• Title/Summary/Keyword: silica monolith

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A New Stationary Phase Prepared from Ground Silica Monolith Particles by Reversible Addition-Fragmentation Chain Transfer Polymerization

  • Lee, Seung-Mi;Zaidi, Shabi Abbas;Cheong, Won-Jo
    • Bulletin of the Korean Chemical Society
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    • v.31 no.10
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    • pp.2943-2948
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    • 2010
  • Silica monolith powders were prepared by a new procedure where ground powders of proper size distribution were obtained without sieving. An initiator was attached to this ground monolith and polystyrene was bound by reversible addition-fragmentation chain transfer polymerization to give a new stationary phase. The separation efficiency of this phase was found better than that of the polystyrene bound phase based on conventional silica particles and that of the C18 bound silica monolith powders.

Porous Silica Particles As Chromatographic Separation Media: A Review

  • Cheong, Won Jo
    • Bulletin of the Korean Chemical Society
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    • v.35 no.12
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    • pp.3465-3474
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    • 2014
  • Porous silica particles are the most prevailing raw material for stationary phases of liquid chromatography. During a long period of time, various methodologies for production of porous silica particles have been proposed, such as crashing and sieving of xerogel, traditional dry or wet process preparation of conventional spherical particles, preparation of hierarchical mesoporous particles by template-mediated pore formation, repeated formation of a thin layer of porous silica upon nonporous silica core (core-shell particles), and formation of specific silica monolith followed by grinding and calcination. Recent developments and applications of useful porous silica particles will be covered in this review. Discussion on sub-$3{\mu}m$ silica particles including nonporous silica particles, carbon or metal oxide clad silica particles, and molecularly imprinted silica particles, will also be included. Next, the individual preparation methods and their feasibilities will be collectively and critically compared and evaluated, being followed by conclusive remarks and future perspectives.

Preparation of Silica Monoliths with Macropores and Mesopores and of High Specific Surface Area with Low Shrinkage using a Template Induced Method

  • Guo, Jianyu;Lu, Yan;Whiting, Roger
    • Bulletin of the Korean Chemical Society
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    • v.34 no.2
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    • pp.447-452
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    • 2013
  • In this study we report a new method for the synthesis of a silica monolithic column bed with bimodal pores (throughpores and mesopores). The template induced synthesis method was used to direct bimodal pores simultaneously instead of the usual post base-treating method. Block polymer Pluronic F127 was chosen as a dual-function template to form hierarchically porous silica monolith with both macropores and mesopores. This is a simplification of the method of monolithic column preparation. Poly(ethylene glycol) was used as a partial substitute for F127 can effectively prevent shrinkage during the monolith aging process without losing much surface area (944 $m^2/g$ to 807 $m^2/g$). More importantly, the resultant material showed a much narrower mesopore size (centered at 6 nm) distribution than that made using only F127 as the template reagent, which helps the mass transfer process. The solvent washing method was used to remove the remaining organic template, and it was proved to be effective enough. The new synthesis method makes the fabrication of the silica monolithic column (especially capillary column) much easier. All the structure parameters indicate that monolith PFA05 prepared by the above method is a good material for separation, with the merits of much higher surface area than usual commercial HPLC silica particles, suitable mesopore volume, narrow mesopore size distribution, low shrinkage and it is easily prepared.

Synthesis of Silica Aerogel at Ambient Pressure and Characterization (II) (실리카 에어로겔의 상압합성 및 특성연구(II))

  • 권영근;최세영;강신규
    • Journal of the Korean Ceramic Society
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    • v.36 no.11
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    • pp.1189-1197
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    • 1999
  • Low-density silica gel monolith was synthesized at ambient pressure by surface modification with TMCS and sub-sequent heat treatment. The mechanical thermal and optical properties of gel were studied. Compressive strength and modulus of compression of 350$^{\circ}C$-heated gel with the density of 0.24g/cm3 were 250kPa and 0.2MPa respectively. The thermal conductivity of silica gels synthesized at ambient pressure exhibited 0.02 W/m$.$K for the density of 0.24g/cm3 which is similar to that of the gel via supercritical drying and their main thermal transfer mechanism is considered to be solid and radiation conduction at room temperature. Ambient-dried silica gels were transparent blue showing about 60% of transmittance in the wavelength of 1500-2100nm and typical absorption bands of existing bonds under heat treatment at 350$^{\circ}C$. Medium scale monolity(${\Phi}$=50mm) at ambient pressure could be successfully prepared through total 5-month process period.

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Preparation and characterization of nanoporous monolith with high thermal insulation performance (나노 기공성 단열 실리카 모노리스 제조 및 특성 연구)

  • Choi, Hyun-Muk;Kim, Seong-Woo
    • Journal of the Korean Applied Science and Technology
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    • v.31 no.1
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    • pp.83-91
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    • 2014
  • In this study, we synthesized two different silica monoliths by using sol-gel, solvent exchange, surface modification, ambient pressure drying processes, and surfactant-based templating technique followed by calcination process. All of the prepared two silica monoliths showed crack-free appearance with fairly good transparency, and furthermore were confirmed to have extremely high porosity, specific surface area, and mean pore size below 30 nm. The silica aerogel sample exhibited finer and more homogeneous nano-sized pore structure due to spring back effect caused by surface modification, which resulted in better thermal insulation performance. Based on measured thermal conductivities and theoretical relationship, multi-layered glass window system in which silica monolith prepared in this study was inserted as a middle layer was revealed to have superior thermal insulation performance compared to conventional air-inserted glass window system.

A Study on the Oxidation of CO and $C_3H_6$ over Noble Metal Supported Catalysts on Monolith (Monolith에 담지한 귀금속촉매상에서 CO와 $C_3H_6$의 동시적 산화반응에 관한 연구)

  • 김태원;고형림;김재형;김경림
    • Journal of Korean Society for Atmospheric Environment
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    • v.14 no.1
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    • pp.63-72
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    • 1998
  • Simultaneous CO and $C_3H_6$ oxidation was carried out over noble metal supported monolith catalysts in a flow thorugh type reactor at the temperature ranging from room temperature to $500^\circ$C. Pt and Pd were selected as major active species, 10wt% of Ce was impregnated as an additive and alumina and silica were used as supports. The reactant gases were simulated and the reaction products were analyzed by on-line G.C.. EDX, SEM, TGA, XRD and optical microscope were used to analyze the characteristics of the prepared catalysts. Under the given conditions in this study, the catalysts supported on alumina showed better activity for CO oxidation, while Pd catalysts showed better activity for $C_3H_6$ oxidation. The improvement of conversion due to increase in thermal stability possibily by Ce addition was observed only for Pt catalysts.

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Capillary Electrochromatography with Liquid Crystal Crown Ether Modified Hybrid Silica Monolith for Analysis of Imidacloprid and Carbendazim in Tomatoes

  • Wang, Mingming;Feng, Rui;Shen, Jing;Chen, Hao;Zeng, Zhaorui
    • Bulletin of the Korean Chemical Society
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    • v.33 no.7
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    • pp.2224-2228
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    • 2012
  • This study describes the ability of capillary electrochromatography (CEC) for the determination of imidacloprid and carbendazim in tomato samples. A novel liquid crystal crown ether modified hybrid silica monolithic column was synthesized, characterized and developed as separation column for the first time. Baseline separation of imidacloprid and carbendazim could be achieved using a mobile phase containing 90% (v/v) 20 mmol/L phosphate buffer (pH 7.0) and 10% (v/v) acetonitrile. The matrix matched calibration curves were linear with correlation coefficient $r^2$ > 0.9998 in the range of 0.20-10.00 mg/L. The limits of detection for imidacloprid and carbendazim were 0.061 and 0.15 mg/kg, respectively, which were below the maximum residue limits established by the European Union as well as Codex Alimentarius. Average recoveries for imidacloprid and carbendazim varied from 101.6-108.0% with relative standard deviations lower than 6.3%. This method was applied to the analysis of tomatoes collected from local markets.