuel technology) results in modified process parameters and enhanced corrosion. To reach the necessary service life of high temperature parts protective coatings may be a sufficient technical solution. A modified Yoldas sol (Al{sub 2}O{sub 3} based) was used to coat X20CrMoV12-1 by spin coating. After appropriate heat treatments transition alumina coatings being about 400 nm thick were obtained. Oxidation studies were carried out in laboratory air at temperatures up to 650 °C for up to 500 h exposure time. In case of the uncoated sample a rough oxide layer formed on the surface and a remarkable weight gain (2.62 mg/cm{sup 2}) were detected. The sol–gel alumina layer (mainly δ-Al{sub 2}O{sub 3}) demonstrated a high protection, i.e. a very low weight gain (0.05 mg/cm{sup 2}). Diffusion of alloying elements into the coating was observed. No indication of spallation of the coating occurred. Local defects (2 μm–30 μm) in the coating led to the formation of iron-oxide islands. - Highlights: • Power plant steel X20 was coated with alumina by sol–gel method. • A 400 nm alumina layer provides good protection up to 650 °C. • Cr and Mn diffusion into Al{sub 2}O{sub 3} supports coating adhesion and protective ability. • Improvement of the coating process must be directed to avoidance of local defects.

Preparation of silane-functionalized silica films via two-step dip coating sol–gel and evaluation of their superhydrophobic properties

International Nuclear Information System (INIS)

Ramezani, Maedeh; Vaezi, Mohammad Reza; Kazemzadeh, Asghar

2014-01-01

Highlights: • Superhydrophobic silica film was prepared by sol–gel process. • The surfaces exhibited superhydrophobicity with water contact angle greater than 150°. • AFM images showed the roughness increases with increasing the percentage of silylation agent. • Before and after modification, the particle size of silica was lower than 50 nm. - Graphical abstract: Schematic illustration of the surface modification of the silica nanoparticle by iso-OTMS on the glass substrate. - Abstract: In this paper, we study the two-step dip coating via a sol–gel process to prepare superhydrophobic silica films on the glass substrate. The water repellency of the silica films was controlled by surface silylation method using isooctyltrimethoxysilane (iso-OTMS) as a surface modifying agent. Silica alcosol was synthesized by keeping the molar ratio of ethyltriethoxysilane (ETES) precursor, ethanol (EtOH) solvent, water (H 2 O) was kept constant at 1:36:6.6 respectively, with 6 M NH 4 OH throughout the experiment and the percentages of hydrophobic agent in hexane bath was varied from 0 to 15 vol.%. The static water contact angle values of the silica films increased from 108° to 160° with an increase in the vol.% of iso-OTMS. At 15 vol%. of iso-OTMS, the silica film shows static water contact angle as high as 160°. The superhydrophobic silica films are thermally stable up to 440 °C and above this temperature, the silica films lose superhydrophobicity. By controlling the primer particle size of SiO 2 about 26 nm, leading to decrease the final size of silica nanoparticles after modification of nanoparticles by isooctyltrimethoxysilane about 42 nm. The films are transparent and have uniform size on the surface. The silica films have been characterized by atomic force microscopy (AFM), fourier transform infrared spectroscopy (FT-IR), transparency, contact angle measurement (CA), Zeta-potential, Thermal stability by TG–DTA analysis

Evaluation of technological properties of alumina refractory systems-zirconia and zirconia-silica-alumina

International Nuclear Information System (INIS)

Marinho, A.R.O.; Carvalho, T.U.S.; Fagury Neto, E.; Rabelo, A.A.

2014-01-01

Alumina-zirconia refractories are noted for being products of excellent cost-effective, however, zirconia may limit its use due to decreasing resistance to thermal shock. This study aims to evaluate these refractories with the addition of microsilica, which can greatly improve their properties. Were used the following starting materials: calcined alumina, zirconia (stabilized and monoclinic) in amounts of 2%, 4% and 6% by weight, plus microsilica (5%w.). The powders were milled together with binder and lubricant for conformation bodies by uniaxial pressing. The samples were dried, calcined and sintered at 1400 °C/2h were characterized using the methods of Archimedes, and scanning electron microscopy (SEM), chemical analysis using energy dispersive X-ray (EDS), and mechanical flexural strength tests at room temperature. Formulations with the presence of microsilica showed satisfactory results and optimized properties. (author)

High toughness alumina/aluminate: The role of hetero-interfaces

International Nuclear Information System (INIS)

Brito, M.E.; Yasuoka, M.; Kanzaki, S.

1996-01-01

Silica doped alumina/aluminate materials present a combination of high strength and high toughness not achieved before in other alumina systems, except for transformation toughened alumina. The authors have associated the increase in toughness to crack bridging by anisotropically grown alumina grains with concurrent interfacial debonding of these grains. A HREM study of grain boundaries and hetero-interface structures in this material shows the absence of amorphous phases at grain boundaries. Local Auger electron analysis of fractured surfaces revealed the coexistence of Si and La at the grain facets exposed by the noticeable intergranular fracture mode of this material. It is concluded that a certain and important degree of boundaries weakness is related to both presence of Si at the interfaces and existence of alumina/aluminate hetero-interfaces

Superparamagnetic iron oxide nanoparticles incorporated into silica nanoparticles by inelastic collision via ultrasonic field: Role of colloidal stability

Energy Technology Data Exchange (ETDEWEB)

Sodipo, Bashiru Kayode; Azlan, Abdul Aziz [Nano-Optoelectronics Research and Technology (NOR) Lab, School of Physics, Universiti Sains Malaysia, 11800 Pulau Pinang, Malaysia Nano-Biotechnology Research (Malaysia); Innovation (NanoBRI), Institute for Research in Molecular Medicine (INFORMM), Universiti Sains Malaysia, 11800, Pulau Pinang (Malaysia)

2015-04-24

Superparamagnetic iron oxide nanoparticles (SPION)/Silica composite nanoparticles were prepared by ultrasonically irradiating colloidal suspension of silica and SPION mixture. Both silica and SPION were synthesized independently via co-precipitation and sol-gel method, respectively. Their mixtures were sonicated at different pH between 3 and 5. Electrophoresis measurement and other physicochemical analyses of the products demonstrate that at lower pH SPION was found incorporated into the silica. However, at pH greater than 4, SPION was unstable and unable to withstand the turbulence flow and shock wave from the ultrasonic field. Results suggest that the formation of the SPION/silica composite nanoparticles is strongly related to the inelastic collision induced by ultrasonic irradiation. More so, the formation the composite nanoparticles via the ultrasonic field are dependent on the zeta potential and colloidal stability of the particles.

Bidisperse silica nanoparticles close-packed monolayer on silicon substrate by three step spin method

Science.gov (United States)

Khanna, Sakshum; Marathey, Priyanka; Utsav, Chaliawala, Harsh; Mukhopadhyay, Indrajit

2018-05-01

We present the studies on the structural properties of monolayer Bidisperse silica (SiO2) nanoparticles (BDS) on Silicon (Si-100) substrate using spin coating technique. The Bidisperse silica nanoparticle was synthesised by the modified sol-gel process. Nanoparticles on the substrate are generally assembled in non-close/close-packed monolayer (CPM) form. The CPM form is obtained by depositing the colloidal suspension onto the silicon substrate using complex techniques. Here we report an effective method for forming a monolayer of bidisperse silica nanoparticle by three step spin coating technique. The samples were prepared by mixing the monodisperse solutions of different particles size 40 and 100 nm diameters. The bidisperse silica nanoparticles were self-assembled on the silicon substrate forming a close-packed monolayer film. The scanning electron microscope images of bidisperse films provided in-depth film structure of the film. The maximum surface coverage obtained was around 70-80%.

Adsorption of Pb(II) using silica gel composite from rice husk ash modified 3-aminopropyltriethoxysilane (APTES)-activated carbon from coconut shell

Science.gov (United States)

Yusmaniar, Purwanto, Agung; Putri, Elfriyana Awalita; Rosyidah, Dzakiyyatur

2017-03-01

Silica gel modified by 3-aminopropyltriethoxysilane (APTES) was synthesized from rice husk ash combined with activated carbon from coconut shell yielded the composite adsorbent. The composite was characterized by Fourier Transform Infra Red spectroscopy (FT-IR), Electron Dispersive X-Ray (EDX), Surface Area Analyzer (SAA) and adsorption test by Atomic Absorption Spectrometry (AAS). This composite adsorbent has been used moderately for the removal of lead ions from metal solutions and compared with silica gel modified APTES and activated carbon. The adsorption experiments of Pb -ions by adsorbents were performed at different pH and contact time with the same metal solutions concentration, volume solution, and adsorbent dosage. The optimum pH for the adsorption was found to be 5.0 and the equilibrium was achieved for Pb with 20 min of contact time. Pb ions adsorption by composite silica gel modified APTES-activated carbon followed by Langmuir isotherm model with qmax value of 46.9483 mg/g that proved an adsorbent mechanism consistent to the mechanism of monolayer formation.

The Intervention of Sucralfate Suspension Gel on Paraquat Poisoned Patients%硫糖铝干预百草枯中毒的研究

Institute of Scientific and Technical Information of China (English)

朱峻波; 于勇涛; 李洪波; 郑粉双; 苏敬; 杨春爱

2016-01-01

目的：探讨硫糖铝治疗百草枯中毒患者的疗效。方法：将100例百草枯中毒的患者分成两组，对照组（50例）与硫糖铝治疗组（50）例，经治疗后对比病人的死亡率，生存率和肺损伤的情况。结果：硫糖铝治疗组病人肺损伤下降，出院时间缩短。结论：早期使用硫糖铝进行胃肠灌洗的病人肺损伤下降，提高了生存率。%Objective: To investigate the effect of sucralfate suspension gel in paraquat-poisoned patients. Methods: 100 paraquat-poisoned patients were divided into two groups: control group (50) and sucralfate suspension gel group (50). The death rate, survival rate and the acute lung injury of the patients after treatment were compared between two groups. Results: The acute lung injury in the sucralfate suspension gel group more reduced, and their recovery time was shorter. Conclusions: Early use of sucralfate suspension gel reduced the acute lung injury reduced, improved the survival rate in paraquat-poisoned patients.

Investigation of Removal Possibilities of Colloidal Alumina from Aqueous Solution by the Use of Anionic Polyacrylamide

International Nuclear Information System (INIS)

Wisniewska, M.; Chibowski, S.; Urban, T.

2016-01-01

Purification of drinking and industrial water required usage of high molecular weight polymer to cause flocculation process of dispersed suspension of contaminants. Poly electrolytes, including ionic polyacrylamide are especially appropriate for these purposes, because in this case the suspension stability can be controlled by both steric and electrostatic forces. Thus the influence of solution p H and hydrolysis degree (carboxyl groups content) of anionic polyacrylamide (PAM) on the alumina (Al_2O_3) suspension stability were studied. The turbidimetry was applied for determination of the examined systems stability. The mechanism of suspension stabilization or destabilization in the polymer presence was proposed on the basis of determined parameters: adsorbed amount of PAM, its adsorption layer thickness, linear dimensions of macromolecules in the solution and zeta potential of alumina particles covered with the polyacrylamide layer. The greatest decrease of the alumina suspension stability in the polymer presence in comparison to that without the polymer was obtained at p H 6 after the addition of PAMs with higher molecular weight (i.e. 14 000 0000) and hydrolysis degrees 20 and 30% (efficient neutralization of solid surface charge). In turn, the most unstable alumina system proved to be that prepared at p H 9 containing PAM with the highest molecular weight and the greatest hydrolysis degree (causing the most effective bridging flocculation).

Simple and Efficient Synthesis of Iron Oxide-Coated Silica Gel Adsorbents for Arsenic Removal: Adsorption Isotherms and Kinetic Study

Energy Technology Data Exchange (ETDEWEB)

Arifin, Eric; Lee, Jiukyu [Interdisciplinary Program in Nanoscience and Technology, Virginia (United States); Cha, Jinmyung [Seoul National Univ., Seoul (Korea, Republic of)

2013-08-15

Iron oxide (ferrihydrite, hematite, and magnetite) coated silica gels were prepared using a low-cost, easily-scalable and straightforward method as the adsorbent material for arsenic removal application. Adsorption of the anionic form of arsenic oxyacids, arsenite (AsO{sup 2-}) and arsenate (AsO{sub 4}{sup -3}), onto hematite coated silica gel was fitted against non-linear 3-parameter-model Sips isotherm and 2-parameter-model Langmuir and Freundlich isotherm. Adsorption kinetics of arsenic could be well described by pseudo-second-order kinetic model and value of adsorption energy derived from non-linear Dubinin-Radushkevich isotherm suggests chemical adsorption. Although arsenic adsorption process was not affected by the presence of sulfate, chloride, and nitrate anions, as expected, bicarbonate and silicate gave moderate negative effects while the presence of phosphate anions significantly inhibited adsorption process of both arsenite and arsenate. When the actual efficiency to remove arsenic was tested against 1 L of artificial arsenic-contaminated groundwater (0.6 mg/L) in the presence competing anions, the reasonable amount (20 g) of hematite coated silica gel could reduce arsenic concentration to below the WHO permissible safety limit of drinking water of 10 μg/L without adjusting pH and temperature, which would be highly advantageous for practical field application.

Development of vapor deposited silica sol-gel particles for use as a bioactive materials system.

Science.gov (United States)

Snyder, Katherine L; Holmes, Hallie R; VanWagner, Michael J; Hartman, Natalie J; Rajachar, Rupak M

2013-06-01

Silica-based sol-gel and bioglass materials are used in a variety of biomedical applications including the surface modification of orthopedic implants and tissue engineering scaffolds. In this work, a simple system for vapor depositing silica sol-gel nano- and micro-particles onto substrates using nebulizer technology has been developed and characterized. Particle morphology, size distribution, and degradation can easily be controlled through key formulation and manufacturing parameters including water:alkoxide molar ratio, pH, deposition time, and substrate character. These particles can be used as a means to rapidly modify substrate surface properties, including surface hydrophobicity (contact angle changes >15°) and roughness (RMS roughness changes of up to 300 nm), creating unique surface topography. Ions (calcium and phosphate) were successfully incorporated into particles, and induced apatitie-like mineral formation upon exposure to simulated body fluid Preosteoblasts (MC3T3) cultured with these particles showed up to twice the adhesivity within 48 h when compared to controls, potentially indicating an increase in cell proliferation, with the effect likely due to both the modified substrate properties as well as the release of silica ions. This novel method has the potential to be used with implants and tissue engineering materials to influence cell behavior including attachment, proliferation, and differentiation via cell-material interactions to promote osteogenesis. Copyright © 2012 Wiley Periodicals, Inc.

Analysis of sorption into single ODS-silica gel microparticles in acetonitrile-water.

Science.gov (United States)

Nakatani, Kiyoharu; Kakizaki, Hiroshi

2003-08-01

Intraparticle mass transfer processes of Phenol Blue (PB) in single octadecylsilyl (ODS)-silica gel microparticles in acetonitrile-water were analyzed by microcapillary manipulation and microabsorption methods. An absorption maximum of PB, the sorption isotherm parameters, and the sorption rate in the microparticle system were highly dependent on the percentage of acetonitrile in solution. The results are discussed in terms of the microscopic polarity surrounding PB in the ODS phase and the relationship between the isotherm parameters and the sorption rate.

Examination of the concrete from an old Portuguese dam: Texture and composition of alkali-silica gel

International Nuclear Information System (INIS)

Fernandes, Isabel; Noronha, Fernando; Teles, Madalena

2007-01-01

Exudations and pop-outs were identified in the interior galleries of a large dam built in the 1960s. The samples collected were examined by a Scanning Electron Microscope. A dense material with a smooth surface and drying shrinkage cracks or a spongy texture were observed in the samples. The semi-quantitative composition was obtained by energy dispersive spectrometry (EDS) and it was concluded that this material corresponds to alkali-silica gel, composed of SiO 2 -Na 2 O-K 2 O-CaO. A viscous white product in contact with an aggregate particle in a cone sampled from a pop-out was observed through use of the scanning electron microscope and it has characteristics similar to the gel present in the exudations and cavities. Reference is made to the potential alkali reactivity of the aggregate present in the concrete. The texture and composition of the products probably resulting from an alkali-silica reaction are presented, set out in ternary diagrams, and discussed

Catalytic oxidation of dichloromethane over sol-gel oxides supported Pd or Ni

International Nuclear Information System (INIS)

Martinez; Leidy Marcela; Montes, Consuelo

2004-01-01

Several supported Pd or Ni catalysts were synthesized by the sol-gel method using y-alumina, silica, sulfated zirconium and sulfated titanium as carriers. The resulting catalysts were characterized by XRD and nitrogen adsorption, and evaluated in the catalytic oxidation of dichloromethane. The effect of different parameters were determined, i.e. method of synthesis, temperature and the type of support. The durability of the best catalyst (0,5% Pd impregnated over sulfated titanium) was tested between 300 degrades Celsius and 350 degrades Celsius during 48 h. Under the conditions of this study, impregnated catalysts exhibited higher activity than those prepared by cogelation. Pd loaded catalysts showed higher conversion into CO 2 and HCl. Catalyst activity also increased with increasing temperature. Y-Alumina and sulfated titanium showed good activity but the formation of CO is favored instead of CO 2 . Therefore, bifunctional catalysts, i.e. containing metallic and acid sites appear to be required for the decomposition of methylene chloride into CO 2 and HCI

Synthesis of Fluorite (CaF2 Crystal from Gypsum Waste of Phosphoric Acid Factory in Silica Gel

Directory of Open Access Journals (Sweden)

Mohammad Misbah Khunur

2012-06-01

Full Text Available This paper report the synthesis and characterization of fluorite single crystal prepared from gypsum waste of phosphoric acid production in silica gel. Instead of its high calcium, gypsum was used to recycle the waste which was massively produces in the phosphoric acid production. The gypsum waste, the raw material of CaCl2 supernatant, was dissolved in concentrated HCl and then precipitated as calcium oxalate (CaC2O4 by addition of ammonium oxalate. The CaCl2 was obtained by dissolving the CaC2O4 with HCl 3M. The crystals were grown at room temperature in silica gel and characterized by AAS, FTIR and powder XRD. The optimum crystal growth condition, which is pH of gel, CaCl2 concentration and growth time, were investigated. The result shows that at optimum condition of pH 5.80, CaCl2 concentrations of 1.2 M, and growth time of 144 hours, colorless crystals with the longest size of 3 mm, were obtained (72.57%. Characterization of the synthesized crystal by AAS indicates that the obtained crystal has high purity. Meanwhile, analysis by FTIR spectra shows a Ca–F peak at 775 cm-1, and powder-XRD analysis confirms that the obtained crystal was fluorite (CaF2. © 2012 BCREC UNDIP. All rights reservedReceived: 11st April 2012; Revised: 4th June 2012; Accepted: 13rd June 2012[How to Cite: M.M. Khunur, A. Risdianto, S. Mutrofin, Y.P. Prananto. (2012. Synthesis of Fluorite (CaF2 Crystal from Gypsum Waste of Phosphoric Acid Factory in Silica Gel. Bulletin of Chemical Reaction Engineering & Catalysis, 7 (1: 71-77.  doi:10.9767/bcrec.7.1.3171.71-77 ][How to Link / DOI: http://dx.doi.org/10.9767/bcrec.7.1.3171.71-77 ] | View in 

K3[Fe(CN)6].3H2O supported on silica gel: An efficient and selective ...

Indian Academy of Sciences (India)

Department of Chemistry, Payame Noor University, 19395-4697 Tehran, I. R. of IRAN e-mail: ... K3[Fe(CN)6].3H2O, Silica gel; oxime; aldehyde; ketone. 1. Introduction .... ysis, hydrogenation, etc., using organic and inorganic reagents. Besides ...

Diffusion and aggregation of implanted Ag and Au in a lithia--alumina--silica glass

International Nuclear Information System (INIS)

Arnold, G.W.; Borders, J.A.

1975-01-01

Optical extinction and Rutherford backscattering (RBS) techniques were employed to obtain information on the size and spatial distribution of Au- and Ag-colloids in implanted (Au + , Ag + ) lithia-alumina-silica glass. The formation of metallic aggregates (colloids), necessary for preparation of a glass-ceramic surface layer, proceeds readily with annealing temperature for Au-implanted samples but not for Ag-implanted material. The optical and RBS spectra show that the particle size and spatial distribution in as-implanted samples are sensitive to sample temperature and ion-beam heating effects, while these parameters for Au-implanted samples are relatively insensitive to temperature and beam current. It is suggested that this behavior is related to differences in the dissolution energies of Ag and Au aggregates. A two-peaked spatial distribution for Ag implanted at room temperature at a dose rate of approximately 1 μA/cm 2 is observed which may result from the trapping of Ag in the compacted damage region of the glass during implantation. (auth)

Diffusion and aggrigation of implanted Ag and Au in a lithia-alumina-silica glass

International Nuclear Information System (INIS)

Arnold, G.W.; Borders, J.A.

1976-01-01

Optical extinction and Rutherford backscattering (RBS) techniques have been employed to obtain information on the size and spatial distribution of Au and Ag colloids in implanted (Au + ,Ag + )lithia-alumina-silica glass. The formation of metallic aggregates (colloids), necessary for preparation of a glass-ceramic surface layer, proceeds readily with annealing temperature for Au-implanted samples but not for Ag-implanted material. The optical and RBS spectra show that the particle size and spatial distribution in Ag-implanted samples are sensitive to sample temperature and ion-beam heating effects, while these parameters for Au-implanted samples are relatively insensitive to temperature and beam current. It is suggested that this behaviour is related to differences in the dissolution energies of Ag and Au aggregates. A two-peaked spatial distribution for Ag implanted at room temperature at a dose rate of approximately 1 μA cm -2 is observed which may result from the trappings of Ag in the ion displacement damage region of the glass during implantation. (author)

Submicrometric gratings fabrication from photosensitive organo-silica-hafnia thin films elaborated by sol-gel processing

Energy Technology Data Exchange (ETDEWEB)

Franc, Janyce [Universite de Lyon, F-42023 Saint-Etienne (France); CNRS, UMR 5516, Laboratoire Hubert Curien, 42023 Saint-Etienne (France); Universite de Saint-Etienne, Jean-Monnet, F-42023 Saint-Etienne (France); Barnier, Vincent, E-mail: barnier@emse.fr [Ecole Nationale Superieure des Mines, SMS-EMSE, CNRS:UMR 5146, LCG, F-42023 Saint-Etienne (France); Vocanson, Francis, E-mail: francis.vocanson@univ-st-etienne.fr [Universite de Lyon, F-42023 Saint-Etienne (France); CNRS, UMR 5516, Laboratoire Hubert Curien, 42023 Saint-Etienne (France); Universite de Saint-Etienne, Jean-Monnet, F-42023 Saint-Etienne (France); Gamet, Emilie; Lesage, Maryline [Universite de Lyon, F-42023 Saint-Etienne (France); CNRS, UMR 5516, Laboratoire Hubert Curien, 42023 Saint-Etienne (France); Universite de Saint-Etienne, Jean-Monnet, F-42023 Saint-Etienne (France); Jamon, Damien [Universite de Lyon, F-42023 Saint-Etienne (France); Laboratoire Claude Chappe, Telecom Saint-Etienne, 42000 Saint-Etienne Cedex 2 (France); Universite de Saint-Etienne, Jean-Monnet, F-42023 Saint-Etienne (France); Jourlin, Yves [Universite de Lyon, F-42023 Saint-Etienne (France); CNRS, UMR 5516, Laboratoire Hubert Curien, 42023 Saint-Etienne (France); Universite de Saint-Etienne, Jean-Monnet, F-42023 Saint-Etienne (France)

2012-07-31

The aim of this study is the elaboration of a high index sol-gel material in order to prepare submicrometric grating. The gratings were obtained after few seconds of UV exposure in one step using an organically modified silica-hafnia matrix. The chemical composition of thin films after UV and annealing treatments were studied using Fourier Transform Infrared Spectroscopy and X-Ray Photoelectron Spectroscopy. The study of optical properties revealed that the annealed films are transparent from 200 to 1000 nm and have a refractive index from 1.550 to 1.701 depending on the hafnium concentration. - Highlights: Black-Right-Pointing-Pointer Silica-hafnia matrix with high refractive index was prepared using sol-gel process. Black-Right-Pointing-Pointer Organic and inorganic networks formation of thin films was investigated. Black-Right-Pointing-Pointer Optical properties are influenced by annealing treatment and initial hafnium amount. Black-Right-Pointing-Pointer The use of high Si:Hf molar ratio can lead to a loss transmittance below 300 nm. Black-Right-Pointing-Pointer Submicrometric grating period can be prepared using a holographic method.

Study of shear thickening behavior in colloidal suspensions

Directory of Open Access Journals (Sweden)

N Maleki Jirsaraee

2015-01-01

Full Text Available We studied the shear thickening behavior of the nano silica suspension (silica nanoparticles 12 nm in size suspended in ethylene glycol under steady shear. The critical shear rate for transition into shear thickening phase was determined at different concentrations and temperatures. The effect of temperature and concentration was studied on the shear thickening behavior. In silica suspension, it was observed that all the samples had a transition into shear thickening phase and also by increasing the temperature, critical shear rate increased and viscosity decreased. Our observations showed that movement in silica suspension was Brownian and temperature could cause a delay in transition into shear thickening phase. Yet, we observed that increasing the concentration would decrease critical shear rate and increase viscosity. Increasing temperature increased Brownian forces and increasing concentration increased hydrodynamic forces, confirming the contrast between these two forces for transition into shear thickening phase for the suspensions containing nano particles

Pore radius fine tuning of a silica matrix (MCM-41) based on the synthesis of alumina nanolayers with different thicknesses by atomic layer deposition

International Nuclear Information System (INIS)

Zemtsova, Elena G.; Arbenin, Andrei Yu.; Plotnikov, Alexander F.; Smirnov, Vladimir M.

2015-01-01

The authors investigated a new approach to modify the surface of the mesoporous silica matrix MCM-41. This approach is based on manipulating the chemical composition of the porous surface layer and also on fine tuning the pore radius by applying the atomic layer deposition (ALD) technique. The synthesis of alumina nanolayers was performed on the planar and the porous matrix (MCM-41) by the ALD technique using aluminum tri-sec-butoxide and water as precursors. The authors show that one cycle on silicon, using aluminum tri-sec-butoxide and water as precursors, results in a 1–1.2 Å increase in alumina nanolayer thickness. This is comparable to the increase in thickness per cycle for other precursors such as trimethylaluminum and aluminum chloride. The authors show that the synthesis of an Al 2 O 3 nanolayer on the pore surface of the mesoporous silica matrix MCM-41 by the ALD technique results in a regular change in the porous structure of the samples. The specific porosity (ml/g) of the MCM-41 was 0.95 and that of MCM-41 after 5 ALD cycles was 0.39. The pore diameter (nm) of MCM-41 was 3.3 and that of MCM-41 after 5 ALD cycles was 2.3

Influence of p H on optical properties of nano structure sol-gel-derived silica films

International Nuclear Information System (INIS)

Heshmatpuor, F.; Adelkhani, H.; Nahavandi, M.; Noorbakhsh Shourabadi, M.

2006-01-01

Sol-gel derived silica films were fabricated by dip-coating onto glass microscope substrates. Film properties such as transmission and surface morphology were monitored as function of dip speed and sol p H. Film transmission was increased with increasing of p H in visible range. The surface morphology of films were investigated with scanning electron microscopy.

Preparation and characterization of rice hull silica products

International Nuclear Information System (INIS)

Quirit, Leni L.; Llaguno, Elma C.; Pagdanganan, Fernando C.; Hernandez, Karen N.

2008-01-01

Rice hull is an abundant agricultural waste material which could be a renewable energy source when combusted. The combustion residue (called rice hull ash or RHA) contains a significant amount (20% of the hull) of potentially high grade silica. Silica gels prepared from rice hull were found to have properties comparable to two commercial desiccant silica gels (Blue Merck and FNG-A) in terms of chemical and amorphous structure, surface area, desiccant characteristics, microstructure and heats of adsorption. These properties were determined from water vapor adsorption measurements, electron microscopy, and from infrared and x-ray diffraction spectra. The acid treated rice hull gels were found to have fewer elemental impurities detected by qualitative x-ray fluorescence, compared to the commercial gels. Thermogravimetric analysis (TGA) data showed that this technique can also be used to indirectly compare impurity levels in the samples, in terms of the amorphous to crystalline phase transition. Using an improved acid treatment method, a silica gel sample was prepared from rice hull and compared to three commercial chromatographic silica gels using quantitative elemental x-ray fluorescence analysis. Elemental levels in the rice hull gel were within the range of levels or close to the detection limits of corresponding elements in the chromatographic gels. Water vapor adsorption, x-ray diffraction, infrared spectroscopy and scanning electron microscopy showed that the rice hull gel was similar to the commercial chromatographic silica gel Davison 12. Zeolites are crystalline aluminosilicates used as molecular sieves for purification and catalytic purposes. Zeolites X and Y were synthesized from rice hull silica gel and aluminum hydroxide. For comparison, controls were synthesized from commercial silica gel. The samples and controls exhibited characteristics infrared peaks corresponding to the vibrations of the TO 4 (T=Si, Al) of the zeolite framework. The x

Effect of silver ions on the energy transfer from host defects to Tb ions in sol–gel silica glass

Energy Technology Data Exchange (ETDEWEB)

Abbass, Abd Ellateef [Department of Physics, University of the Free State, Bloemfontein (South Africa); Department of Physics, Sudan University of Science and Technology (Sudan); Swart, H.C. [Department of Physics, University of the Free State, Bloemfontein (South Africa); Kroon, R.E., E-mail: KroonRE@ufs.ac.za [Department of Physics, University of the Free State, Bloemfontein (South Africa)

2015-04-15

Plasmonic metal structures have been suggested to enhance the luminescence from rare-earth (RE) ions, but this enhancement is not yet well understood or applied to phosphor materials. Although some reports using Ag nanoparticles (NPs) in glass have attributed enhancement of RE emission to the strong electric fields associated with Ag NPs, it has also been proposed that the enhancement is instead due to energy transfer from Ag ions to RE ions. Our work using sol–gel silica shows a third possibility, namely that enhancement of the RE (e.g. Tb) emission is due to energy transfer from defects of the host material to the Tb ions, where the addition of Ag influences the silica host defects. The oxidation state of Ag as a function of annealing temperature was investigated by x-ray diffraction, transmission electron microscopy, UV–vis measurements and x-ray photoelectron spectroscopy, while optical properties were investigated using a Cary Eclipse fluorescence spectrophotometer or by exciting samples with a 325 nm He–Cd laser. The results showed that Ag ions have a significant effect on the silica host defects, which resulted in enhancement of the green Tb emission at 544 nm for non-resonant excitation using a wavelength of 325 nm. - Highlights: • Conversion of Ag ions to metallic nanoparticles after annealing of sol–gel silica. • Addition of Ag resulted in enhanced green luminescence from Tb ions in silica. • Enhancement is attributed to the effect of added Ag on the host defects of silica.

Method of producing zeolite encapsulated nanoparticles

DEFF Research Database (Denmark)

2015-01-01

The invention therefore relates to a method for producing zeolite, zeolite-like or zeotype encapsulated metal nanoparticles, the method comprises the steps of: 1) Adding one or more metal precursors to a silica or alumina source; 2) Reducing the one or more metal precursors to form metal...... nanoparticles on the surface of the silica or alumina source; 3) Passing a gaseous hydrocarbon, alkyl alcohol or alkyl ether over the silica or alumina supported metal nanoparticles to form a carbon template coated zeolite, zeolite-like or zeotype precursor composition; 4a) Adding a structure directing agent...... to the carbon template coated zeolite, zeolite-like or zeotype precursor composition thereby creating a zeolite, zeolite-like or zeotype gel composition; 4b) Crystallising the zeolite, zeolite-like or zeotype gel composition by subjecting said composition to a hydrothermal treatment; 5) Removing the carbon...

Method for producing zeolites and zeotypes

DEFF Research Database (Denmark)

2015-01-01

The invention relates to a method for producing zeolite, zeolite-like or zeotype particles comprising the steps of: 1 ) Adding one or more metal precursors to a silica or alumina source; 2) Reducing the one or more metal precursors to form metal nanoparticles on the surface of the silica or alumina...... source; 3) Passing a gaseous hydrocarbon, alkyl alcohol or alkyl ether over the silica or alumina supported metal nanoparticle to form a carbon template coated zeolite, zeolite-like or zeotype precursor composition; 4a) Adding a structure directing agent to the carbon template coated zeolite, zeolite......-like or zeotype precursor composition thereby creating a zeolite, zeolite-like or zeotype gel composition; 4b) Crystallising the zeolite, zeolite-like or zeotype gel composition by subjecting said composition to a hydrothermal treatment; 5) Removing the carbon template and structure directing agent and isolating...

Integrating nanohybrid membranes of reduced graphene oxide: chitosan: silica sol gel with fiber optic SPR for caffeine detection

Science.gov (United States)

Kant, Ravi; Tabassum, Rana; Gupta, Banshi D.

2017-05-01

Caffeine is the most popular psychoactive drug consumed in the world for improving alertness and enhancing wakefulness. However, caffeine consumption beyond limits can result in lot of physiological complications in human beings. In this work, we report a novel detection scheme for caffeine integrating nanohybrid membranes of reduced graphene oxide (rGO) in chitosan modified silica sol gel (rGO: chitosan: silica sol gel) with fiber optic surface plasmon resonance. The chemically synthesized nanohybrid membrane forming the sensing route has been dip coated over silver coated unclad central portion of an optical fiber. The sensor works on the mechanism of modification of dielectric function of sensing layer on exposure to analyte solution which is manifested in terms of red shift in resonance wavelength. The concentration of rGO in polymer network of chitosan and silica sol gel and dipping time of the silver coated probe in the solution of nanohybrid membrane have been optimized to extricate the supreme performance of the sensor. The optimized sensing probe possesses a reasonably good sensitivity and follows an exponentially declining trend within the entire investigating range of caffeine concentration. The sensor boasts of an unparalleled limit of detection value of 1.994 nM and works well in concentration range of 0-500 nM with a response time of 16 s. The impeccable sensor methodology adopted in this work combining fiber optic SPR with nanotechnology furnishes a novel perspective for caffeine determination in commercial foodstuffs and biological fluids.

Immobilization of Aspergillus niger. beta. -D-glucosidase on aminated chitin and alumina/alginate

Energy Technology Data Exchange (ETDEWEB)

Bon, E.; Freire, D.; Mendes, M.F.; Soares. V.F.

1986-01-01

The immobilization of ..beta..-glucosidase was studied by (a) covalent coupling to aminated chitin (IME-C) and (b) adsorption onto alumina followed by gel entrapment of the suspension with calcium alginate (IME-A). The levels of catalytic activity determined against salicin at 50 C were 23.0 U/g and 0.2 U/g for the IME-C and IMA-A respectively. The first system was shown to be quite stable with a loss of only 2% of the initial activity over 14 days. The IME-A system had a half life of 14 days. The activity of IME-C was studied using cellobiose and enzymatic hydrolysates of sugar cane bagasse at several cellobiose concentrations. The activities obtained with cellobiose were 104.0 U/g and 72.0 U/g respectively. 13 references.

Silica particles and method of preparation thereof

NARCIS (Netherlands)

2015-01-01

The invention is in the field of silica products. More in particular, the invention is in the field of amorphous silica particles. The invention is directed to amorphous silica particles and related products including clusters of said silica particles, a suspension of said silica particles, and an

Preparation and Characterization of Activated Alumina

Science.gov (United States)

Rabia, A. R.; Ibrahim, A. H.; Zulkepli, N. N.

2018-03-01

Activated alumina is a high surface area and highly porous form of aluminum oxide that can be employed for contaminant species adsorb from ether gases or liquids without changing its form. The research in getting this material has generated huge interested. Thus, this paper presented preparation of activated alumina from chemical process. Pure aluminum (99.9% pure) reacted at room temperature with an aqueous NaOH in a reactor to produce a solution of sodium aluminate (NaAlO2). This solution was passed through filter paper and the clear filtrate was neutralized with H2SO4, to pH 6, 7 or 8, resulting in the precipitation of a white gel, Al(OH)3·XH2O. The washed gel for sulfate ions were dried at 80 °C for 6 h, a 60 mesh sieve was to separate and sort them into different sizes. The samples were then calcined (burn) for 3h in a muffle furnace, in air, at a heating rate of 2 °C min-1. The prepared activated alumina was further characterized for better understanding of its physical properties in order to predict its chemical mechanism.

Thin layer chromatography of glucose and sorbitol on Cu(II)-impregnated silica gel plates

Energy Technology Data Exchange (ETDEWEB)

Hadzija, O. (Ruder Boskovic Inst., Zagreb (Croatia)); Spoljar, B. (Ruder Boskovic Inst., Zagreb (Croatia)); Sesartic, L. (Inst. of Immunology, Zagreb (Croatia))

1994-04-01

A thin-layer chromatographic (TLC) separation of glucose and sorbitol on CU(II)-impregnated silica gel plates with n-propanol: Water (4:1) v/v as developer and potassium permanganate as detecting reagent has been worked out. The new impregnant is completely insoluble in water and thus enables the use of an aqueous developer. The R[sub f]-values are 55 and 10 for glucose and sorbitol, respectively. (orig.)

Thermodynamics of the Sorption of Benzimidazoles on Octadecyl Silica Gel from Water-Methanol Eluents

Science.gov (United States)

Shafigulin, R. V.; Bulanova, A. V.

2018-02-01

The standard enthalpy and entropy component of transferring benzimidazoles from water-methanol solutions to surfaces of octadecyl silica gel are determined using reversed-phase high-performance liquid chromatography (RP HPLC). The dependences between the enthalpy and polarizability of the molecules of the studied benzimidazoles, the enthalpy and the entropy factor are studied, and the influence of the quantitative composition of the water-methanol solution on the enthalpy are studied.

Germania and Alumina Dopant Diffusion and Viscous Flow Effects at Preparation of Doped Optical Fibers

Directory of Open Access Journals (Sweden)

Jens Kobelke

2017-01-01

Full Text Available We report on germania and alumina dopant profile shift effects at preparation of compact optical fibers using packaging methods (Stack-and-Draw method, Rod-in-Tube (RiT technique. The sintering of package hollow volume by viscous flow results in a shift of the core-pitch ratio in all-solid microstructured fibers. The ratio is increased by about 5% in the case of a hexagonal package. The shift by diffusion effects of both dopants is simulated for typical slow speed drawing parameters. Thermodynamic approximations of surface dissociation of germania doped silica suggest the need of an adequate undoped silica barrier layer to prevent an undesired bubble formation at fiber drawing. In contrast, alumina doping does not estimate critical dissociation effects with vaporous aluminium oxide components. We report guide values of diffusion length of germania and alumina for the drawing process by kinetic approximation. The germania diffusion involves a small core enlargement, typically in the sub-micrometer scale. Though, the alumina diffusion enlarges it by a few micrometers. A drawn pure alumina preform core rod transforms to an amorphous aluminosilicate core with a molar alumina concentration of only about 50% and a non-gaussian concentration profile.

Sol-gel transitions and liquid crystal phase transitions in concentrated aqueous suspensions of colloidal gibbsite platelets

NARCIS (Netherlands)

Mourad, M.C.D.; Byelov, D.V.; Petukhov, A.V.; de Winter, D.A.M.; Verkleij, A.J.; Lekkerkerker, H.N.W.

2009-01-01

In this paper, we present a comprehensive study of the sol-gel transitions and liquid crystal phase transitions in aqueous suspensions of positively charged colloidal gibbsite platelets at pH 4-5 over a wide range of particle concentrations (50-600 g/L) and salt concentrations (10-4-10-1 M NaCl). A

Determination of palladium content in palladium-alumina/palladium-silica/palladium-tin oxide catalyst for nuclear reactor applications

International Nuclear Information System (INIS)

Sharma, P.K.; Bassan, M.K.T.; Avhad, D.K.; Singhal, R.K.

2012-01-01

Alumina and silica act as support for finely divided palladium metal powder in synthesis of catalyst. These catalyst (Pd-Al 2 O 3 , Pd-SiO 2 and Pd-SnO 2 ) used in nuclear power reactor (moderator cover gas system) for the conversion of hydrogen. In Indian nuclear power programme these catalyst are regularly used in Kaiga 1 and 2 and Rajasthan atomic power plant 3 and 4. The performance of the catalyst, solely depends on the concentration of palladium, which is the active component in this catalyst composition. Therefore it is highly desirable to have rouged analytical methodology for the accurate estimation of palladium. Leaching of Pd from the bulk matrix is tedious due to the less reactive nature of Pd therefore complete solubilization of the matrix is carried out by fusion method

Deposition of GdVO4:Eu3+ nanoparticles on silica nanospheres by a simple sol gel method

Science.gov (United States)

Liu, Guixia; Hong, Guangyan; Wang, Jinxian; Dong, Xiangting

2006-07-01

The deposition and coating of GdVO4:Eu3+ nanoparticles on spherical silica was carried out using a simple sol-gel method at low temperature. The GdVO4:Eu3+-coated silica composites obtained were characterized by differential thermal analysis (DTA), thermogravimetric (TG) analysis, x-ray diffraction (XRD), Fourier-transform IR spectroscopy (FT-IR), transmission electron microscopy (TEM), x-ray photoelectron spectroscopy (XPS), photoluminescence spectra, and kinetic decay. It is found that the ~5 nm GdVO4:Eu3+ nanoparticles coating the silica spheres are crystal in the as-prepared samples and the crystallinity increases with increasing annealing temperature. The composites obtained are spherical in shape with an average size of 100 nm. The GdVO4:Eu3+ nanoparticles are linked with silica cores by a chemical bond. The photoluminescence spectra of the obtained GdVO4:Eu3+-coated silica composites are similar to those of the bulk GdVO4:Eu3+ phosphors. The strongest peak is near 617 nm, which indicates that Eu3+ is located in the low symmetry site with non-inversion centre.

Sol–gel one-pot synthesis in soft conditions of mesoporous silica materials ready for drug delivery system

NARCIS (Netherlands)

Tourne-Peteilh, C.; Begu, S.; Lerner, D.A.; Galarneau, A.; Lafont, U.; Devoiselle, J.M.

2011-01-01

The present work reveals a new and simple strategy, a one-step sol–gel procedure, to encapsulate a low water-soluble drug in silica mesostructured microparticles and to improve its release in physiological media. The synthesis of these new materials is based on the efficient solubilisation of a

Direct Visualization of the Hydration Layer on Alumina Nanoparticles with the Fluid Cell STEM in situ.

Science.gov (United States)

Firlar, Emre; Çınar, Simge; Kashyap, Sanjay; Akinc, Mufit; Prozorov, Tanya

2015-05-21

Rheological behavior of aqueous suspensions containing nanometer-sized powders is of relevance to many branches of industry. Unusually high viscosities observed for suspensions of nanoparticles compared to those of micron size powders cannot be explained by current viscosity models. Formation of so-called hydration layer on alumina nanoparticles in water was hypothesized, but never observed experimentally. We report here on the direct visualization of aqueous suspensions of alumina with the fluid cell in situ. We observe the hydration layer formed over the particle aggregates and show that such hydrated aggregates constitute new particle assemblies and affect the flow behavior of the suspensions. We discuss how these hydrated nanoclusters alter the effective solid content and the viscosity of nanostructured suspensions. Our findings elucidate the source of high viscosity observed for nanoparticle suspensions and are of direct relevance to many industrial sectors including materials, food, cosmetics, pharmaceutical among others employing colloidal slurries with nanometer-scale particles.

KCl-induced high temperature corrosion of selected commercial alloys. Part II: alumina and silica-formers

DEFF Research Database (Denmark)

Kiamehr, Saeed; Dahl, Kristian Vinter; Montgomery, Melanie

2016-01-01

for 168 h in flowing N2(g)+5%O2(g)+15%H2O(g) (vol.%) with samples covered under KCl powder. A KCl-free exposure was also performed for comparison.Corrosion morphology and products were studied with scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and X-ray diffractometry (XRD......Laboratory testing on selected alumina and silica-forming alloys was performed to evaluate their performance against high temperature corrosion induced by potassium chloride (KCl). The alloys studied were FeCrAlY, Kanthal APM, Nimonic 80A, 214, 153MA and HR160. Exposure was conducted at 600 °C......-chromium-silicon-oxygen containing layer forms as the innermost corrosion product. The layer was uniformly distributed over the surface and appears to render some protection as this alloy exhibited the best performance among the investigated alloys. To reveal further aspects of the corrosion mechanism, Nimonic 80A was exposed...

A NOVEL GEL ELECTROLYTE FOR VALVE-REGULATED LEAD ACID BATTERY

Directory of Open Access Journals (Sweden)

Metin GENÇTEN

2017-03-01

Full Text Available A novel gel electrolyte system used in lead-acid batteries was investigated in this work. The gel systems were prepared by addition different amount of Al2O3, TiO2 and B2O3 into the gelled system consisting of 6 wt% fumed silica and 30 wt% sulfuric acid solution. The anodic peak currents and peak redox capacities of the gel electrolytes were characterized by cyclic voltammetric method. They decreased by the time B2O3 and Al2O3 were used as additives in fumed silica based gel electrolyte system. However, these values increased by the adding 3.0 wt% of TiO2. The solution and charge transfer resistances of the gel electrolytes were investigated by electrochemical impedance spectroscopy. While the solution resistances were lower in gel systems having different amount additives than pure fumed silica based gel, the charge transfer resistance was the lowest in gel electrolytes consisting fumed silica and fumed silica-TiO2. The battery performances were studied by obtaining discharge curves of prepared gel electrolytes. The performance of gelled systems were higher than that of non-gelled electrolyte at room temperature. The mixture of fumed silica-TiO2 was suggested an alternative gel formulation for gel VRLA batteries.

Silica based gel as a potential waste form for high level waste from fuel reprocessing

International Nuclear Information System (INIS)

Ford, C.E.; Dempster, T.J.; Melling, P.J.

1983-10-01

To assess the feasibility of safe disposal of high-level radioactive waste as synthetic clay, or material that would react with ground water to form clay, experiments have been carried out to determine the hydrothermal crystallisation and leaching behaviour of silica based gels fired at 900 deg C. Crystallisation rates at a pressure of 500 bars and at temperatures below 400 deg C are negligible and this more or less precludes pre-disposal production of synthetic clay on the scale required. Leaching experiments suggest that the leach rates of Cs from gels by distilled water are higher than those of boro-silicate glasses and SYNROC at the lower temperatures that would be preferred for geological storage. However, amounts of bulk dissolution of gels may be lower than those of boro-silicate glasses. The initial leaching behaviour of gels might be considerably improved by hot compaction at 900 to 1000 deg C. Consideration of likely waste form dissolution behaviour in a repository environment suggests that gels of appropriate composition might perform as well as, or better than, boro-silicate glasses. A novel hypothetical plant is described that could produce the gel waste form on the scale required on a more or less continuous basis. (author)

Structure and dynamics of spin-labeled insulin entrapped in a silica matrix by the sol-gel method.

Science.gov (United States)

Vanea, E; Gruian, C; Rickert, C; Steinhoff, H-J; Simon, V

2013-08-12

The structure and conformational dynamics of insulin entrapped into a silica matrix was monitored during the sol to maturated-gel transition by electron paramagnetic resonance (EPR) spectroscopy. Insulin was successfully spin-labeled with iodoacetamide and the bifunctional nitroxide reagent HO-1944. Room temperature continuous wave (cw) EPR spectra of insulin were recorded to assess the mobility of the attached spin labels. Insulin conformation and its distribution within the silica matrix were studied using double electron-electron resonance (DEER) and low-temperature cw-EPR. A porous oxide matrix seems to form around insulin molecules with pore diameters in the order of a few nanometers. Secondary structure of the encapsulated insulin investigated by Fourier transform infrared spectroscopy proved a high structural integrity of insulin even in the dried silica matrix. The results show that silica encapsulation can be used as a powerful tool to effectively isolate and functionally preserve biomolecules during preparation, storage, and release.

Sugarcane bagasse lignin, and silica gel and magneto-silica as drug vehicles for development of innocuous methotrexate drug against rheumatoid arthritis disease in albino rats.

Science.gov (United States)

Wahba, Sanaa M R; Darwish, Atef S; Shehata, Iman H; Abd Elhalem, Sahar S

2015-03-01

The present study clarifies co-therapy action of deliveries from their textural changes point of view. Methotrexate (MTX) was immobilized onto biodegradable lignin, silica gel and iron/silica nanocomposite. Loaded-MTX was i.p. injected into albino rats at doses of 0.25 and 0.5mg/kg/week for 2.5months, after which spleen, liver, testes and knee joint tissues were collected for tests. IFN-γ and IL-17A mRNA gene expressions in spleen in all biological samples were determined by RT-PCR. Physicochemical features of drug carriers were monitored by XRD, BET-PSD, SEM and TEM. Drug inflammatory-site targeting was found to be closely related to the physico-features of deliverers. The interlayered lignin of micro- and meso-pore channels directed MTX toward concealed infected cells in liver and testes tissues, while meso-structured silica flacks satisfied by gathering MTX around knee joints. The magneto-silica nanocomposite targeted MTX toward spleen tissue, which is considered as a lively factory for the production of electron rich compounds. Copyright © 2014 Elsevier B.V. All rights reserved.

Synthesis of all-silica zeolites from highly concentrated gels containing hexamethonium cations

KAUST Repository

Liu, Xiaolong

2012-07-01

A pure and highly crystalline all-silica EU-1 zeolite has been obtained from the crystallization of gels containing very low water contents in the presence of hexamethonium cations. Decreasing the water content in the gel down to H 2O/Si < 1 inhibited the formation of ZSM-48, which is usually observed under more diluted standard crystallization conditions. Moreover, addition of NH 4F to the synthesis led to the formation of "half-fluorinated" ITQ-13 in which fluoride anions occupied only the center of D4R cages. In larger cages, the charge of the template was compensated by framework connectivity defects, clearly demonstrating once more the essential role of F - in the formation of D4R units. The formation of such hybrid (F,OH) is particularly interesting from a synthesis point of view, particularly for understanding the respective roles of fluoride and hydroxide anions in the crystallization process. © 2012 Elsevier Inc. All rights reserved.

Preparation and characterization of ultrafine alumina via sol-gel polymeric route

Energy Technology Data Exchange (ETDEWEB)

Ibrahim, D.M. [Ceramic Department, National Research Centre, Dokki, Cairo (Egypt); Abu-Ayana, Y.M. [Polymers and Pigments Department, National Research Centre, Dokki, Cairo (Egypt)], E-mail: yosreya20@gmail.com

2008-10-15

Ultrafine alumina powder was prepared through resin formation between urea and formaldehyde. Aluminium stearate soap was introduced during resin preparation. Ethylene glycol was used to terminate the thermosetting reaction. Calcination of the product was carried out at 700, 1000, 1100, 1300 and 1400 deg. C to obtain aluminium oxide. IR and Raman spectroscopic analysis indicated the occupation of Al{sup 3+} at different sites in the polymer network (C=O, -NH{sub 2}, C-O, -NH, and -CH{sub 2}OH). X-ray diffraction of powder calcined at 1000 deg. C revealed the presence of a mixture of {alpha}- and {theta}-alumina together, while a mixture of {alpha}- and {beta}-alumina phases were obtained on calcination at 1400 deg. C. Transmission electron microscope (TEM) examination of the powder fired at 700 deg. C showed uniform grains in the form of clusters with average size between 22.02 and 30.5 nm. Clusters are multi-particles as evident from the electron diffraction pattern. Crystallite size of alumina powder calcined at 1000 deg. C was found to be {approx}25.67 nm, while that of powder calcined at1400 deg. C was {approx}30.52 nm. The calculated specific surface area of alumina powder calcined at 1000 deg. C was 59.17 m{sup 2} g{sup -1}, while that calcined at 1400 deg. C was 49.77 m{sup 2} g{sup -1}.

Ultra-small dye-doped silica nanoparticles via modified sol-gel technique

Science.gov (United States)

Riccò, R.; Nizzero, S.; Penna, E.; Meneghello, A.; Cretaio, E.; Enrichi, F.

2018-05-01

In modern biosensing and imaging, fluorescence-based methods constitute the most diffused approach to achieve optimal detection of analytes, both in solution and on the single-particle level. Despite the huge progresses made in recent decades in the development of plasmonic biosensors and label-free sensing techniques, fluorescent molecules remain the most commonly used contrast agents to date for commercial imaging and detection methods. However, they exhibit low stability, can be difficult to functionalise, and often result in a low signal-to-noise ratio. Thus, embedding fluorescent probes into robust and bio-compatible materials, such as silica nanoparticles, can substantially enhance the detection limit and dramatically increase the sensitivity. In this work, ultra-small fluorescent silica nanoparticles (NPs) for optical biosensing applications were doped with a fluorescent dye, using simple water-based sol-gel approaches based on the classical Stöber procedure. By systematically modulating reaction parameters, controllable size tuning of particle diameters as low as 10 nm was achieved. Particles morphology and optical response were evaluated showing a possible single-molecule behaviour, without employing microemulsion methods to achieve similar results. [Figure not available: see fulltext.

Surface modification on a glass surface with a combination technique of sol–gel and air brushing processes

KAUST Repository

Tsai, Meng-Yu; Hsu, Chin-Chi; Chen, Ping-Hei; Lin, Chao-Sung; Chen, Alexander

2011-01-01

This study fabricated the large area and optically transparent superhydrophobic silica based films on glass surface with optimized hardness. A silane coupling agent, tetraethoxysilane (TEOS), effectively bonds silica particles onto the glass substrate. Desired surface roughness was obtained by adjusting nano silica particles concentration of the precursors prepared by the sol-gel process. Silica suspension was coated onto the glass substrate by the air brushing methods. This method can deposit a uniform, transparent coating on the glass substrate efficiently. Diluting the precursor by adding ethanol or a mixture of D.I. water and ethanol further improved the transmittance and superhydrophobicity efficiency. The results showed that as the silica particle concentration and the thickness of the coating were increased, the surface roughness was enhanced. Rougher surface displayed a higher superhydrophobicity and lower transmittance. Therefore, the concentration of silica particle, volume of coatings, and the ratio of ethanol and D.I. water are of great importance to deposit a transparent, superhydrophobic coating on glass. © 2011 Elsevier B.V. All rights reserved.

Surface modification on a glass surface with a combination technique of sol–gel and air brushing processes

KAUST Repository

Tsai, Meng-Yu

2011-08-01

This study fabricated the large area and optically transparent superhydrophobic silica based films on glass surface with optimized hardness. A silane coupling agent, tetraethoxysilane (TEOS), effectively bonds silica particles onto the glass substrate. Desired surface roughness was obtained by adjusting nano silica particles concentration of the precursors prepared by the sol-gel process. Silica suspension was coated onto the glass substrate by the air brushing methods. This method can deposit a uniform, transparent coating on the glass substrate efficiently. Diluting the precursor by adding ethanol or a mixture of D.I. water and ethanol further improved the transmittance and superhydrophobicity efficiency. The results showed that as the silica particle concentration and the thickness of the coating were increased, the surface roughness was enhanced. Rougher surface displayed a higher superhydrophobicity and lower transmittance. Therefore, the concentration of silica particle, volume of coatings, and the ratio of ethanol and D.I. water are of great importance to deposit a transparent, superhydrophobic coating on glass. © 2011 Elsevier B.V. All rights reserved.

Fabrication of silica glass containing yellow oxynitride phosphor by the sol-gel process

Energy Technology Data Exchange (ETDEWEB)

Segawa, Hiroyo; Yoshimizu, Hisato; Hirosaki, Naoto; Inoue, Satoru, E-mail: SEGAWA.Hiroyo@nims.go.jp [National Institute for Materials Science, 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan)

2011-06-15

We have prepared silica glass by the sol-gel method and studied its ability to disperse the Ca-{alpha}-SiAlON:Eu{sup 2+} phosphor for application in white light emitting diodes (LEDs). The emission color generated by irradiating doped glass with a blue LED at 450 nm depended on the concentration of SiAlON and the glass thickness, resulting in nearly white light. The luminescence efficiency of 1-mm-thick glass depended on the SiAlON concentration, and was highest at 4 wt% SiAlON.

Determination of picomolar beryllium levels in seawater with inductively coupled plasma mass spectrometry following silica-gel preconcentration

Energy Technology Data Exchange (ETDEWEB)

Tazoe, Hirofumi, E-mail: tazoe@cc.hirosaki-u.ac.jp [Department of Radiation Chemistry, Institute of Radiation Emergency Mediation, Hirosaki University, 66-1 Hon-cho, Hirosaki, Aomori 036-8564 (Japan); College of Humanities and Sciences, Nihon University, 3-25-40, Sakurajosui, Setagaya-ku, Tokyo 156-8550 (Japan); Yamagata, Takeyasu [College of Humanities and Sciences, Nihon University, 3-25-40, Sakurajosui, Setagaya-ku, Tokyo 156-8550 (Japan); Obata, Hajime [Atmosphere and Ocean Research Institute, The Tokyo University, 5-1-5 Kashiwanoha, Kashiwa-shi, Chiba 277-8564 (Japan); Nagai, Hisao [College of Humanities and Sciences, Nihon University, 3-25-40, Sakurajosui, Setagaya-ku, Tokyo 156-8550 (Japan)

2014-12-10

Highlights: • We developesd the simplest and robust SPE method for ultra low picomolar level beryllium in seawater. • Just silica gel column can quantitatively adsorb beryllium in neutral pH condition containing natural seawater. • EDTA solution can eliminate seawater matrixes retaining Be in the column, which optimize to ICP-MS detemination. • Accurate and precise Be data have been obtained for natural seawater from North Pacific Ocean. - Abstract: A robust and rapid method for the determination of natural levels of beryllium (Be) in seawater was developed to facilitate mapping Be concentrations in the ocean. A solid-phase extraction method using a silica gel column was applied for preconcentration and purification of Be in seawater prior to determination of Be concentrations with inductively coupled plasma mass spectrometry (ICP-MS). Be was quantitatively adsorbed onto silica gel from solutions with pH values ranging from 6.3 to 9, including natural seawater. The chelating agent ethylenediamine tetraacetic acid was used to remove other ions in the seawater matrix (Na, Mg, and Ca) that interfere with the ICP-MS analysis. The reproducibility of the method was 3% based on triplicate analyses of natural seawater samples, and the detection limit was 0.4 pmol kg{sup −1} for 250 mL of seawater, which is sufficient for the analysis of seawater in the open ocean. The method was then used to determine the vertical profile of Be in the eastern North Pacific Ocean, which was found to be a recycled-type profile in which the Be concentration increased with depth from the surface (7.2 pmol kg{sup −1} at <200 m) to deep water (29.2 pmol kg{sup −1} from 3500 m to the bottom)

Determination of picomolar beryllium levels in seawater with inductively coupled plasma mass spectrometry following silica-gel preconcentration

International Nuclear Information System (INIS)

Tazoe, Hirofumi; Yamagata, Takeyasu; Obata, Hajime; Nagai, Hisao

2014-01-01

Highlights: • We developesd the simplest and robust SPE method for ultra low picomolar level beryllium in seawater. • Just silica gel column can quantitatively adsorb beryllium in neutral pH condition containing natural seawater. • EDTA solution can eliminate seawater matrixes retaining Be in the column, which optimize to ICP-MS detemination. • Accurate and precise Be data have been obtained for natural seawater from North Pacific Ocean. - Abstract: A robust and rapid method for the determination of natural levels of beryllium (Be) in seawater was developed to facilitate mapping Be concentrations in the ocean. A solid-phase extraction method using a silica gel column was applied for preconcentration and purification of Be in seawater prior to determination of Be concentrations with inductively coupled plasma mass spectrometry (ICP-MS). Be was quantitatively adsorbed onto silica gel from solutions with pH values ranging from 6.3 to 9, including natural seawater. The chelating agent ethylenediamine tetraacetic acid was used to remove other ions in the seawater matrix (Na, Mg, and Ca) that interfere with the ICP-MS analysis. The reproducibility of the method was 3% based on triplicate analyses of natural seawater samples, and the detection limit was 0.4 pmol kg −1 for 250 mL of seawater, which is sufficient for the analysis of seawater in the open ocean. The method was then used to determine the vertical profile of Be in the eastern North Pacific Ocean, which was found to be a recycled-type profile in which the Be concentration increased with depth from the surface (7.2 pmol kg −1 at <200 m) to deep water (29.2 pmol kg −1 from 3500 m to the bottom)

Update on quadruple suspension design for Advanced LIGO

International Nuclear Information System (INIS)

Aston, S M; Carbone, L; Cutler, R M; Hoyland, D; Barton, M A; Bland, B; Bell, A S; Beveridge, N; Cagnoli, G; Cantley, C A; Cumming, A V; Cunningham, L; Hammond, G D; Haughian, K; Hough, J; Brummitt, A J; Greenhalgh, R J S; Hayler, T M; Heptonstall, A; Heefner, J

2012-01-01

We describe the design of the suspension systems for the major optics for Advanced LIGO, the upgrade to LIGO—the Laser Interferometric Gravitational-Wave Observatory. The design is based on that used in GEO600—the German/UK interferometric gravitational wave detector, with further development to meet the more stringent noise requirements for Advanced LIGO. The test mass suspensions consist of a four-stage or quadruple pendulum for enhanced seismic isolation. To minimize suspension thermal noise, the final stage consists of a silica mirror, 40 kg in mass, suspended from another silica mass by four silica fibres welded to silica ears attached to the sides of the masses using hydroxide-catalysis bonding. The design is chosen to achieve a displacement noise level for each of the seismic and thermal noise contributions of 10 −19 m/√Hz at 10 Hz, for each test mass. We discuss features of the design which has been developed as a result of experience with prototypes and associated investigations. (paper)

SCC modification by use of amorphous nano-silica

NARCIS (Netherlands)

Quercia Bianchi, G.; Spiesz, P.R.; Hüsken, G.; Brouwers, H.J.H.

2014-01-01

In this study two different types of nano-silica (nS) were applied in self-compacting concrete (SCC), both having similar particle size distributions (PSD), but produced through two different processes: fumed powder silica and precipitated silica in colloidal suspension. The influence of nano-silica

Catechol functionalized aminopropyl silica gel: synthesis, characterization and preconcentrative separation of uranium(VI) from thorium(IV)

International Nuclear Information System (INIS)

Metilda, P.; Mary Gladis, J.; Prasada Rao, T.P.

2005-01-01

A novel solid phase extractant is prepared by chemically immobilizing catechol with diazotized aminopropyl silica gel. The resulting catechol functionalized silica gel (CASG) was characterized by FTIR, and microanalysis and was used for selective enrichment of uranium(VI) from other inorganic ions. The optimum pH range for maximum sorption of uranium(VI) and thorium(IV) was found to be in the range 3.5-6.0. The above actinides were eluted with 10 cm 3 of 1.0 mol dm -3 HCl and determined by using an Arsenazo III spectrophotometric procedure. The calibration graph was rectilinear over the uranium(VI) concentration in the range 2-100 μg dm -3 with a relative standard deviation of 2.15% (for 25 μg of uranium(VI) present in 1.0 dm 3 of sample). The validation of the developed preconcentration procedure was carried out by analyzing marine sediment (MESS-3, NRC, Canada) and soil (IAEA soil-7, Austria) reference materials. The developed preconcentration method enables a simple instruments like a spectrophotometer gave comparable values of uranium(VI) to that of standard inductively coupled plasma-mass spectrometric values during the analysis of real soil and sediment samples. (orig.)

Removal of lindane from an aqueous solution by using aminopropyl silica gel-immobilized calix[6]arene.

Science.gov (United States)

Tor, Ali; Aydin, Mehmet Emin; Aydin, Senar; Tabakci, Mustafa; Beduk, Fatma

2013-11-15

An aminopropyl silica gel-immobilized calix[6]arene (C[6]APS) has been used for the removal of lindane from an aqueous solution in batch sorption technique. The C[6]APS was synthesized with p-tert-butylcalix[6]arene hexacarboxylate derivative and aminopropyl silica gel in the presence of N,N'-diisopropyl carbodiimide coupling reagent. The sorption study was carried out as functions of solution pH, contact time, initial lindane concentration, C[6]APS dosage and ionic strength of solution. The matrix effect of natural water samples on the sorption efficiency of C[6]APS was also investigated. Maximum lindane removal was obtained at a wide pH range of 2-8 and sorption equilibrium was achieved in 2h. The isotherm analysis indicated that the sorption data can be represented by both Langmuir and Freundlich isotherm models. Increasing ionic strength of the solutions increased the sorption efficiency and matrix of natural water samples had no effect on the sorption of lindane. By using multilinear regression model, regression equation was also developed to explain the effects of the experimental variables. Copyright © 2013 Elsevier B.V. All rights reserved.

A novel sol–gel process to facilely synthesize Ni{sub 3}Fe nanoalloy nanoparticles supported with carbon and silica

Energy Technology Data Exchange (ETDEWEB)

Xu, L.Q. [Institute of Materials Engineering, Nanjing National Laboratory of Microstructures, Jiangsu Provincial Laboratory for Nanotechnology and School of Physics, Nanjing University, Nanjing 210093 (China); School of Physics and Information Technology, Ningxia Teachers University, Guyuan, Ningxia 756000 (China); Chen, L.Y.; Huang, H.F.; Xie, R.; Xia, W.B.; Wei, J.; Zhong, W. [Institute of Materials Engineering, Nanjing National Laboratory of Microstructures, Jiangsu Provincial Laboratory for Nanotechnology and School of Physics, Nanjing University, Nanjing 210093 (China); Tang, S.L., E-mail: tangsl@nju.edu.cn [Institute of Materials Engineering, Nanjing National Laboratory of Microstructures, Jiangsu Provincial Laboratory for Nanotechnology and School of Physics, Nanjing University, Nanjing 210093 (China); Du, Y.W. [Institute of Materials Engineering, Nanjing National Laboratory of Microstructures, Jiangsu Provincial Laboratory for Nanotechnology and School of Physics, Nanjing University, Nanjing 210093 (China)

2014-04-01

Graphical abstract: The TEM and HRTEM images and the magnetization curves taken in both zero-field-cooled (ZFC) and field-cooled (FC) modes of Ni{sub 3}Fe nanoparticles calcined at 300 °C for 2 h under Ar flowing. Display Omitted - Highlights: • Ultrafine Ni{sub 3}Fe nanoalloy nanoparticles were synthesized via a modified novel sol–gel process. • The prepared Ni{sub 3}Fe nanoalloy nanoparticles have a narrow size distribution. • The Ni{sub 3}Fe nanoparticles exhibit superparamagnetic behaviors at room temperature. - Abstract: In this paper, we present a modified novel silica sol–gel process and explored the possibility, for the first time, to synthesize binary nanoalloy nanoparticles. We successfully prepared ultrafine Ni{sub 3}Fe nanoparticles supported with carbon and silica via this simple one-pot reaction without H{sub 2} reduction. X-ray diffraction (XRD) and selected area electron diffraction (SAED) investigations of the Ni{sub 3}Fe nanoparticles show that the nanoparticles have a face-centered-cubic (fcc) crystal structure. The TEM images show that grain sizes of Ni{sub 3}Fe nanoparticles have a narrow size distribution. Moreover, the grain size of the nanoparticles is not very sensitive to the elevated annealing temperature. The Ni{sub 3}Fe nanoparticles exhibit typical superparamagnetic behavior at room temperature, and the blocking temperatures (T{sub B}) are determined by the temperature-dependent magnetization (M–T curves) measurements. This novel silica sol–gel method is expected to have broad applications in synthesizing nanoalloy nanoparticles.

Preparasi Katalis Cu/Silika Gel dari Kristobalit Alam Sabang serta Uji Aktivitasnya pada Reaksi Dehidrogenasi Etanol

Directory of Open Access Journals (Sweden)

Surya Lubis

2009-06-01

Full Text Available Cu/Silica gel catalyst preparation by using silica content which is obtained from Sabang natural crystobalit has been done. Isolated silica from crystobalit is reacted with natrium hidroxide to produce silicate natrium that reacted further with sulphate acid to produce silica gel. Silica gel is characterized by infra red spektroscopy dan BET test. BET test result showed that silica gel obtained has specific surface area 260,04 m2/gram and ion Cu  impregnation into silica gel pores produce Cu/silica gel catalyst with spesific surace area 158,53 m/gram ith Cu2+ metal content = 193 ppm. Catalyst activation test Cu/silica gel at dehidrogenation reaction of etanol to produce asetaldehide was done at temperature 100oC – 300oC. Reseach showed that the highest asetaldehide consentration (20,24% is obtained at temperature 300oC.   Keywords: asetaldehide, crystobalit, Cu/silica gel, dehidrogenation, ethanol

Gel electrophoresis of inorganic cations

International Nuclear Information System (INIS)

Schoenhofer, F.; Grass, F.

1978-01-01

In order to be able to separate the largest possible amounts of substance, polyacryl amide gel (PAA) and silica gel are used as carrier for the electrophoresis. Milligramme quantities can easily be separated on PAA gel plates. Electrophoretic ion focussing considerably improves it. Separations of Sr/Y and lanthanoids were carried out. The behaviour of the readily soluble complexing agent acids on silica gel thin layers was minutely investigated and an interpretation of the focussing effect was derived. The conditions for separating radionuclides were optimized. A further improved separation can be achieved by a time sequence combination of normal electrophoresis and ion focussing. Selective isolation methods are advantageous to determine radionuclide traces in environmental samples. The selective adsorption on preformed deposits was transferred to electrophoresis. After pre-investigations on silica gel layers, strontium and barium could also be retained on PAA gel and radium on strontium sulphate in PAA, whereas the disturbing calcium can easily pass through. Cesium can also be retained by prussian blue in the electrophoresis. (orig.) [de

Selective solid phase extraction and pre-concentration of heavy metals from seawater by physically and chemically immobilized 4-amino-3-hydroxy-2-(2-chlorobenzene)-azo-1-naphtalene sulfonic acid silica gel

International Nuclear Information System (INIS)

Mahmoud, M.E.; Soayed, A.A.; Hafez, O.F.

2003-01-01

4-Amino-3-hydroxy-2 - (2-chlorobenzene)-azo-l-naphthalene sulfonic acid (AHCANSA) was used as a chelating modifier to improve the reactivity of the silica gel surface in terms of selective binding and extraction of heavy metal ions. The surface cover-age values were found to be 0.488 and 0.473 mmol g -1 for the newly modified physically adsorbed silica gel phase (I) and chemically immobilized-AHCANSA phase (II), respectively. The modified silica gel phases (I, II) were tested for stability in different acidic buffer solutions (pH 1-6) and found to be highly resistant to hydrolysis and leaching by buffer solutions above pH 2. The application of these two phases as solid extractors for a series of mono-, di-, and tri-valent metal ions from aqueous solutions was also performed with different controlling factors such as the pH value of metal ion solutions and equilibrium shaking time. The mmol g -1 metal capacity values determined by silica gel phases (I, II) were found to confirm high affinity and selectivity characters for binding with heavy metal ions such as Cr 3+ , Ni 2+ , Cu 2+ , Zn 2+ , Cd 2+ and Pb 2+ in a range of 0.250-0.483. The tested alkali and alkaline earth metals, Na + , K + , Mg 2+ and Ca 2+ , were found to exhibit little interaction and binding ability with the modified silica gel phases. The selectivity characters incorporated into the modified silica gel phases were further utilized and applied in solid phase extraction and pre-concentration of trace concentration levels (∼1.0 μg mL -1 and 2.00-2.50 ng mL -1 ) from real seawater samples. The percentage recovery values determined for Cr 3+ , Cu 2+ , Zn 2+ , Cd 2+ and Pb 2+ were found to be in the range of 95.2-98.1 ± 2.0-5.0 %, and the pre-concentration recovery values for the same tested heavy metal ions were found to be in the range of 92.5-97.1 ± 3.0-6.0 % for the two newly modified silica gel phases with a pre-concentration factor of 500. Refs. 25 (author)

Microstructure investigation on micropore formation in microporous silica materials prepared via a catalytic sol-gel process by small angle X-ray scattering.

Science.gov (United States)

Shimizu, Wataru; Hokka, Junsuke; Sato, Takaaki; Usami, Hisanao; Murakami, Yasushi

2011-08-04

The so-called sol-gel technique has been shown to be a template-free, efficient way to create functional porous silica materials having uniform micropores. This appears to be closely linked with a postulation that the formation of weakly branched polymer-like aggregates in a precursor solution is a key to the uniform micropore generation. However, how such a polymer-like structure can precisely be controlled, and further, how the generated low-fractal dimension solution structure is imprinted on the solid silica materials still remain elusive. Here we present fabrication of microporous silica from tetramethyl orthosilicate (TMOS) using a recently developed catalytic sol-gel process based on a nonionic hydroxyacetone (HA) catalyst. Small angle X-ray scattering (SAXS), nitrogen adsorption porosimetry, and transmission electron microscope (TEM) allowed us to observe the whole structural evolution, ranging from polymer-like aggregates in the precursor solution to agglomeration with heat treatment and microporous morphology of silica powders after drying and hydrolysis. Using the HA catalyst with short chain monohydric alcohols (methanol or ethanol) in the precursor solution, polymer-like aggregates having microscopic correlation length (or mesh-size) micropores with diameters 2 nm) in the solid product due to apertures between the particle-like aggregates. The data demonstrate that the extremely fine porous silica architecture comes essentially from a gaussian polymer-like nature of the silica aggregates in the precursor having the microscopic mesh-size and their successful imprint on the solid product. The result offers a general but significantly efficient route to creating precisely designed fine porous silica materials under mild condition that serve as low refractive index and efficient thermal insulation materials in their practical applications.

Effect of suspension characteristics on in-flight particle properties and coating microstructures achieved by suspension plasma spray

Science.gov (United States)

Aubignat, E.; Planche, M. P.; Allimant, A.; Billières, D.; Girardot, L.; Bailly, Y.; Montavon, G.

2014-11-01

This paper focuses on the influence of suspension properties on the manufacturing of coatings by suspension plasma spraying (SPS). For this purpose, alumina suspensions were formulated with two different liquid phases: water and ethanol. Suspensions were atomized with a twin-fluid nozzle and injected in an atmospheric plasma jet. Suspension injection was optimized thanks to shadowgraphy observations and drop size distribution measurements performed by laser diffraction. In-flight particle velocities were evaluated by particle image velocimetry. In addition, splats were collected on glass substrates, with the same conditions as the ones used during the spray process. Scanning electron microscopy (SEM) and profilometry analyses were then performed to observe the splat morphology and thus to get information on plasma / suspension interactions, such as particle agglomeration. Finally, coatings were manufactured, characterized by SEM and compared to each other.

Sol-gel materials for optofluidics - process and applications

DEFF Research Database (Denmark)

Mikkelsen, Morten Bo Lindholm

2011-01-01

This Ph.D. thesis is concerned with the use of sol-gel materials in optofluidic applications and the physics of DNA molecules in nanoconfinement. The bottom-up formation of solid material, which is provided by the sol-gel process, enables control of the chemical composition and porosity...... of the material. At early stages of gelation, thin gel coatings can be structured by nanoimprint lithography, and purely inorganic silica materials can be obtained by subsequent thermal annealing. The sol-gel process thus constitutes a unique method for nanofabrication of silica materials of special properties....... In this work, sol-gel silica is introduced as a new material class for the fabrication of lab-on-a-chip devices for DNA analysis. An imprint process with a rigid, non-permeable stamp was developed, which enabled fabrication of micro- and nanofluidic silica channels in a single process step without use of any...

Silica-Immobilized Enzyme Reactors

Science.gov (United States)

2007-08-01

Silica-IMERs 14 implicated in neurological disorders such as Schizophrenia and Parkinson’s disease.[86] Drug discovery for targets that can alter the...primarily the activation of prodrugs and proantibiotics for cancer treatments or antibiotic therapy , respectively.[87] Nitrobenzene nitroreductase was...BuChE) Monolith disks* Packed Silica Biosilica Epoxide- Silica Silica-gel Enzyme Human AChE Human AChE Human AChE Equine BuChE Human

Alkali passivation mechanism of sol-gel derived TiO2-SiO2 films coated on soda-lime-silica glass substrates

Energy Technology Data Exchange (ETDEWEB)

Matsuda, A; Matsuno, Y; Katayama, S; Tsuno, T [Nippon Steel Glass Co. Ltd., Tokyo (Japan); Toge, N; Minami, T [University of Osaka Prefecture, Osaka (Japan). College of Engineering

1992-09-01

TiO2-SiO2 films prepared by the sol-gel method serves as an effective alkali passivation layer on a soda-lime-silica glass substrate and the film is superior to a sol-gel derived pure SiO2 film from the view point of weathering resistance improvement. To clarify the reason, alkali passivation mechanism of sol-gel derived TiO2-SiO2 glass films with different TiO2 contents coated on a soda-lime-silica glass substrate was studied by SIMS (secondary ion mass spectroscopy) and XPS (X-ray photoelectron spectroscopy) analyses, and compared with the results of a sol-gel derived pure SiO2 film. As a result, the following conclusions were obtained: An increase in TiO2 content in the TiO2 SiO2 film increases the sodium concentration in the film, which was induced by sodium migration from the glass substrate during the heat-treatment. Because of the presence of sodium the TiO2 -SiO2 films serve not as a barrier but as an effective getter of alkali ions and thereby effectively improve the weathering resistance Of the glass substrate. 10 refs., 6 figs.

Replication of butterfly wing and natural lotus leaf structures by nanoimprint on silica sol-gel films

International Nuclear Information System (INIS)

Saison, Tamar; Peroz, Christophe; Chauveau, Vanessa; Sondergard, Elin; Arribart, Herve; Berthier, Serge

2008-01-01

An original and low cost method for the fabrication of patterned surfaces bioinspired from butterfly wings and lotus leaves is presented. Silica-based sol-gel films are thermally imprinted from elastomeric molds to produce stable structures with superhydrophobicity values as high as 160 deg. water contact angle. The biomimetic surfaces are demonstrated to be tuned from superhydrophobic to superhydrophilic by annealing between 200 deg. C and 500 deg. C

Replication of butterfly wing and natural lotus leaf structures by nanoimprint on silica sol-gel films

Energy Technology Data Exchange (ETDEWEB)

Saison, Tamar; Peroz, Christophe; Chauveau, Vanessa; Sondergard, Elin; Arribart, Herve [Unite mixte CNRS/Saint Gobain Saint Gobain Recherche, BP135, 93303 Aubervilliers (France); Berthier, Serge [Institut des Nanosciences de Paris, UMR 7588, CNRS, Universite Pierre et Marie Curie-Paris 6, 140 rue Lourmel, 75015 Paris (France)], E-mail: cperoz@lbl.gov

2008-12-01

An original and low cost method for the fabrication of patterned surfaces bioinspired from butterfly wings and lotus leaves is presented. Silica-based sol-gel films are thermally imprinted from elastomeric molds to produce stable structures with superhydrophobicity values as high as 160 deg. water contact angle. The biomimetic surfaces are demonstrated to be tuned from superhydrophobic to superhydrophilic by annealing between 200 deg. C and 500 deg. C.

Natural gels in the Yucca Mountain Area, Nevada, USA

International Nuclear Information System (INIS)

Levy, S.S.

1991-01-01

Relict gels at Yucca Mountain include pore- and fracture-fillings of silica and zeolite related to diagenetic and hydrothermal alternation of vitric tuffs. Water-rich free gels in fractures at Rainier Mesa consist of smectite with or without silica-rich gel fragments. Gels are being studied for their potential role in transport of radionuclides from a nuclear-waste repository

Epoxy-silica nanocomposite interphase control using task-specific ionic liquids via hydrolytic and non-hydrolytic sol-gel processes

Czech Academy of Sciences Publication Activity Database

Donato, Ricardo Keitel; Perchacz, Magdalena; Ponyrko, Sergii; Donato, Katarzyna Zawada; Schrekker, H. S.; Beneš, Hynek; Matějka, Libor

2015-01-01

Roč. 5, č. 111 (2015), s. 91330-91339 ISSN 2046-2069 R&D Projects: GA ČR(CZ) GA14-05146S; GA ČR GAP108/12/1459 Institutional support: RVO:61389013 Keywords : epoxy-silica nanocomposite * sol-gel processes * ionic liquids Subject RIV: CD - Macromolecular Chemistry Impact factor: 3.289, year: 2015

Applicability of Sol-Gel Derived Adsorbent for the Production of (n,f) 99Mo Generator

International Nuclear Information System (INIS)

Lee, Jun-Sig; Lee, Jong-Sup; Park, Ul-Jae; Son, Kwang-Jae; Han, Hyon-Soo; Kim, Myung Sic; Koo, Sung Chan; Chung, Young-Ju

2007-01-01

High performance adsorbents as the column material for (n,γ) 99 Mo/ 99 mTc and 188 W/ 188 Re generators have been developed at KAERI. These adsorbents should have enough loading capacities to produce such generators with high activities as the loading isotopes are not carrier-free. In this regard, the adsorbents are synthesized by sol-gel processing in which the ligand density can easily be adjusted and maximized. The marginal capacity of such adsorbents should be higher than 200 mg/g for molybdenum. From the previous works, the sol-gel processing techniques are adequately applied to meet the criteria. Further studies are being undertaken to employ the adsorbents for the production of high capacity (n,f) 99 Mo/ 99 mTc. Domestically, a private company has lined up the production facility of the molybdenum generator in the activity range of 300 ∼ 1,000 mCi/ea. The column elements are composed of manganese oxide doped on silica and alumina at the backup layer. In this column, the manganese oxide is the main reactive layer to retain (n,f) 99 Mo. The sol-gel derived adsorbent, in this study, is employed as the replacement of the manganese oxide doped silica in the column and tested for the loading efficiency of (n,f) 99 Mo, elution of 99 mTc, labeling property of the eluted 99 mTc. The same loading and elution procedures as the commercial production are applied for the tests and quality controls

Heterogeneous phase gamma irradiation of ethylene-hydrogen mixtures

International Nuclear Information System (INIS)

Molinari, M.A.; Lires, O.A.; Videla, G.J.

1975-11-01

Experiments of radioinduced ethylene hydrogenation were performed. The G yield of volatile saturated hydrocarbons was 0,49 for silica-gel with simultaneous irradiation and 0,09-0,05 for the other solids (silica-alumina and molecular sieve 5A). The highest yield corresponds to 4,5% of saturated products in relation to initial ammount of ethylene (silica-gel). Polymerization was the most important reaction, with yields as high as 95%. Changes in color and appearance of silica-aluminia in contact with moisture was observed, after the irradiation process. (author) [es

Amperometric detector for gas chromatography based on a silica sol-gel solid electrolyte.

Science.gov (United States)

Steinecker, William H; Miecznikowski, Krzysztof; Kulesza, Pawel J; Sandlin, Zechariah D; Cox, James A

2017-11-01

An electrochemical cell comprising a silica sol-gel solid electrolyte, a working electrode that protrudes into a gas phase, and reference and counter electrodes that contact the solid electrolyte comprises an amperometric detector for gas chromatography. Under potentiostatic conditions, a current related to the concentration of an analyte in the gas phase is produced by its oxidation at the three-phase boundary among the sol-gel, working electrode, and the gas phase. The sol-gel is processed to contain an electrolyte that also serves as a humidistat to maintain a constant water activity even in the presence the gas chromatographic mobile phase. Response was demonstrated toward a diverse set of analytes, namely hydrogen, 1,2-ethandithiol, phenol, p-cresol, and thioanisole. Using flow injection amperometry of hydrogen with He as the carrier gas, 90% of the steady-state current was achieved in < 1s at a flow rate of 20mLmin -1 . A separation of 1,2-ethandithiol, phenol, p-cresol, and thioanisole at a 2.2mLmin -1 flow rate was achieved with respective detection limits (k = 3 criterion) of 4, 1, 3, and 70 ppmv when the working electrode potential was 800mV. Copyright © 2017 Elsevier B.V. All rights reserved.

Performance comparison of a silica gel-water and activated carbon-methanol two beds adsorption chillers

Directory of Open Access Journals (Sweden)

Szelągowski Adam

2017-01-01

Full Text Available The aim of the study is to compare the efficiency of adsorption refrigerating equipment working with different working pairs. Adsorption cooling devices can operate with a relatively low temperature of heat sources while consuming only a small amount of electricity for the operation of auxiliary equipment. Refrigerants used in adsorption devices are substances that do not have a negative impact on the environment. All that makes that adsorption refrigeration seems to be a good solution for utilizing renewable and waste heat sources for cold production. To carry out the experiment the adsorption cooling device has been developed and researched in Institute of Heat Engineering at Warsaw University of Technology. The test bench consisted of two cylindrical adsorbers, condenser, evaporator, oil heater and two oil coolers. In order to perform the correct action it has been developed and implemented special control algorithm device, allowed to keep the temperature in the evaporator at a preset level. The unit tested for two sorption pairs: activated carbon – methanol, and silica gel – water. For activated carbon - methanol working pair it was obtained energy efficiency rating (EER equals to 0.14 and specific cooling power (SPC of 16 W/kg. For silica gel - water EER of refrigeration unit was 0.25 and SPC was equal to 208 W/kg.

Silica Gel Coated Spherical Micro resonator for Ultra-High Sensitivity Detection of Ammonia Gas Concentration in Air.

Science.gov (United States)

Mallik, Arun Kumar; Farrell, Gerald; Liu, Dejun; Kavungal, Vishnu; Wu, Qiang; Semenova, Yuliya

2018-01-26

A silica gel coated microsphere resonator is proposed and experimentally demonstrated for measurements of ammonia (NH 3 ) concentration in air with ultra-high sensitivity. The optical properties of the porous silica gel layer change when it is exposed to low (parts per million (ppm)) and even ultra-low (parts per billion (ppb)) concentrations of ammonia vapor, leading to a spectral shift of the WGM resonances in the transmission spectrum of the fiber taper. The experimentally demonstrated sensitivity of the proposed sensor to ammonia is estimated as 34.46 pm/ppm in the low ammonia concentrations range from 4 ppm to 30 ppm using an optical spectrum analyser (OSA), and as 800 pm/ppm in the ultra-low range of ammonia concentrations from 2.5 ppb to 12 ppb using the frequency detuning method, resulting in the lowest detection limit (by two orders of magnitude) reported to date equal to 0.16 ppb of ammonia in air. In addition, the sensor exhibits excellent selectivity to ammonia and very fast response and recovery times measured at 1.5 and 3.6 seconds, respectively. Other attractive features of the proposed sensor are its compact nature, simplicity of fabrication.

Catechol functionalized aminopropyl silica gel: synthesis, characterization and preconcentrative separation of uranium(VI) from thorium(IV)

Energy Technology Data Exchange (ETDEWEB)

Metilda, P.; Mary Gladis, J.; Prasada Rao, T.P. [Regional Research Lab. (CSIR), Trivandrum (India)

2005-07-01

A novel solid phase extractant is prepared by chemically immobilizing catechol with diazotized aminopropyl silica gel. The resulting catechol functionalized silica gel (CASG) was characterized by FTIR, and microanalysis and was used for selective enrichment of uranium(VI) from other inorganic ions. The optimum pH range for maximum sorption of uranium(VI) and thorium(IV) was found to be in the range 3.5-6.0. The above actinides were eluted with 10 cm{sup 3} of 1.0 mol dm{sup -3} HCl and determined by using an Arsenazo III spectrophotometric procedure. The calibration graph was rectilinear over the uranium(VI) concentration in the range 2-100 {mu}g dm{sup -3} with a relative standard deviation of 2.15% (for 25 {mu}g of uranium(VI) present in 1.0 dm{sup 3} of sample). The validation of the developed preconcentration procedure was carried out by analyzing marine sediment (MESS-3, NRC, Canada) and soil (IAEA soil-7, Austria) reference materials. The developed preconcentration method enables a simple instruments like a spectrophotometer gave comparable values of uranium(VI) to that of standard inductively coupled plasma-mass spectrometric values during the analysis of real soil and sediment samples. (orig.)

Modified silica sol coatings for surface enhancement of leather.

Science.gov (United States)

Mahltig, Boris; Vossebein, Lutz; Ehrmann, Andrea; Cheval, Nicolas; Fahmi, Amir

2012-06-01

The presented study reports on differently modified silica sols for coating applications on leather. Silica sols are prepared by acidic hydrolysis of tetraethoxysilane and modified by silane compounds with fluorinated and non-fluorinated alkylgroups. In contrast to many earlier investigations regarding sol-gel applications on leather, no acrylic resin is used together with the silica sols when applying on leather. The modified silica particles are supposed to aggregate after application, forming thus a modified silica coating on the leather substrate. Scanning electron microscopy investigation shows that the applied silica coatings do not fill up or close the pores of the leather substrate. However, even if the pores of the leather are not sealed by this sol-gel coating, an improvement of the water repellent and oil repellent properties of the leather substrates are observed. These improved properties of leather by application of modified silica sols can provide the opportunity to develop sol-gel products for leather materials present in daily life.

Study of the confined solutions properties: case of gel formed during nuclear glass alteration

International Nuclear Information System (INIS)

Matar-Briman, I.

2012-01-01

In this study, we have investigated the thermodynamic properties, the structure and the dynamics of confined solutions in model gels and in a gel coming from glass alteration. The first step was to determine the structure and the dynamics of pure confined water in porous materials by using nuclear magnetic resonance and neutron scattering. Meso-porous silica was elaborated and grafted by sol-gel route to decrease the pore sizes from 2.7 to 2 nm and to modify pore surfaces to have Si-OH, Zr-OH and Al-OH. The second step involved determining the dynamics of water in leachate confined in the model gels and in the gel of altered glass by using neutron scattering. In the model gels and at a 10 -12 -10 -9 second timescale, two kinds of waters were highlighted: first, an interfacial water linked to the pore surfaces and second, a free water in the pore core. Their ratio depends on the pore size and pore surface composition. Whatever the pore surface, when the pore size decreases the free water ratio in the pore center also decreases. For pores smaller than 2.3 nm and pore surfaces with Zr-OH or Al-OH surfaces, water is strongly linked to the surface and few water molecules are mobile. This is due to the ability of alumina and zirconia to immobilize water molecules through chemical coordination bonds stronger than the physical bonds established between silica and water. The result also highlight that pore surface composition could be the predominant parameter affecting the fixed proton content. Moreover, the mobility of water confined in a leachate is not modified. The study of the water dynamics in a gel formed during alteration of glass constituted of SiO 2 , Al 2 O 3 and CaO, and having a porosity between 2 and 7 nm showed the same behavior as water confined in pores presenting an Al-OH surface. (author) [fr

Gel/Space Ratio Evolution in Ternary Composite System Consisting of Portland Cement, Silica Fume, and Fly Ash.

Science.gov (United States)

Wu, Mengxue; Li, Chen; Yao, Wu

2017-01-11

In cement-based pastes, the relationship between the complex phase assemblage and mechanical properties is usually described by the "gel/space ratio" descriptor. The gel/space ratio is defined as the volume ratio of the gel to the available space in the composite system, and it has been widely studied in the cement unary system. This work determines the gel/space ratio in the cement-silica fume-fly ash ternary system (C-SF-FA system) by measuring the reaction degrees of the cement, SF, and FA. The effects that the supplementary cementitious material (SCM) replacements exert on the evolution of the gel/space ratio are discussed both theoretically and practically. The relationship between the gel/space ratio and compressive strength is then explored, and the relationship disparities for different mix proportions are analyzed in detail. The results demonstrate that the SCM replacements promote the gel/space ratio evolution only when the SCM reaction degree is higher than a certain value, which is calculated and defined as the critical reaction degree (CRD). The effects of the SCM replacements can be predicted based on the CRD, and the theological predictions agree with the test results quite well. At low gel/space ratios, disparities in the relationship between the gel/space ratio and the compressive strength are caused by porosity, which has also been studied in cement unary systems. The ratio of cement-produced gel to SCM-produced gel ( G C to G S C M ratio) is introduced for use in analyzing high gel/space ratios, in which it plays a major role in creating relationship disparities.

Gel/Space Ratio Evolution in Ternary Composite System Consisting of Portland Cement, Silica Fume, and Fly Ash

Directory of Open Access Journals (Sweden)

Mengxue Wu

2017-01-01

Full Text Available In cement-based pastes, the relationship between the complex phase assemblage and mechanical properties is usually described by the “gel/space ratio” descriptor. The gel/space ratio is defined as the volume ratio of the gel to the available space in the composite system, and it has been widely studied in the cement unary system. This work determines the gel/space ratio in the cement-silica fume-fly ash ternary system (C-SF-FA system by measuring the reaction degrees of the cement, SF, and FA. The effects that the supplementary cementitious material (SCM replacements exert on the evolution of the gel/space ratio are discussed both theoretically and practically. The relationship between the gel/space ratio and compressive strength is then explored, and the relationship disparities for different mix proportions are analyzed in detail. The results demonstrate that the SCM replacements promote the gel/space ratio evolution only when the SCM reaction degree is higher than a certain value, which is calculated and defined as the critical reaction degree (CRD. The effects of the SCM replacements can be predicted based on the CRD, and the theological predictions agree with the test results quite well. At low gel/space ratios, disparities in the relationship between the gel/space ratio and the compressive strength are caused by porosity, which has also been studied in cement unary systems. The ratio of cement-produced gel to SCM-produced gel ( G C to G S C M ratio is introduced for use in analyzing high gel/space ratios, in which it plays a major role in creating relationship disparities.

Kinetic evaluation of propyne surface diffusivity on silica-alumina-supported chromium(VI) using positron annihilation surface detection

International Nuclear Information System (INIS)

Ferrieri, R.A.; Wolf, A.P.

1984-01-01

A study has been performed on the rate of the translational surface diffusivity of propyne on a silica-alumina-supported Cr(VI) catalyst. This rate was measured via nonchemical acetylene-propyne sorbate interactions coupled with positron annihilation surface detection (PASD). The surface displacement rate of [ 11 C]acetylene by propyne was measured in a transient experiment as a function of the adjacent Cr-site distance and correlated to propyne surface diffusivity, D/sub s/. Results indicated that D/sub s/ increased linearly when the adjacent site distance was decreased for catalysts loaded with between 0.08 and 0.8 wt % of chromium. However, D/sub s/ fell off drastically to nearly zero when greater Cr-site dispersion was achieved at support loadings below 0.08 wt % of chromium. Catalytic selectivity for p-xylene production was also measured as a function of D/sub s/ and was shown to have a strong dependence of its rate. 25 references, 4 figures

Functionalization of {gamma}-alumina cores by polyvinylpirrolidone: properties of the resulting biocompatible nanoparticles in aqueous suspension

Energy Technology Data Exchange (ETDEWEB)

Fernandez, L. [Universidad Nacional del Comahue, Dpto de Quimica, Facultad de Ingenieria (Argentina); Arranz, G.; Palacio, L. [Universidad de Valladolid, Dpto. Fisica Aplicada, Facultad de Ciencias (Spain); Soria, C.; Sanchez, M.; Perez, G. [Universidad Nacional del Comahue, Dpto de Quimica, Facultad de Ingenieria (Argentina); Lozano, A. E. [UA-CSIC-UVA, Surface and Porous Materials (SMAP) (Spain); Hernandez, A.; Pradanos, P., E-mail: pradanos@termo.uva.e [Universidad de Valladolid, Dpto. Fisica Aplicada, Facultad de Ciencias (Spain)

2009-02-15

A biocompatible polymer has been used to functionalize 45-50 nm diameter {gamma}-alumina nanoparticles. Because the target was to use these systems in real applications, polyvinylpirrolidone (PVP) was chosen due to the characteristics of non-toxicity, biocompatibility, and feasibility of this polymer to form complexes with many cations and chemical species. This approach allows the use of these materials in medicine and food, textile, or pharmaceutical industry. The functionalization process required a previous attachment of an active group on the surface of the nanoparticles. Subsequently, a polymer chain was generated in situ, using vinyltrimethoxysilane (VTMS) and 1-vinyl-2-pyrrolidone (VP) as reactives. The morphology and topology of the nanocompound has been characterized in aqueous suspensions, attending to possible applications in this medium. The results obtained from the different techniques show that the polymer chain was successfully grafted to the nanoparticle surface, and allow an estimation of the size of the modified particle. Their electrical and conformational behavior have also been studied in different aqueous chemical environments.

Functionalization of γ-alumina cores by polyvinylpirrolidone: properties of the resulting biocompatible nanoparticles in aqueous suspension

International Nuclear Information System (INIS)

Fernandez, L.; Arranz, G.; Palacio, L.; Soria, C.; Sanchez, M.; Perez, G.; Lozano, A. E.; Hernandez, A.; Pradanos, P.

2009-01-01

A biocompatible polymer has been used to functionalize 45-50 nm diameter γ-alumina nanoparticles. Because the target was to use these systems in real applications, polyvinylpirrolidone (PVP) was chosen due to the characteristics of non-toxicity, biocompatibility, and feasibility of this polymer to form complexes with many cations and chemical species. This approach allows the use of these materials in medicine and food, textile, or pharmaceutical industry. The functionalization process required a previous attachment of an active group on the surface of the nanoparticles. Subsequently, a polymer chain was generated in situ, using vinyltrimethoxysilane (VTMS) and 1-vinyl-2-pyrrolidone (VP) as reactives. The morphology and topology of the nanocompound has been characterized in aqueous suspensions, attending to possible applications in this medium. The results obtained from the different techniques show that the polymer chain was successfully grafted to the nanoparticle surface, and allow an estimation of the size of the modified particle. Their electrical and conformational behavior have also been studied in different aqueous chemical environments.

Development and characterization of colloidal silica-based slow-release permanganate gel (SRP-G): laboratory investigations.

Science.gov (United States)

Lee, Eung Seok; Gupta, Neha

2014-08-01

Slow-release permanganate (MnO4(-)) gel (SRP-G) is a hyper-saline KMnO4 solution that can be used for treating large, dilute, or deep plumes of chlorinated solvents in groundwater. Ideally, the SRP-G injected into aquifers will slowly gelate to form MnO4(-) gel in situ, and the gel will slowly releases MnO4(-). Objectives of this study were to develop SRP-G using colloidal silica as gelling solution, characterize its gelation and release kinetics, and delineate its dynamics in a saturated sandy media. The SRP-G exhibited a two-phase increase in viscosity: a lag phase characterized by little increase in viscosity followed by a short gelation phase. Gelation lag times of SRP-G solutions increased (from 0.5h to 13d) with decreasing KMnO4 concentrations (from 25 to 8 g L(-1)). Permanganate release from gelated SRP-G increased with increasing KMnO4 concentrations, and was characterized as asymptotic release with initial peak (0.9-2.2 mg min(-1)) followed by more attenuated release. Gelation lag times of SRP-G flowing in sands (linear velocity=2.1md(-1)) increased (1, 3, and 6h) with decreasing KMnO4 concentrations (25.0, 23.0, and 22.9 g L(-1)). Permanganate release from gelated SRP-Gs continued for up to 3d and was characterized as asymptotic release with an initial peak release (∼1.2 g min(-1)) followed by more attenuated release over 70h. Dilution of SRP-G by dispersion in porous media affects gelation and release kinetics. Increasing the silica concentration in the SRP-G may facilitate gelation and extend the duration of MnO4(-) release from emplaced SRP-G in porous media. Copyright © 2014. Published by Elsevier Ltd.

Investigation of adsorption performance deterioration in silica gel–water adsorption refrigeration

International Nuclear Information System (INIS)

Wang Dechang; Zhang Jipeng; Xia Yanzhi; Han Yanpei; Wang Shuwei

2012-01-01

Highlights: ► Adsorption deterioration of silica gel in refrigeration systems is verified. ► Possible factors to cause such deterioration are analyzed. ► Specific surface area, silanol content and adsorption capacity are tested. ► The pollution is the primary factor to decline the adsorption capacity. ► Deteriorated samples are partly restored after being processed by acid solution. - Abstract: Silica gel acts as a key role in adsorption refrigeration systems. The adsorption deterioration must greatly impact the performance of the silica gel–water adsorption refrigeration system. In order to investigate the adsorption deterioration of silica gel, many different silica gel samples were prepared according to the application surroundings of silica gel in adsorption refrigeration systems after the likely factors to cause such deterioration were analyzed. The specific surface area, silanol content, adsorption capacity and pore size distribution of those samples were tested and the corresponding adsorption isotherms were achieved. In terms of the experimental data comparisons, it could be found that there are many factors to affect the adsorption performance of silica gel, but the pollution was the primary one to decline the adsorption capacity. In addition, the adsorption performance of the deteriorated samples after being processed by acid solution was explored in order to find the possible methods to restore its adsorption performance.

Effects of the silica nanoparticles (NPSiO2 on the stabilization and transport of hazardous nanoparticle suspensions into landfill soil columns

Directory of Open Access Journals (Sweden)

Elizabeth Mendes de Oliveira

Full Text Available Abstract This study evaluates the stability and transport behaviors of hazardous nanoparticles into soil landfills using experimental procedures to simulate the effects of natural silica nanoparticle suspensions during their percolation into the soil layers of municipal waste landfills. For this, we prepared stabilized suspensions of nanoparticle oxides containing silicon (NPSiO2, titanium (NPTiO2, copper (NPCuO and zinc (NPZnO, which are recognized as hazardous to the environment, and we conducted leaching experiments within the soil column by simulating landfills layers and simulating the capture and attenuation of nanomaterials into municipal waste landfills. The results demonstrated that the presence of NPSiO2 in suspensions increases the stable concentrations of copper, zinc and titanium oxides and strongly decreases soil layer effectiveness. In contrast, NPZnO improves effectiveness due to its ability to promote agglomeration and setting conditions, allowing further complexation.

Carbon monoxide adsorption studies on Ru:Mn bimetallic catalysts supported on alumina, silica and titania supported for the determination of metal surface area overview

International Nuclear Information System (INIS)

Hussain, S.T.

1992-01-01

Supported Ru: Mn bimetallic samples were studied using CO-chemisorption on alumina, silica and titania supports for the determination of active metal site/metal surface area. The data indicates the presence of Mn on the surface of Ru. With the increase of Mn loadings a decrease in the CO adsorption occurred indicating that presence of Mn masks the active sites responsible for Co-adsorption. On the titania supported system reduced at high and low temperature the CO-chemisorption data suggest the unusual behaviour. This behaviour is possibly caused due to creation of new active surface sites. (author)

Zirconia toughened SiC whisker reinforced alumina composites small business innovation research

Science.gov (United States)

Loutfy, R. O.; Stuffle, K. L.; Withers, J. C.; Lee, C. T.

1987-01-01

The objective of this phase 1 project was to develop a ceramic composite with superior fracture toughness and high strength, based on combining two toughness inducing materials: zirconia for transformation toughening and SiC whiskers for reinforcement, in a controlled microstructure alumina matrix. The controlled matrix microstructure is obtained by controlling the nucleation frequency of the alumina gel with seeds (submicron alpha-alumina). The results demonstrate the technical feasibility of producing superior binary composites (Al2O3-ZrO2) and tertiary composites (Al2O3-ZrO2-SiC). Thirty-two composites were prepared, consolidated, and fracture toughness tested. Statistical analysis of the results showed that: (1) the SiC type is the key statistically significant factor for increased toughness; (2) sol-gel processing with a-alumina seed had a statistically significant effect on increasing toughness of the binary and tertiary composites compared to the corresponding mixed powder processing; and (3) ZrO2 content within the range investigated had a minor effect. Binary composites with an average critical fracture toughness of 6.6MPam sup 1/2, were obtained. Tertiary composites with critical fracture toughness in the range of 9.3 to 10.1 MPam sup 1/2 were obtained. Results indicate that these composites are superior to zirconia toughened alumina and SiC whisker reinforced alumina ceramic composites produced by conventional techniques with similar composition from published data.

gel template method

Indian Academy of Sciences (India)

TiO2 nanotubes have been synthesized by sol–gel template method using alumina membrane. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy, UV absorption spectrum and X-ray diffraction techniques have been used to investigate the structure, morphology and optical ...

PENGARUH PERBEDAAN SIFAT PENYANGGA ALUMINA TERHADAP SIFAT KATALIS HYDROTREATING BERBASIS NIKEL-MOLIBDENUM

Directory of Open Access Journals (Sweden)

Maria Ulfah

2012-11-01

Full Text Available EFFECT OF ALUMINA SUPPORT PROPERTIES ON THE NICKEL-MOLIBDENUM BASE HYDROTREATING CATALYST. Effect of surface characteristics of three species of synthesized γ-alumina (alumina-1, alumina-2 and alumina-3 on characteristics NiMo catalysts has been studied. Those aluminas are derived from boehmite Catapal B by varying rasio mol nitric acid to boehmite. A sol-gel method is used to synthesize γ-Al2O3 support. The Nitrogen adsorption, X-ray diffraction (XRD, Temperature Programmed Reduction (TPR of H2, Temperature Programmed Desorption (TPD of NH3, and mechanical strength are used to characterize the supports and catalysts. The results showed that the surface area alumina affects the formation of crystalline MoO3 in the NiMo catalyst, while γ-Al2O3-3 support which has the highest surface area (about 195 m2/g compared to the other two types of alumina (>195 m2/g does not have a crystalline MoO3. The formation of crystalline MoO3 is not influenced by the acidity alumina. Based on the results of XRD, it is  indicated that the supported alumina-3 NiMo catalyst (having the highest acid strength shows that there is no presence of crystalline MoO3. Pore size distribution of support did not change significantly after the deposition of Ni and Mo oxides. Mechanical strength of support also affects the strength NiMo catalyst. Support alumina-3 which has the highest mechanical strength gives the mechanical strength of the highest NiMo catalyst. Pengaruh sifat penyangga γ-alumina hasil pengembangan (alumina-1, alumina-2 dan alumina-3 pada karakter katalis hydrotreating nikel-molibdenum (NiMo telah dipelajari. Ketiga jenis γ-alumina diturunkan dari boehmite “Catapal B” dengan menvariasikan nisbah mol asam nitrat terhadap boehmite. Pembuatan γ-alumina menggunakan metoda sol-gel. Adsorpsi Nitrogen, X-ray difraksi (XRD, Temperature Programmed Reduction (TPR H2, Temperature Programmed Desorption (TPD NH3, dan kekuatan mekanik digunakan untuk

Ion-conductive properties of polyether-based composite electrolytes filled with mesoporous silica, alumina and titania

International Nuclear Information System (INIS)

Tominaga, Yoichi; Endo, Masanori

2013-01-01

Composite polymer electrolytes were prepared consisting of amorphous polyether, Li salt and mesoporous inorganic filler, and we investigated their ion-conductive properties. We synthesized three types of filler, mesoporous silica, alumina and titania (MP-Si, Al, Ti), and characterized their structural and physicochemical properties using SEM, TEM, SAXS and BET surface area measurements. From these measurements, we confirmed that MP fillers have well-defined arrays of mesoporous and hexagonal structures. Dependence on the MP filler content of the glass transition temperature (T g ) revealed that the addition of filler to original polyether-salt electrolyte causes T g decrease, to due to the dissociation of aggregated ions such as triples or crystalline complex domains. The MP-Ti composites had the greatest ionic conductivity (1.4 × 10 −5 S/cm, 7.5 wt% at 30 °C) of all samples, and the values were more than double that of the original. The addition of MP-Ti also increased the lithium transference number, because the electrolyte/filler interface provided active sites that increase mobile Li ions and conducting paths so as to enhance the mobility

Sinus lift using a nanocrystalline hydroxyapatite silica gel in severely resorbed maxillae: histological preliminary study.

Science.gov (United States)

Canullo, Luigi; Dellavia, Claudia

2009-10-01

The aim of this preliminary study was to evaluate histologically a nanocrystalline hydroxyapatite silica gel in maxillary sinus floor grafting in severely resorbed maxillae. A total of 16 consecutive patients scheduled for sinus lift were recruited during this study. Patients were randomly divided in two groups, eight patients each. In both groups, preoperative residual bone level ranged between 1 and 3 mm (mean value of 2.03 mm). No membrane was used to occlude the buccal window. Second surgery was carried out after a healing period of 3 months in Group 1 and 6 months in Group 2. Using a trephine bur, one bone specimen was harvested from each augmented sinus and underwent histological and histomorphometric analysis. Histological analysis showed significant new bone formation and remodeling of the grafted material. In the cores obtained at 6 months, regenerated bone, residual NanoBone, and bone marrow occupied respectively 48 +/- 4.63%, 28 +/- 5.33%, and 24 +/- 7.23% of the grafted volume. In the specimens taken 3 months after grafting, mean new bone was 8 +/- 3.34%, mean NanoBone was 45 +/- 5.10%, and mean bone marrow was 47 +/- 6.81% of the bioptical volume. Within the limits of this preliminary prospective study, it was concluded that grafting of maxillary sinus using nanostructured hydroxyapatite silica gel as only bone filler is a reliable procedure also in critical anatomic conditions and after early healing period.

Disiloxanes and Functionalized Silica Gels: One Route, Two Complementary Outcomes-Guanidinium and Pyridinium Ion-Exchangers.

Directory of Open Access Journals (Sweden)

Łukasz Tabisz

Full Text Available Five novel disiloxane compounds comprising guanidinium and pyridinium moieties were obtained with high yields and purity. The verified synthetic pathways were then applied for modification of pre-functionalized silica gel, producing materials with the analogous organic side-chains. These halide-containing compounds and materials were then compared as to their ion-exchange properties: two disiloxanes proved to be effective in leaching different anions (nitrate, benzoate and ascorbate from solid to organic phase, and pyridinium-functionalized silica gels showed selectivity towards perchlorate ion, removing it from methanolic solutions with preference to other singly charged anions. The results presented demonstrate that both compounds and materials containing silicon-carbon bonds can be produced using the same methodology, but offer strikingly different application opportunities. Comparison of their properties provides additional insight into the binding mode of different anions and hints at how the transition from a flexible siloxane bridge to immobilization on solid surface influences anion-binding selectivity. Additionally, one of the siloxane dipodands was found to form a crystalline and poorly soluble nitrate salt (1.316 g/L, water, although it was miscible with a wide range of solvents as a hydrochloride. A possible explanation is given with the help of semi-empirical calculations. A simple, time- and cost-efficient automated potentiometric titration methodology was used as a viable analytical tool for studying ion-exchange processes for both compounds and materials, in addition to standard NMR, FT-IR and ESI-MS methods.

Sol-gel encapsulation for controlled drug release and biosensing

Science.gov (United States)

Fang, Jonathan

The main focus of this dissertation is to investigate the use of sol-gel encapsulation of biomolecules for controlled drug release and biosensing. Controlled drug release has advantages over conventional therapies in that it maintains a constant, therapeutic drug level in the body for prolonged periods of time. The anti-hypertensive drug Captopril was encapsulated in sol-gel materials of various forms, such as silica xerogels and nanoparticles. The primary objective was to show that sol-gel silica materials are promising drug carriers for controlled release by releasing Captopril at a release rate that is within a therapeutic range. We were able to demonstrate desired release for over a week from Captopril-doped silica xerogels and overall release from Captopril-doped silica nanoparticles. As an aside, the antibiotic Vancomycin was also encapsulated in these porous silica nanoparticles and desired release was obtained for several days in-vitro. The second part of the dissertation focuses on immobilizing antibodies and proteins in sol-gel to detect various analytes, such as hormones and amino acids. Sol-gel competitive immunoassays on antibody-doped silica xerogels were used for hormone detection. Calibration for insulin and C-peptide in standard solutions was obtained in the nM range. In addition, NASA-Ames is also interested in developing a reagentless biosensor using bacterial periplasmic binding proteins (bPBPs) to detect specific biomarkers, such as amino acids and phosphate. These bPBPs were doubly labeled with two different fluorophores and encapsulated in silica xerogels. Ligand-binding experiments were performed on the bPBPs in solution and in sol-gel. Ligand-binding was monitored by fluorescence resonance energy transfer (FRET) between the two fluorophores on the bPBP. Titration data show that one bPBP has retained its ligand-binding properties in sol-gel.

Remaining Sites Verification Package for the 100-F-44:4, Discovery Pipeline in Silica Gel Pit. Attachment to Waste Site Reclassification Form 2008-030

International Nuclear Information System (INIS)

Capron, J.M.

2008-01-01

The 100-F-44:4, Discovery Pipeline in Silica Gel Pit subsite is located in the 100-FR-1 Operable Unit of the Hanford Site, near the location of the former 110-F Gas Storage Tanks structure. The 100-F-44:4 subsite is a steel pipe discovered October 17, 2004, during trenching to locate the 118-F-4 Silica Gel Pit. Based on visual inspection and confirmatory investigation sampling data, the 100-F-44:4 subsite is a piece of non-hazardous electrical conduit debris. The 100-F-44:4 subsite supports unrestricted future use of shallow zone soil and is protective of groundwater and the Columbia River. No residual contamination exists within the deep zone. Therefore, no deep zone institutional controls are required

Simple measurement of 14C in the environment using a gel suspension method

International Nuclear Information System (INIS)

Wakabayashi, G.; Ohura, H.; Okai, T.; Matoba, M.

1999-01-01

A simple analytical method for environmental 14 C with a low background liquid scintillation counter was developed. A new gelling agent, N-lauroyl-L-glutamic-α,γ-dibutylamide was used, for the liquid scintillation counting of 14 C as CaCO 3 (gel suspension method). Our procedure for sample preparation was much simpler than that of conventional methods and required no special equipment. The samples prepared with the standard sample of CaCO 3 were measured to evaluate the self absorption of the sample, the optimum condition of counting and the detection limit. Our results indicated that the newly developed technique could be efficiently applied for the monitoring of environmental 14 C. (author)

Sugarcane bagasse lignin, and silica gel and magneto-silica as drug vehicles for development of innocuous methotrexate drug against rheumatoid arthritis disease in albino rats

International Nuclear Information System (INIS)

Wahba, Sanaa M.R.; Darwish, Atef S.; Shehata, Iman H.; Abd Elhalem, Sahar S.

2015-01-01

The present study clarifies co-therapy action of deliveries from their textural changes point of view. Methotrexate (MTX) was immobilized onto biodegradable lignin, silica gel and iron/silica nanocomposite. Loaded-MTX was i.p. injected into albino rats at doses of 0.25 and 0.5 mg/kg/week for 2.5 months, after which spleen, liver, testes and knee joint tissues were collected for tests. IFN-γ and IL-17A mRNA gene expressions in spleen in all biological samples were determined by RT-PCR. Physicochemical features of drug carriers were monitored by XRD, BET-PSD, SEM and TEM. Drug inflammatory-site targeting was found to be closely related to the physico-features of deliverers. The interlayered lignin of micro- and meso-pore channels directed MTX toward concealed infected cells in liver and testes tissues, while meso-structured silica flacks satisfied by gathering MTX around knee joints. The magneto-silica nanocomposite targeted MTX toward spleen tissue, which is considered as a lively factory for the production of electron rich compounds. - Highlights: • Opening the door to synthesize smart targeted drug deliveries against RA disease • Therapy action of MTX-laden lignin and Fe 3 O 4 /SiO 2 composite toward RA disease • Procure selective targeted drug deliveries of near 100% curing against RA disease • Revolutionary clinical therapies for RA disease by inventive MTX-delivery models

Defect-induced luminescence in sol-gel silica samples doped with Co(II) at different concentrations

Energy Technology Data Exchange (ETDEWEB)

Jimenez-Sandoval, S. [Centro de Investigacion y Estudios Avanzados, Queretaro, Apdo. Postal 1-798, Queretaro, Qro. 76001 (Mexico); Estevez, M. [Fisica Aplicada y Tecnologia Avanzada, UNAM, Apdo. Postal 1-1010, Queretaro, Qro. 76000 (Mexico); Pacheco, S. [Instituto Mexicano del Petroleo, Av. 100 metros (Mexico); Vargas, S. [Fisica Aplicada y Tecnologia Avanzada, UNAM, Apdo. Postal 1-1010, Queretaro, Qro. 76000 (Mexico); Rodriguez, R. [Fisica Aplicada y Tecnologia Avanzada, UNAM, Apdo. Postal 1-1010, Queretaro, Qro. 76000 (Mexico)], E-mail: rogelior@servidor.unam.mx

2007-12-20

The defect-induced luminescence properties of silica samples prepared by the sol-gel method and doped with Co(II) are reported. Silica monoliths doped with different concentrations of Co(II) were laser irradiated (He-Ne 632.8 nm) producing fluorescence. However, this fluorescence is exponentially reduced with the irradiation time, to practically disappear. The rate the fluorescence decays can be well modeled with a double exponential function of the irradiation time, containing two different relaxation times; a baseline is also required to take into account some residual fluorescence. The characteristic times involved in this luminescence quenching process are in the range of seconds. This luminescence suppression can be associated to the local heating produced by the laser irradiation when focused in a small area (2 {mu}m in diameter) on the sample. This heating process reduces physical (grain boundaries, surface states) and chemical (oxygen vacancies produced by the dopant) defects in the sample.

Binding of Sr from milk by solid phase extraction with cryptand C222 sorbed on silica gel, cation exchange, chelating or adsorbent resins for simplified 90Sr analysis

International Nuclear Information System (INIS)

Tait, David; Wiechen, Arnold; Haase, Gerhard

1995-01-01

Several commercially available resins have been found to bind the bicyclic polyether cryptand C222 from aqueous acetonitrile solutions. The presence of C222 on some of these resins strongly improved their affinity for Sr, so that relatively small amounts of such resins sorbed Sr from milk. The resins investigated were silica gel, polyacrylic acid crosslinked with divinylbenzene (DVB), polystyrene crosslinked with divinylbenzene (PS-DVB) and PS-DVB containing sulphonate, aminomethylphosphonate, iminodiacetate and mercapto groups. The resins for which binding of C222 resulted in the largest improvement in Sr sorption from milk were PS-DVB containing mercapto groups (Chelite S) and silica gel (Si 60). Thus, 2 ml wet volume of either Chelite S containing 133 μmol of C222, or silica gel Si-60 containing 143 μmol of C222 sorbed 90 and 48%, respectively, of the Sr from 100-ml milk samples. As the sorption of Sr from milk by these systems is relatively slow, contact times of 24-36 h are required to attain these results. The Chelite S-C222 system separates Sr effectively from Cs and Ca. Under the conditions described here some 6% of the natural 40 K in milk sorbs with Sr to the resin. Ba behaves similarly to Sr. 90 Sr/ 90 Y sorbed on the silica gel Si-60-C222 system can be measured directly and efficiently by liquid scintillation counting. If adequate specificity can be attained this system might provide a very simple method of determining 90 Sr in milk

Initial investigation of a novel light-scattering gel phantom for evaluation of optical CT scanners for radiotherapy gel dosimetry

International Nuclear Information System (INIS)

Bosi, Stephen; Naseri, Pourandokht; Puran, Alicia; Davies, Justin; Baldock, Clive

2007-01-01

There is a need for stable gel materials for phantoms used to validate optical computerized tomography (CT) scanners used in conjunction with radiation-induced polymerizing gel dosimeters. Phantoms based on addition of light-absorbing dyes to gelatine to simulate gel dosimeters have been employed. However, to more accurately simulate polymerizing gels one requires phantoms that employ light-scattering colloidal suspensions added to the gel. In this paper, we present the initial results of using an optical CT scanner to evaluate a novel phantom in which radiation-exposed polymer gels are simulated by the addition of colloidal suspensions of varying turbidity. The phantom may be useful as a calibration transfer standard for polymer gel dosimeters. The tests reveal some phenomena peculiar to light-scattering gels that need to be taken into account when calibrating polymer gel dosimeters

Sol–gel-based silver nanoparticles-doped silica – Polydiphenylamine nanocomposite for micro-solid-phase extraction

Energy Technology Data Exchange (ETDEWEB)

Bagheri, Habib, E-mail: bagheri@sharif.edu; Banihashemi, Solmaz

2015-07-30

A nanocomposite of silica-polydiphenylamine doped with silver nanoparticles (Ag–SiO{sub 2}-PDPA) was successfully synthesized by the sol–gel process. For its preparation, PDPA was mixed with butanethiol capped Ag nanoparticles (NPs) and added to the silica sol solution. The Ag NPs were stabilized as a result of their adsorption on the SiO{sub 2} spheres. The surface characteristic of nanocomposite was investigated using scanning electron microscopy (SEM). In this work the Ag–SiO{sub 2}-PDPA nanocomposite was employed as an efficient sorbent for micro-solid-phase extraction (μ-SPE) of some selected pesticides. An amount of 15 mg of the prepared sorbent was used to extract and determine the representatives from organophosphorous, organochlorine and aryloxyphenoxy propionic acids from aqueous samples. After the implementation of extraction process, the analytes were desorbed by methanol and determined using gas chromatography–mass spectrometry (GC–MS). Important parameters influencing the extraction and desorption processes such as pH of sample solution, salting out effect, type and volume of the desorption solvent, the sample loading and eluting flow rates along with the sample volume were experimentally optimized. Limits of detection (LODs) and the limits of quantification (LOQs) were in the range of 0.02–0.05 μg L{sup −1} and 0.1–0.2 μg L{sup −1}, respectively, using time scheduled selected ion monitoring (SIM) mode. The relative standard deviation percent (RSD %) with four replicates was in the range of 6–10%. The applicability of the developed method was examined by analyzing different environmental water samples and the relative recovery (RR %) values for the spiked water samples were found to be in the range of 86–103%. - Highlights: • A sol–gel-based silver nanoparticles doped silica-polydiphenylamine nanocomposite was synthesized. • The sorbent was applied to micro-solid-phase extraction of some selected pesticides in water

Preparation of Silica Modified with 2-Mercaptoimidazole and its SorptionProperties of Chromium(III

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Harry Budiman

2009-01-01

Full Text Available Modified silica gel was prepared to remove the heavy metal of chromium(III from water sample. Silica gel was used as supporting material and the 2-mercaptoimidazole was immobilized onto surface silica so that the silica would have selective properties to adsorb the heavy metal chromium(III through the formation of coordination compound between the 2-mercaptoimidazole and chromium(III. The characterization of modified silica gel was carried out by analyzing the Fourier Transform Infrared Spectrum of this material in order to ensure the immobilization of 2-mercaptoimidazole onto the surface. The effect of pH solution, initial concentration of chromium(III, and interaction time were investigated in batch mode to find the adsorption properties of chromium(III onto modified silica. The condition optimum of these parameters was applied to determine the removal percentage of chromium(III in water sample using the modified silica gel

Synthesis and Gas Transport Properties of Hyperbranched Polyimide–Silica Hybrid/Composite Membranes

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Masako Miki

2013-12-01

Full Text Available Hyperbranched polyimide–silica hybrids (HBPI–silica HBDs and hyperbranched polyimide–silica composites (HBPI–silica CPTs were prepared, and their general and gas transport properties were investigated to clarify the effect of silica sources and preparation methods. HBPI–silica HBDs and HBPI–silica CPTs were synthesized by two-step polymerization of A2 + B3 monomer system via polyamic acid as precursor, followed by hybridizing or blending silica sources. Silica components were incorporated by the sol-gel reaction with tetramethoxysilane (TMOS or the addition of colloidal silica. In HBPI-silica HBDs, the aggregation of silica components is controlled because of the high affinity of HBPI and silica caused by the formation of covalent bonds between HBPI and silica. Consequently, HBPI-silica HBDs had good film formability, transparency, and mechanical properties compared with HBPI-silica CPTs. HBPI-silica HBD and CPT membranes prepared via the sol-gel reaction with TMOS showed specific gas permeabilities and permselectivities for CO2/CH4 separation, that is, both CO2 permeability and CO2/CH4 selectivity increased with increasing silica content. This result suggests that gas transport can occur through a molecular sieving effect of the porous silica network derived from the sol-gel reaction and/or through the narrow interfacial region between the silica networks and the organic matrix.

Hydrogen generation systems utilizing sodium silicide and sodium silica gel materials

Science.gov (United States)

Wallace, Andrew P.; Melack, John M.; Lefenfeld, Michael

2015-07-14

Systems, devices, and methods combine reactant materials and aqueous solutions to generate hydrogen. The reactant materials can sodium silicide or sodium silica gel. The hydrogen generation devices are used in fuels cells and other industrial applications. One system combines cooling, pumping, water storage, and other devices to sense and control reactions between reactant materials and aqueous solutions to generate hydrogen. Multiple inlets of varied placement geometries deliver aqueous solution to the reaction. The reactant materials and aqueous solution are churned to control the state of the reaction. The aqueous solution can be recycled and returned to the reaction. One system operates over a range of temperatures and pressures and includes a hydrogen separator, a heat removal mechanism, and state of reaction control devices. The systems, devices, and methods of generating hydrogen provide thermally stable solids, near-instant reaction with the aqueous solutions, and a non-toxic liquid by-product.

Sol-gel technology for biomedical engineering

International Nuclear Information System (INIS)

Podbielska, H.; Ulatowska-Jarza, A.

2005-01-01

Sol-gel derived silica possess many promising features, including low-temperature preparation procedure, porosity, chemical and physical stability. Applications exploiting porous materials to encapsulate sensor molecules, enzymes and many other compounds, are developing rapidly. In this paper some potential applications, with emphasis on biomedical and environmental ones, are reviewed. The material preparation procedure is described and practical remarks on silica-based sol-gels are included. It is reported that sol-gels with entrapped various molecules may be used in construction of implants and coatings with bioactive properties. It is shown how to exploit the sol-gel production route for construction of sol-gel coated fiberoptic applicators for laser therapy. The applications of bioactive materials are discussed, as well. It is demonstrated that it is possible to immobilize photosensitive compounds in sol-gel matrix without loosing their photoactivity. Some examples of sol-gel based biosensors are demonstrated, as well, showing their potential for detecting various gases, toxic substances, acidity, humidity, enzymes and biologically active agents. (authors)

Novas técnicas de reometria aplicadas a suspensões cerâmicas Novel rheometric techniques applied to ceramic suspensions

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R. D. dos Anjos

2005-06-01

Full Text Available Suspensões cerâmicas com adequado comportamento reológico são imprescindíveis para a aplicação, adequação do processamento e otimização das propriedades finais dos produtos. No entanto, o uso de técnicas de reometria para análise de suspensões cerâmicas foi pouco explorado na literatura, quando comparado a outros sistemas, tais como polímeros fundidos. Desse modo, pretende-se demonstrar que o emprego de técnicas mais modernas de reometria permite uma nova compreensão desses materiais e das interações entre seus componentes. Neste trabalho foi estabelecida uma metodologia de análise para sistemas cerâmicos tendo como objeto de pesquisa uma suspensão de alumina e sol de sílica. Foi realizada uma série de medidas de viscosidade (eta, módulos de armazenamento (G' e de perda (G" e de força normal (Fn, cujos resultados servirão de base para estudos posteriores no mesmo sistema, visando aplicação em concretos refratários.Ceramic suspensions with suitable rheological properties are essential on application, process control and optimization of end products and properties. Nevertheless, the use of rheometric techniques to analyze such suspensions has been scarcely studied when compared to other systems, such as molten polymers. Therefore, in the present work, novel rheometric techniques will be presented which can allow a further understanding regarding these materials and the interaction among their components. A systematic study applying these techniques was established and the viscosity, storage modulus, loss modulus and normal force measurements were evaluated in a ceramic suspension containing alumina and silica sol. These results will be the fundaments for further studies, aiming their application on refractory castables.

Sugarcane bagasse lignin, and silica gel and magneto-silica as drug vehicles for development of innocuous methotrexate drug against rheumatoid arthritis disease in albino rats

Energy Technology Data Exchange (ETDEWEB)

Wahba, Sanaa M.R. [Zoology department, Women College, Ain-Shams University,11566 Cairo (Egypt); Darwish, Atef S., E-mail: atef_mouharam@sci.asu.edu.eg [Chemistry department, Faculty of Science, Ain Shams University, Cairo (Egypt); Shehata, Iman H. [Microbiology and Immunology Department, Faculty of Medicine, Ain-Shams University, Cairo (Egypt); Abd Elhalem, Sahar S. [Zoology department, Women College, Ain-Shams University,11566 Cairo (Egypt)

2015-03-01

The present study clarifies co-therapy action of deliveries from their textural changes point of view. Methotrexate (MTX) was immobilized onto biodegradable lignin, silica gel and iron/silica nanocomposite. Loaded-MTX was i.p. injected into albino rats at doses of 0.25 and 0.5 mg/kg/week for 2.5 months, after which spleen, liver, testes and knee joint tissues were collected for tests. IFN-γ and IL-17A mRNA gene expressions in spleen in all biological samples were determined by RT-PCR. Physicochemical features of drug carriers were monitored by XRD, BET-PSD, SEM and TEM. Drug inflammatory-site targeting was found to be closely related to the physico-features of deliverers. The interlayered lignin of micro- and meso-pore channels directed MTX toward concealed infected cells in liver and testes tissues, while meso-structured silica flacks satisfied by gathering MTX around knee joints. The magneto-silica nanocomposite targeted MTX toward spleen tissue, which is considered as a lively factory for the production of electron rich compounds. - Highlights: • Opening the door to synthesize smart targeted drug deliveries against RA disease • Therapy action of MTX-laden lignin and Fe{sub 3}O{sub 4}/SiO{sub 2} composite toward RA disease • Procure selective targeted drug deliveries of near 100% curing against RA disease • Revolutionary clinical therapies for RA disease by inventive MTX-delivery models.

Silica-gel structural characterization during the initial phases of gelation and drying

International Nuclear Information System (INIS)

Ferreira, Max Passos

1996-01-01

For centuries, glasses and ceramics have been made via melting or solid state reactions at temperatures above 100 deg C. The sol-gel process offers new approaches to the synthesis of glasses and ceramics, combining control of composition and structure at the molecular level with the ability to shape materials in bulk, powder, fiber and thin-film forms. The growth of sol-gel technology research is due to the many unique features of that class of materials. Major applications include optical elements and integrated optical devices, ceramic filters, membranes, supercondutors, magnetic, catalytic and manostructured materials to antioxidant, anticorrosion coatings and composite and biomedical materials. In this work a variety of techniques like spectroscopy, Raman spectroscopy, ultraviolet-visible spectroscopy, light scattering nuclear magnetic resonance, X ray diffraction and nitrogen adsorption have been employed to investigate the initial phase of the sol-gel transition of gamma ray irradiated tetramethoxysilane (TMOS) solutions and non-irradiated TMOS solution and to get information about the structure of the silica gels obtained under different gelation conditions. Typically the tetramethoxysilane solutions were prepared using a molar ratio of TMOS to demineralized water of 1 to 16. Some experiments were made under catalysed conditions. The mixing was carried out at room temperature. The turbidity and light scattering experiments on the polycondensation of tetramethoxysilane show that exists no drastic difference in the gelling time of a gamma ray irradiated and a non-irradiated TMOS+H 2 O (1+16 M) solution. In the absence of a catalyst, the gelling time for both reactions occurs in about 3.30 h. When HNO 3 (o.03 M) was used, the gelling time observed was 3 days. Raman and ultraviolet-visible spectroscopy show no drastic difference during the initial phase at the sol-gel transition under ambient temperature/pressure and under gamma radiation. The gels heated

X-ray absorption spectroscopy of U (VI) sorbed onto alumina

International Nuclear Information System (INIS)

Kumar, Sumit; Jain, Aishwarya; Tomar, B.S.; Manchanda, V.K.; Poswal, A.K.; Jha, S.N.; Sabharwal, S.C.

2009-01-01

Sorption of U (VI) by alumina varying pH has been studied by X-ray absorption Spectroscopy. The experiments were carried out using the EXAFS beamline (BL-8) of INDUS-2 at Raja Ramanna Centre for Advanced Technology, Indore. The absorption intensity was found to increase with the increasing pH of the suspension. (author)

Novel Approach for Enhanced Scandium and Titanium Leaching Efficiency from Bauxite Residue with Suppressed Silica Gel Formation.

Science.gov (United States)

Alkan, Gözde; Yagmurlu, Bengi; Cakmakoglu, Seckin; Hertel, Tobias; Kaya, Şerif; Gronen, Lars; Stopic, Srecko; Friedrich, Bernd

2018-04-04

The need of light weight alloys for future transportation industry puts Sc and Ti under a sudden demand. While these metals can bring unique and desired properties to alloys, lack of reliable sources brought forth a supply problem which can be solved by valorization of the secondary resources. Bauxite residue (red mud), with considerable Ti and Sc content, is a promising resource for secure supply of these metals. Due to drawbacks of the direct leaching route from bauxite residue, such as silica gel formation and low selectivity towards these valuable metals, a novel leaching process based on oxidative leaching conditions, aiming more efficient and selective leaching but also considering environmental aspects via lower acid consumption, was investigated in this study. Combination of hydrogen peroxide (H 2 O 2 ) and sulfuric acid (H 2 SO 4 ) was utilized as the leaching solution, where various acid concentrations, solid-to-liquid ratios, leaching temperatures and times were examined in a comparative manner. Leaching with 2.5 M H 2 O 2 : 2.5 M H 2 SO 4 mixture at 90 °C for 30 min was observed to be the best leaching conditions with suppressed silica gel formation and the highest reported leaching efficiency with high S/L ratio for Sc and Ti; 68% and 91%; respectively.

Synthesis and new structure shaping mechanism of silica particles formed at high pH

International Nuclear Information System (INIS)

Zhang, Henan; Zhao, Yu; Akins, Daniel L.

2012-01-01

For the sol–gel synthesis of silica particles under high pH catalytic conditions (pH>12) in water/ethanol solvent, we have deduced that the competing dynamics of chemical etching and sol–gel process can explain the types of silica particles formed and their morphologies. We have demonstrated that emulsion droplets that are generated by adding tetraethyl orthosilicate (TEOS) to a water–ethanol solution serve as soft templates for hollow spherical silica (1–2 μm). And if the emulsion is converted by the sol–gel process, one finds that suspended solid silica spheres of diameter of ∼900 nm are formed. Moreover, several other factors are found to play fundamental roles in determining the final morphologies of silica particles, such as by variation of the pH (in our case, using OH – ) to a level where condensation dominates; by changing the volume ratios of water/ethanol; and using an emulsifier (specifically, CTAB) - Graphical abstract: “Local chemical etching” and sol–gel process have been proposed to interpret the control of morphologies of silica particles through varying initial pHs in syntheses. Highlights: ► Different initial pHs in our syntheses provides morphological control of silica particles. ► “Local chemical etching” and sol–gel process describes the formation of silica spheres. ► The formation of emulsions generates hollow silica particles.

Granulated Silica Method for the Fiber Preform Production

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Sönke Pilz

2017-07-01

Full Text Available During the past few years, we have studied the granulated silica method as a versatile and cost effective way of fiber preform production and the sol-gel method. Until now, we have used the sol-gel technology together with an iterative re-melting and milling step in order to produce rare earth or transition metal doped granular material for the granulated silica method. Here, we present that the iterative re-melting (laser-assisted and milling step is no longer needed to reach a high homogeneity. The sol-gel method also offers a high degree of compositional flexibility with respect to dopants; it further facilitates achieving high concentrations, even in cases when several dopants are used. We employed optical active doped sol-gel derived granulate for the fiber core, whereas pure or index-raised granulated silica has been employed for the cladding. Based on the powder-in-tube technique, where silica glass tubes are appropriately filled with these granular materials, fibers has been directly drawn (“fiber rapid prototyping”, or eventually after an additional optional quality enhancing vitrification step. The powder-in-tube technique is also ideally suited for the preparation of microstructured optical fibers.

Topotactic preparation of textured alumina ceramics from dehydroxylation of gibbsite films

Energy Technology Data Exchange (ETDEWEB)

Louaer, Seif-Eddine; Wang, Yao, E-mail: yao@buaa.edu.cn; Guo, Lin, E-mail: guolin@buaa.edu.cn

2014-11-14

In this paper, textured alumina ceramics were prepared from dehydroxylation of gibbsite films and the pseudomorphic and topotactic nature of the dehydroxylation of textured gibbsite films has been investigated. First, the precursor film with a (001)-textured structure was obtained via vacuum filtration deposition of diluted aqueous suspensions of gibbsite nanoplatelets. Subsequently, (001)-textured α-alumina ceramics were successfully achieved by sintering of the deposited gibbsite films without addition of α-alumina seeds. The Scanning Electron Microscope (SEM) and X-ray Diffraction (XRD) results show that, during the phase transition from gibbsite to α-alumina, both layered morphology and crystal's axis orientation have been retained to a considerable extent. For the first time, a direct XRD evidence of gibbsite topotactic dehydroxylation to the α-alumina phase is presented. It is believed that the method described here exploits gibbsite's pseudomorphic and topotactic dehydroxylation, not on individual particles scale but on a bulk form. The resulting structure can be considered as inorganic scaffolds which can have applications for fabrication of dense, textured alumina-based ceramics and other layered/textured nanocomposites. - Highlights: • Gibbsite nanoplatelets were assembled on their basal plane to form (001)-textured films. • Textured alumina ceramics were prepared by sintering textured gibbsite films without addition of α-alumina seeds. • Both pseudomorphic and topotactic aspects were exploited in bulk form instead of individual nanoparticulate size. • Direct XRD evidence of the topotactic dehydroxylation from gibbsite to α-alumina is presented in this work.

Topotactic preparation of textured alumina ceramics from dehydroxylation of gibbsite films

International Nuclear Information System (INIS)

Louaer, Seif-Eddine; Wang, Yao; Guo, Lin

2014-01-01

In this paper, textured alumina ceramics were prepared from dehydroxylation of gibbsite films and the pseudomorphic and topotactic nature of the dehydroxylation of textured gibbsite films has been investigated. First, the precursor film with a (001)-textured structure was obtained via vacuum filtration deposition of diluted aqueous suspensions of gibbsite nanoplatelets. Subsequently, (001)-textured α-alumina ceramics were successfully achieved by sintering of the deposited gibbsite films without addition of α-alumina seeds. The Scanning Electron Microscope (SEM) and X-ray Diffraction (XRD) results show that, during the phase transition from gibbsite to α-alumina, both layered morphology and crystal's axis orientation have been retained to a considerable extent. For the first time, a direct XRD evidence of gibbsite topotactic dehydroxylation to the α-alumina phase is presented. It is believed that the method described here exploits gibbsite's pseudomorphic and topotactic dehydroxylation, not on individual particles scale but on a bulk form. The resulting structure can be considered as inorganic scaffolds which can have applications for fabrication of dense, textured alumina-based ceramics and other layered/textured nanocomposites. - Highlights: • Gibbsite nanoplatelets were assembled on their basal plane to form (001)-textured films. • Textured alumina ceramics were prepared by sintering textured gibbsite films without addition of α-alumina seeds. • Both pseudomorphic and topotactic aspects were exploited in bulk form instead of individual nanoparticulate size. • Direct XRD evidence of the topotactic dehydroxylation from gibbsite to α-alumina is presented in this work

Investigations of the uptake of transuranic radionuclides by humic and fulvic acids chemically immobilized on silica gel and their competitive release by complexing agents

International Nuclear Information System (INIS)

Bulman, R.A.; Szabo, G.; Clayton, R.F.; Clayton, C.R.

1998-01-01

The chemistry of the interactions of transuranic elements (TUs) with humic substances needs to be understood so that humate-mediated movement of transuranic radionuclides through the environment can be predicted. This paper reports the chemical immobilization on silica gel of humic and fulvic acids and evaluates the potential of these new materials for the retention of Pu and Am. In addition to the preparation of the foregoing immobilized humic substances, other low molecular weight metal-binding ligands have also been immobilized on silica gel to investigate the binding sites for transuranic elements (TUs) in humic substances. The X-ray photoelectron spectra (XPS) of Th(IV) complexed by humic acid and the immobilized humic acid are similar thus it appears that immobilization of humic acid does not generate any configurational changes in the Th(IV)-binding sites of the macromolecule. A variety of chelating agents partly mobilize these TUs sorbed on the solid phases. A batch method was used to determine the distribution coefficients (R d ) of Pu and Am between the silica gels and aqueous solutions of phosphate and citrate. The effects of the immobilized ligands, the anions and pH in the solution on sorption were assessed. Distributed coefficients (R d ) for the uptake of Pu and Am by these prepared solid phases are, in some cases, of a similar order of magnitude as those determined for soil and particles suspended in terrestrial surface waters

Bulk and interfacial stresses in suspensions of soft and hard colloids

International Nuclear Information System (INIS)

Truzzolillo, D; Roger, V; Dupas, C; Cipelletti, L; Mora, S

2015-01-01

We explore the influence of particle softness and internal structure on both the bulk and interfacial rheological properties of colloidal suspensions. We probe bulk stresses by conventional rheology, by measuring the flow curves, shear stress versus strain rate, for suspensions of soft, deformable microgel particles and suspensions of near hard-sphere-like silica particles. A similar behaviour is seen for both kinds of particles in suspensions at concentrations up to the random close packing volume fraction, in agreement with recent theoretical predictions for sub-micron colloids. Transient interfacial stresses are measured by analyzing the patterns formed by the interface between the suspensions and their solvent, due to a generalized Saffman–Taylor hydrodynamic instability. At odds with the bulk behaviour, we find that microgels and hard particle suspensions exhibit vastly different interfacial stress properties. We propose that this surprising behaviour results mainly from the difference in particle internal structure (polymeric network for microgels versus compact solid for the silica particles), rather than softness alone. (paper)

Synthesis and electron paramagnetic resonance study of a nitroxide free radical covalently bonded on aminopropyl-silica gel

International Nuclear Information System (INIS)

Tudose, Madalina; Constantinescu, Titus; Balaban, Alexandru T.; Ionita, Petre

2008-01-01

A solid spin-labeled material was obtained starting from 2-chloro-3,5-dinitro-N-(4-(2,2,6,6-tetramethyl-piperidine-1-oxyl) -benzamide) and aminopropyl-silica gel. Stability tests showed that even after several months the spin-labeled material had the same properties as immediately after synthesis. EPR properties of the TEMPO-derivatized silica were studied as a function of solvent polarity and temperature. Rotational correlation times were calculated from EPR spectra and correlated with solvent characteristics and temperature. Polar solvents induce a fast motion of the spin-label, clearly seen in the EPR spectra by the apparition of the well-known TEMPO radical triplet. The solid spin-labeled (dry) sample showed a high interspin interaction, which can be disrupted not only by different (liquid) solvents, but also by absorption of different solids, like cyclodextrins, dendrimers or polyethyleneglycols. Also, changes induced by the temperature were studied in the case of toluene wet sample. From 150 to 370 K, the spectrum is changing from a slow motion spectrum type to a fast motion regime. The preparative procedures to obtain the spin-labeled silica as well as some of its parameters are described

Synthesis and electron paramagnetic resonance study of a nitroxide free radical covalently bonded on aminopropyl-silica gel

Energy Technology Data Exchange (ETDEWEB)

Tudose, Madalina; Constantinescu, Titus [Institute of Physical Chemistry, Spl. Independentei 202, 060021 Bucharest (Romania); Balaban, Alexandru T. [Texas A and M University at Galveston, Marine Sciences Department, Galveston, TX 77551 (United States); Ionita, Petre [Institute of Physical Chemistry, Spl. Independentei 202, 060021 Bucharest (Romania)], E-mail: pionita@icf.ro

2008-01-30

A solid spin-labeled material was obtained starting from 2-chloro-3,5-dinitro-N-(4-(2,2,6,6-tetramethyl-piperidine-1-oxyl) -benzamide) and aminopropyl-silica gel. Stability tests showed that even after several months the spin-labeled material had the same properties as immediately after synthesis. EPR properties of the TEMPO-derivatized silica were studied as a function of solvent polarity and temperature. Rotational correlation times were calculated from EPR spectra and correlated with solvent characteristics and temperature. Polar solvents induce a fast motion of the spin-label, clearly seen in the EPR spectra by the apparition of the well-known TEMPO radical triplet. The solid spin-labeled (dry) sample showed a high interspin interaction, which can be disrupted not only by different (liquid) solvents, but also by absorption of different solids, like cyclodextrins, dendrimers or polyethyleneglycols. Also, changes induced by the temperature were studied in the case of toluene wet sample. From 150 to 370 K, the spectrum is changing from a slow motion spectrum type to a fast motion regime. The preparative procedures to obtain the spin-labeled silica as well as some of its parameters are described.

Synthesis and characterization of titanium oxide supported silica materials

Science.gov (United States)

Schrijnemakers, Koen

2002-01-01

Titania-silica materials are interesting materials for use in catalysis, both as a catalyst support as well as a catalyst itself. Titania-silica materials combine the excellent support and photocatalytic properties of titania with the high thermal and mechanical stability of silica. Moreover, the interaction of titania with silica leads to new active sites, such as acid and redox sites, that are not found on the single oxides. In this Ph.D. two recently developed deposition methods were studied and evaluated for their use to create titanium oxide supported silica materials, the Chemical Surface Coating (CSC) and the Molecular Designed Dispersion (MDD). These methods were applied to two structurally different silica supports, an amorphous silica gel and the highly ordered MCM-48. Both methods are based on the specific interaction between a titanium source and the functional groups on the silica surface. With the CSC method high amounts of titanium can be obtained. However, clustering of the titania phase is observed in most cases. The MDD method allows much lower titanium amounts to be deposited without the formation of crystallites. Only at the highest Ti loading very small crystallites are formed after calcination. MCM-48 and silica gel are both pure SiO2 materials and therefore chemically similar to each other. However, they possess a different morphology and are synthesized in a different way. As such, some authors have reported that the MCM-48 surface would be more reactive than the surface of silica gel. In our experiments however no differences could be observed that confirmed this hypothesis. In the CSC method, the same reactions were observed and similar amounts of Ti and Cl were deposited. In the case of the MDD method, no difference in the reaction mechanism was observed. However, due to the lower thermal and hydrothermal stability of the MCM-48 structure compared to silica gel, partial incorporation of Ti atoms in the pore walls of MCM-48 took place

Development of a bi-functional silica monolith for electro-osmotic pumping and DNA clean-up/extraction using gel-supported reagents in a microfluidic device.

Science.gov (United States)

Oakley, Jennifer A; Shaw, Kirsty J; Docker, Peter T; Dyer, Charlotte E; Greenman, John; Greenway, Gillian M; Haswell, Stephen J

2009-06-07

A silica monolith used to support both electro-osmotic pumping (EOP) and the extraction/elution of DNA coupled with gel-supported reagents is described. The benefits of the combined EOP extraction/elution system were illustrated by combining DNA extraction and gene amplification using the polymerase chain reaction (PCR) process. All the reagents necessary for both processes were supported within pre-loaded gels that allow the reagents to be stored at 4 degrees C for up to four weeks in the microfluidic device. When carrying out an analysis the crude sample only needed to be hydrodynamically introduced into the device which was connected to an external computer controlled power supply via platinum wire electrodes. DNA was extracted with 65% efficiency after loading lysed cells onto a silica monolith. Ethanol contained within an agarose gel matrix was then used to wash unwanted debris away from the sample by EOP (100 V cm(-1) for 5 min). The retained DNA was subsequently eluted from the monolith by water contained in a second agarose gel, again by EOP using an electric field of 100 V cm(-1) for 5 min, and transferred into the PCR reagent containing gel. The eluted DNA in solution was successfully amplified by PCR, confirming that the concept of a complete self-contained microfluidic device could be realised for DNA sample clean up and amplification, using a simple pumping and on-chip reagent storage methodology.

Extraction of Alumina from Red Mud for Synthesis of Mesoporous Alumina by Adding CTABr as Mesoporous Directing Agent

Directory of Open Access Journals (Sweden)

Eka Putra Ramdhani

2018-05-01

Full Text Available Mines in Bintan were producing bauxite for many years. The production process of bauxite to alumina produced much red mud. From X-ray Fluorescence (XRF, alumina content on Bintan’s red mud was 28.87 wt.%. This research was studying on the extraction alumina from red mud with reduction of hematite (Fe2O3 and desilication processes. After extraction process alumina was collected about 52.89 wt.%. Synthesis of mesoporous alumina from red mud using sol-gel method at the room temperature for 72 h with cetyltrimethylammonium bromide (CTABr as mesoporous directing agent. The CTABr/Al-salt ratio, i.e. 1.57; 4.71 and 7.85 with the sample code of AMC-1, AMC-3, AMC-5, respectively. The product was calcined at 550 °C for 6 h. The synthesized materials were characterized by X-ray Diffraction (XRD, scanning electron microscopy-energy dispersive X-ray (SEM-EDX, transmission electron microscopy (TEM, and N2 adsorption-desorption techniques. XRD pattern of AMC-1, AMC-3, and AMC-5 showed that all synthesized materials have amorphous phase. The morphology were wormhole aggregate that were showed by SEM and TEM characterization. N2 adsorption-desorption characterization showed the distribution of pore size of about 3.2 nm. The highest surface area and pore volume were obtained in solid-solid ratio CTABr/GM-AL by 1.57 (AMC-1 i.e. 241 m2/g and 0.107 cm3/g, respectively.

Study of Physical Properties of Nano-Silica Coated Cotton Textiles

OpenAIRE

Sidra Saleemi; Farooq Ahmed; Samandar Malik

2015-01-01

This research was aimed to investigate the effect of silica sol-gel coating on air permeability, stiffness and tensile properties of dyed cotton fabric. Various concentrations of silica nanoparticles were applied on dyed cotton substrate using two different cross-linkers through sol-gel method. The homogenous sol-gel coating dispersions were prepared by using an ultrasonicator. Coated samples were tested for mechanical and comfort properties such as tensile strength, stiffness, crease recover...

Determination of Copper in Different Ethanolic Matrices Using a Chloropropyl Silica Gel Modified with a Nanostructured Cubic Octa(3-aminopropyloctasilsesquioxane