• Title/Summary/Keyword: Double end-capping

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Preparation of Cucurbituril Anchored Silica Gel by Cross Polymerization and Its Chromatographic Applications

  • Cheong, Won-Jo;Go, Joung-Ho;Baik, Yoon-Suk;Kim, Sung-Soon;Nagarajan, Erumaipatty R;Selvapalam, Narayanan;Ko, Young-Ho;Kim, Ki-Moon
    • Bulletin of the Korean Chemical Society
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    • v.29 no.10
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    • pp.1941-1945
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    • 2008
  • A new chromatographic stationary phase has been prepared by cross polymerization between allylsilica and perallyloxycucurbit[6]uril and characterized by elemental analysis and FT-IR spectroscopy. The double endcapping has been proven to improve the separation efficiency of the cucurbituril-based stationary phase material. The first end-capping was carried out when allylsilica was made. The second end-capping was done as the final step of the whole process, and the use of a mixture of hexamethyldisilazane (HMDS) and trimethylchlorosilane (TMCS) as an end-capping reagent was found better than the use of only HMDS or TMCS. Our stationary phase has shown generally good results in separation of nonpolar and polar analytes. This phase showed even better separation performance than the commercial C18 phase for the case where hostguest chemistry was properly incorporated in solute retention.

The Synthesis and Characterization of (TBMA)Macromer Grafted Anionic Acrylic Copolymer ((TBMA)Macromer를 그라프트시킨 음이온성 아크릴 공중합체의 합성과 물성)

  • Kim, Hyoung-Ook;Noh, Si-Tae;Kang, Shin-Chun
    • Applied Chemistry for Engineering
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    • v.4 no.3
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    • pp.627-636
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    • 1993
  • Anionic acrylic resin utilizing macromer(TBMA-g-MMA) copolymer was synthesized by preparing (TBMA) macromer using anionic living polymerization, followed by graft copolymerization with MMA macromer. To control the anionic site content in graft copolymer, the relative composition((TBMA) macromer/MMA ratio) of the graft copolymer was controlled at 7/3, 10/90, 15/85, 20/80, 30/70, 40/60, 50/50 in weight content. In the course of anionic living polymerization of(TBMA) macromer, broad molecular weight distribution (1.4~1.5) was obtained by using n-butyllithium-diphenyethylene initiatior system at $-78^{\circ}C$. To introduce the double bond at the end of chain in termination step, methacryloyl chloride was reacted after insertion of benzaldehyde as capping material. Moreover, TBMA parts in graft copolymer were hydrolyzed in the presence of p-toluenesulfonic acid catalyst, and neutralization of graft copolymer with triethylamine was granted acrylic resin to anionic site. Molecular weight and molecular weight distribution of(TBMA) macromer were determined by GPC, and the hydrolysis of TBMA with neutralization of acrylic resin were determined by IR and NMR. From water dispersion and stability point of view, stable dispersion state appeared at low molecular weight(TBMA) macromer with a small TBMA content as a result of scrutiny about the relation to TBMA content and branch length for(TBMA) macromer molecular weight in graft copolymer.

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