• Analytical Science and Technology
• /
• v.17 no.6
• /
• pp.532-535
• /
• 2004

A method on the determination of Co(II) after adsorbing of Co(II) on 2-mercaptobenzothiazole-loaded silica gel was studied. The conditions on the separation of Co(II) such as pH of solution, the amount of 2-mercaptobenzothiazole, the flow rate for adsorption, and the desorption solvent were optimized to 9.0, 0.05 g, $10mL\;min^{-1}$ and 1 M $HNO_3$ in ethanol, respectively. Under these optimum conditions, the calibration curve of Co(II) was obtained over concentration range of $2{\sim}120ng\;mL^{-1}$. The detection limit was $0.6ng\;mL^{-1}$. Recovery yields of Co(II) in various natural water samples were more than 90%.

• Bulletin of the Korean Chemical Society
• /
• v.30 no.7
• /
• pp.1516-1520
• /
• 2009

A sensitive technique for the determination of trace Co(II) in various samples after column preconcentration by adsorbing onto silica gel loaded with 1-nitroso-2-naphthol was developed. Several experimental conditions, such as pH of sample solution, the amount of silica gel loaded with 1-nitroso-2-naphthol, the flow rate for adsorption and so forth, were optimized. The interfering effects of diverse concomitant ions were investigated. Fe(III) interfered with more than any other ions, but the interference by Fe(III) was completely eliminated by adjusting the amount of silica gel loaded with 1-nitroso-2-naphthol to 0.30 g. The dynamic range, the correlation coefficient ($R^2$), and the detection limit obtained by the proposed technique were 3.0-140.0 ng m$L^{-1}$, 0.9942, and 1.81 ng m$L^{-1}$, respectively. For validating the technique, the aqueous samples (tap water, reservoir water, stream water, and wastewater) and the plastic samples were used as real samples. Recovery yields of 93.0-107.0% were obtained. These measured data were not different from ICP-MS data at the 95% confidence level by F test. Based on the results of the experiment, it has been found that the proposed technique can be applied to the determination of Co(II) in various real samples.

• Membrane Journal
• /
• v.16 no.2
• /
• pp.123-132
• /
• 2006

The PTMSP-silica-PEI composite membranes were synthesized from tetraethoxysilane (TEOS) and poly (1-trimethylsilyl-1-propyne) (PTMSP) by sol-gel process. The PTMSP-silica nanocomposite membranes were characterized by $^1H-NMR$, FT-IR, TGA, XPS, SEM, GPC and gas permeation measurements were accomplished with $H_2,\;O_2,\;N_2,\;CO_2,\;CH_4$. The gases permeability increased with increasing TEOS content. Both the permeability and selectivity of $H_2,\;CH_4$ increased to 15 wt% TEOS. While the permeability of $O_2,\;CO_2$ increased without decrease of selectivity.

• Bulletin of the Korean Chemical Society
• /
• v.32 no.10
• /
• pp.3644-3649
• /
• 2011

Multinuclear solid-state nuclear magnetic resonance (NMR) experiments were performed to investigate the local structure changes of nanoporous silica during hydrothermal treatment and surface modification with 3-aminopropyltriethoxysilane (3-APTES). The nanoporous silica was prepared by sol-gel polymerization using inexpensive sodium silicate as a silica precursor. Using $^1H$ magic angle spinning (MAS) NMR spectra, the hydroxyl groups, which play an important role in surface reactions, were probed. Various silicon sites such as $Q^2$, $Q^3$, $Q^4$, $T^2$, and $T^3$ were identified with $^{29}Si$ cross polarization (CP) MAS NMR spectra and quantified with $^{29}Si$ MAS NMR spectra. The results indicated that about 25% of the silica surface was modified. $^1H$ and $^{29}Si$ NMR data proved that the hydrothermal treatment induced dehydration and dehyroxylation. The $^{13}C$ CP MAS and $^1H$ MAS NMR spectra of 3-APTES attached on the surface of nanoporous silica revealed that the amines of the 3-aminopropyl groups were in the chemical state of ${NH_3}^+$ rather than $NH_2$.

• Membrane Journal
• /
• v.11 no.3
• /
• pp.116-123
• /
• 2001

Polyimide-silica hybrid membranes were prepared and the effect of silica content on the structural properties and the gas transport properties was studied. The hybrid membranes were obtained by the sol-gel process starting from 1,2,4,5-benzenetetracarboxylic dianhydride(PMDA), 4,4`-diamino- diphenyl oxide(ODA) and tetraethoxysilane(TEOS) in N,N` dimethylacetatmide (DMAc) solvent. The structural characterizations of the membrane were performed by FT-IR, EDX, TGA and SEM. The gas permeation experiments with ${N_2}, {O_2}, {H_2}, {CO_2}and ${CH_4}$ were carried out at the temperature of $25^{\circ}C$ and in the range of pressure from 3atm to 7atm. the hybrid membranes showed higher thermal stability than PI membranes. The silica patricles were uniformly embedded in the polyimide matrix and the size of silica particles increased with increasing silica content. The permeability coefficients of ${N_2}, {O_2}, {H_2}, {CO_2}and ${CH_4}$ increased with increasing silica content but the diffusion coefficients might appear to be a result of a solubility enhancement. In spite of the permeability enhancement, an increase in the selectivities of ${H_2}/{N_2}, ${H_2}/{O_2} and ${H_2}/{CO_2} was observed.

• Clean Technology
• /
• v.15 no.4
• /
• pp.258-264
• /
• 2009

Thermodynamic measurements were performed to show the possibility of recovering $CO_2$ from fuel gas (the mixture of $CO_2$ and $H_2$) by forming gas hydrates with water where water was dispersed in the pores of silica gel particles having nominal 100 nm of pore diameter. The hydrate-phase equilibria for the ternary $CO_2+H_2$+water in pores were measured and $CO_2$ concentrations in vapor and hydrate phase were determined under the hydrate-vapor two phase region at constant 274.15 K. It was shown that the inhibition effect appeared due to silica gel pores, and the corresponding equilibrium dissociation pressures became higher than those of bulk water hydrates at a specific temperature. In addition, direct measurement of $CO_2$ content in the hydrate phase showed that the retrieved gas from the dissociation of hydrate contained more than 95 mol% of $CO_2$ when 42 mol% of $CO_2$ and balanced Hz mixture was applied. Compared with data obtained in case of bulk water hydrates, which showed just 83 mol% of $CO_2$ where 2-stage hydrate slurry reactor was intended to utilize this property, the hydrate formation in porous silica gel has enhanced the feasibility of $CO_2$ separation process. Hydrate formation as not for slurry but solid particle makes it possible to used fixed bed reactor, and can be a merit of well-understood technologies in the industrial field.

• Membrane Journal
• /
• v.18 no.2
• /
• pp.146-156
• /
• 2008

In this study, PTMSP of high permeability and high molecular weight was synthesized, and PTMSP-PDMS graft copolymer was synthesized from poly [1-(trimethylsily)propyne] (PTMSP) and hydroxy-terminated poly(dimethylsiloxane) (PDMS). The PTMSP-PDMS-silica composites were prepared by the addition of 15, 30, or 50 wt% tetraethoxysilane (TEOS) to PTMSP-PDMS graft copolymer by sol-gel process. To investigate the physico-chemical characteristics of PTMSP-PDMS-silica/PEI composite membranes, the analytical methods such as $^1H$-NMR, FT-IR, TGA, XPS, GPC, and SEM have been utilized. The gas permeability and selectivity properties of $H_2,\;O_2,\;N_2,\;CO_2,\;CH_4,\;n-C_4H_{10}$, were evaluated. Permeability of the composite membranes increased as TEOS content and pressure increased. Selectivity of $H_2,\;O_2,\;N_2,\;CO_2,\;CH_4,\;and\;n-C_4H_{10}$, showed the maximum value at 30 wt% of TEOS content and decreased thereafter.

• Applied Biological Chemistry
• /
• v.50 no.4
• /
• pp.348-351
• /
• 2007

The stem barks of Fraxinus rhynchophylla was extracted with 95% EtOH, and the concentrated extract was successively partitioned with $CH_2Cl_2$, n-BuOH, and $H_2O$ in order to investigate the major phytochemicals. From the $CH_2Cl_2$ soluble fraction, a sterol (1) was isolated through the repeated silica gel column chromatographies. Three additional compounds (2-4) were isolated from the n-BuOH soluble fraction through silica gel, RP-18, and Sephadex LH-20 column chromatographies. Their chemical structures were elucidated as daucosterol $(1;{\beta}-sitosterol-3-O-{\beta}-D-glucopyranoside)$, caffeic acid (2), 6,8-dihydroxy-7-methoxycoumarin (3), and coniferaldehyde glucoside (4) by comparing their spectral data with those in the literatures. All isolates (1-4) were the first to be isolated from F. rhynchophylla.

• Applied Chemistry for Engineering
• /
• v.30 no.1
• /
• pp.68-73
• /
• 2019

We prepared hydrophobic silica particles by a sol-gel process from tetraethyl orthosilicate (TEOS), followed by coupling the reaction with octyltrimethoxysilane (OTMS) or hexadecyltrimethoxysilane (HDTMS) under various reaction conditions. We confirmed the extent of silica surface modification with organic compounds by SEM-EDS, thermogravimetry and elemental analysis. The silica particles obtained after the hydrolysis reaction of TEOS in ethanol at $50^{\circ}C$ for 24 h and the coupling reaction with OTMS for 2 h at the same temperature displayed the optimum performance in terms of the dispersity in an organic solvent and the surface roughness of films composited with epoxy resins. The oxygen permeability of the composite film with modified-silica was 12% lower than that of using the film without modified-silica.

• New & Renewable Energy
• /
• v.3 no.2 s.10
• /
• pp.47-52
• /
• 2007

Hydrate phase equilibrium for the binary $CO_{2}$+water and $CH_{4}$+water mixtures in silica gel pore of nominal 6, 30, and 100 nm were measured and compared with the cacluated results based on van der Waals and Platteeuw model. At a specific temperature three-phase hydrate-water-vapor (HLV) equilibrium curves for pore hydrates were shifted to the higher-pressure condition depending on pore sizes when compared with those of bulk hydrates. Notably, hydrate phase equilibria for the case of 100 nominal nm pore size were nearly identical with those of bulk hydrates. The activities of water in porous silica gels were modified to account for capillary effect, and the calculation results were generally in good agreement with the experimental data.