• Title/Summary/Keyword: monolithic column

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Preparation and Characterization of Monolithic Poly(methacrylic acid - ethylene glycol dimethacrylate) Columns for High Performance Liquid Chromatography

  • Yan, Hong-yuan;Row, Kyung-Ho
    • Bulletin of the Korean Chemical Society
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    • v.27 no.1
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    • pp.71-76
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    • 2006
  • Porous polymer monolithic columns were prepared by the direct free radical copolymerization of methacrylic acid and ethylene glycol dimethacrylate within the confines of a chromatographic column in the presence of toluene-dodecanol as a porogenic solvent. The separation characteristics of the monolithic columns were tested by a homologous series of xanthine derivatives, theophylline and caffeine. The effects of the polymerization mixture composition and polymerization condition, mobile phase composition, flow rate and temperature on the retention times and separation efficiencies were investigated. The results showed that the selection of correct porogenic solvents and appropriate polymerization conditions are crucial for the preparation of the monolithic stationary phases. The separation efficiency was only extremely weakly dependent on flow rate and temperatures. Hydrogen-bonding interaction played an important role in the retention and separation. Compared with conventional particle columns, the monolithic column exhibited good stability, ease of regeneration, high separation efficiency and fast analysis.

Interface treatment in shotcrete jacketing of reinforced concrete columns to improve seismic performance

  • Vandoros, Konstantinos G.;Dritsos, Stephanos E.
    • Structural Engineering and Mechanics
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    • v.23 no.1
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    • pp.43-61
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    • 2006
  • An investigation of the effectiveness of the interface treatment when column concrete jacketing is performed is presented. Alternative methods of interface connection were used in order to investigate the performance of strengthened concrete columns. These connecting techniques involved roughening the surface of the original column, embedding steel dowels into the original column and a combination of these two techniques. The experimental program included three strengthened specimens, one original specimen (unstrengthened) and one as-built specimen (monolithic). The specimens represented half height full-scale old Greek Code (1950's) designed ground floor columns of a typical concrete frame building. The jackets of the strengthened specimens were constructed with shotcrete. All specimens were subjected to displacement controlled earthquake simulation loading. The seismic performance of the strengthened specimens is compared to both the original and the monolithic specimens. The comparison was performed in terms of strength, stiffness and hysteretic response. The results demonstrate the effectiveness of the strengthening methods and indicate that the proper construction of a jacket can improve the behaviour of the specimens up to a level comparable to monolithic behaviour. It was found that different methods of interface treatment could influence the failure mechanism and the crack patterns of the specimens. It was also found that the specimen that combined roughening with dowel placement performed the best and all strengthened columns were better at dissipating energy than the monolithic specimen.

Separation of Caffeine and Tryptophan Using Molded Macroporous Poly(glycidyl methacrylate-co-ethylene glycol dimethacrylate) Rods (주조된 매크로 다공성 Poly(glycidyl methacrylate-co-ethylene glycol dimethacrylate) 막대를 이용한 카페인과 트립토판의 분리)

  • Jin, Longmei;Yan, Hongyuan;Row, Kyung Ho
    • Korean Chemical Engineering Research
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    • v.43 no.5
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    • pp.603-608
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    • 2005
  • The molded macroporous poly (glycidyl methacrylate-co-ethylene glycol dimethacrylate) rods produced by a facile molding process were polymerized in situ within a tubular mold, chromatographic column ($4.6{\times}100mm$) by free radical polymerization. It was complemented by epoxy derivatized monolithic column and chemical modification of the epoxide groups with the sulphuric acid. By variation of the polymerization conditions, such as the ratio of the monomers, the porogen (pore generating material), and the temperature, the pore size could be varied, so the retention time of the samples may be adjusted. For the mixture of caffeine and tryptophan in the prepared monolithic column, the influences of polymerization material compositions to the efficiency, selectivity, and resolution of the monolithic column were investigated.

High Speed Separation of PFCs in Human Serum by C18-Monolithic Column Liquid Chromatography-Tandem Mass Spectrometry

  • Lee, Won-Woong;Lee, Sun-Young;Yu, Se Mi;Hong, Jongki
    • Bulletin of the Korean Chemical Society
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    • v.33 no.11
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    • pp.3727-3734
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    • 2012
  • An analytical method has been developed for the rapid determination of perfluorinated compounds (PFCs) in human serum samples. The extraction and purification of PFCs from human serum were performed by the modified method of previous report. Ten PFCs were rapidly separated within 3.3 min by C18-monolithic column liquid chromatography (LC) and detected by electrospray ionization (ESI) tandem mass spectrometry (MS/MS) in negative ion mode. The runtime of PFCs on monolithic column LC was up to 4-fold faster than that on conventional column LC. The effect of triethylamine (TEA) to the mobile phase has investigated on the overall MS detection sensitivity of PFCs in ESI ionization. Quantification was performed by LC-MS/MS in multiple-ion reaction monitoring (MRM) mode, using $^{13}C$-labeled internal standards. Method validation was performed to determine recovery, linearity, precision, and limits of quantification, followed by, the analysis of a standard reference material (SRM 1957 from NIST). The overall recoveries ranged between 81.5 and 106.3% with RSDs of 3.4 to 16.2% for the entire procedure. The calibration range extended from 0.33 to 50 $ng\;mL^{-1}$, with a correlation coefficient ($R^2$) greater than 0.995 and the limits of quantification with 0.08 to 0.46 $ng\;mL^{-1}$. This approach can be used for rapid and sensitive quantitative analysis of 10 PFCs in human serum with high performance and accuracy.

Enhancement of Analytical Method for Phenolic Compounds in Mainstream Cigarette Smoke Using High Efficiency Column and RRLC system (고효율 컬럼과 RRLC를 이용한 담배 주류연 중 페놀 화합물의 분석 효율화)

  • Min, Hye-Jeong;Kang, Young-Hee;Lee, Jeong-Min;Jang, Gi-Chul
    • Journal of the Korean Society of Tobacco Science
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    • v.32 no.1
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    • pp.35-40
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    • 2010
  • This study was carried out to enhance the analytical methods of phenolic compounds in mainstream cigarette smoke using high efficiency column and RRLC(Rapid Resolution Liquid Chromatography) system, and to compare these methods. RRLC system offers significantly faster results with higher data quality of phenolic compounds than conventional HPLC, but it is disadvantage that it is expensive. On the other hand, the method using monolithic column offers faster results by the use of conventional HPLC system without new equipment introduction. In this study, we used the linear type smoking machine and Health Canada method for pre-treatment process of phenolic compounds. The analysis time of phenolic compounds using RRLC and monolithic column was individually 8 and 15 minutes, whereas in the conventional HPLC it was 45 minutes. These new methods were accompanied with the minimal solvent consumption and had lower analysis costs. Also, we proved that there were no difference between new methods and conventional method in accuracy by statistic.

Performance of Precast Concrete Beam-Column Connections Subjected to Cyclic Loading (반복하중을 받는 프리캐스트 콘크리트 보-기둥 접합부의 거동 연구)

  • Kim, Kyu-Rhee;Park, Hong-Gun
    • Proceedings of the Korea Concrete Institute Conference
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    • 2004.11a
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    • pp.619-622
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    • 2004
  • In this study, a moment resisting precast concrete beam-column connection is proposed. An experimental study was carried out to investigate the connection behavior subjected to cyclic loading. Three precast beam-column interior connections and one monolithic connection were tested. Variable included the detailing used at the joint to achieve structural constructability and the location of mild steel reinforcement and high strength bar. During specimen fabrication, the joint details enables ease and speed of construction. Connection performance is evaluated on the basis of ductility, energy dissipation capacity, connection strength, and drift capacity. Based on test results, the precast concrete beam-column connection is capable of matching or exceeding the performance of the monolithic connection.

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A Study on the Energy Dissipation Capacity of Precast Concrete Beam-Column Connection using DDC (DDC를 활용한 건식 보-기둥 모멘트 접합부의 내진 성능에 관한 연구)

  • Hong, Sung-Gul;Lee, Sang-Jin
    • Proceedings of the Korea Concrete Institute Conference
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    • 2004.11a
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    • pp.85-88
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    • 2004
  • In this study, a simple moment-resisting precast concrete beam-column connection is proposed for highly seismic zone using dywidag ductile rod [DDC]. DDC is superior system for ductility, energy dissipation capacity, connection strength, and drift capacity. A study was carried out to investigate the connection behavior subjected to cyclic inelastic loading. Four Precast beam-column interior connections and one monolithic connection will be tested. The variables will be examined were the strength relationship between joint's ductile rod and beam reinforcement for gain energy dissipation capacity. The specimens will be tested only reverse cyclic loading in accordance with a prescribed displacement history. Connection performance is evaluated on the basis of ductility, energy dissipation capacity, connection strength, and drift capacity. the precast connection using DDC is capable of matching of exceeding the performance of the monolithic connection and thereby provides moment-resisting behavior.

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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.

Retention Mechanism of Caffeine and Tryptophan in Macroporous Poly[Methacrylic Acid-co-Ethylene Glycol Dimenthacrylate] Rods (매크로 다공성 Poly[Methacrylic Acid-co-Ethylene Glycol Dimenthacrylate] 막대에서 Caffeine과 Tryptophan의 체류 메카니즘)

  • Jin, Longmei;Yan, Hongyuan;Zheng, Jinzhu;Row, Kyung-Ho
    • KSBB Journal
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    • v.21 no.5
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    • pp.401-404
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    • 2006
  • Macroporous Poly(Methacrylic acid-co-Ethylene Glycol Dimethacrylate) Rods were in situ thermal initialized within a empty column($3.9{\times}150mm$) by free radical polymerization. The polymerization mixture was consisted of monomer, cross-linking monomer, porogenic solvent, initiator and control the ratio of these materials, column efficiency could be developed. Caffeine and tryptophan as separation substances and the retention mechanism of this kind of monolithic column was mainly hydrogen bond function.

A Novel Method to Fabricate Tough Cylindrical Ti2AlC/Graphite Layered Composite with Improved Deformation Capacity

  • Li, Aijun;Chen, Lin;Zhou, Yanchun
    • Journal of the Korean Ceramic Society
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    • v.49 no.4
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    • pp.369-374
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    • 2012
  • Based on the structure feature of a tree, a cylindrical $Ti_2AlC$/graphite layered composite has been fabricated through heat treating a graphite column and six close-matched thin wall $Ti_2AlC$ cylinders bonded with the $Ti_2AlC$ powders at $1300^{\circ}C$ and low oxygen partial pressure. SEM examination reveals that the bond interlayers between cylinders or that between cylinder and column are not fully dense without any crack formation. During the compressive test, the strain of the $Ti_2AlC$/graphite layered composite is about twice higher than that of the monolithic $Ti_2AlC$ ceramic, and the compressive strength of the layered composite is 348 MPa. The layered composite show the noncatastrophic fracture behaviors due to the debonding and shelling off of the layers, which are different from the monolithic $Ti_2AlC$ ceramic. The mechanism of the improved deformation capacity and noncatastrophic failure modes are attributed to the presence of the central soft graphite column and cracks deflection by the bond interlayers.