Self-immobilization and/or thermal treatment for preparing silica-poly(methyloctylsiloxane) stationary phases

被引:16
作者
Bottoli, CBG
Vigna, CRM
Fischer, G
Albert, K
Collins, KE
Collins, CH
机构
[1] Univ Estadual Campinas, Inst Quim, LABCROM Lab Pesquisas & Cromatog Liquida, BR-13087971 Campinas, SP, Brazil
[2] Univ Tubingen, Inst Organ Chem, D-72076 Tubingen, Germany
关键词
stationary phases; LC; silica-poly(methyloctylsiloxane) stationary phases; polysiloxane;
D O I
10.1016/j.chroma.2003.08.107
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
Batches of poly(methyloctylsiloxane) (PMOS)-loaded silica were prepared by the deposition of PMOS, into the pores of HPLC silica. Portions of PMOS-loaded silica were allowed to remain at ambient temperature, without further treatment for 2, 9, 20, 31, 51, 105 and 184 days after preparation to undergo self-immobilization (irreversible adsorption of a layer of polymer on silica at ambient temperature in the absence of initiators). Other portions were subjected to a thermal treatment (100degreesC for 4h) after 1, 2, 5, 7, 9, 15, 20, 25, 70, 111 and 184 days. Self-immobilized and thermally treated samples were characterized by % C, Si-29 cross-polarization magic angle spinning (CP/MAS) NMR spectroscopy and reversed-phase column performance. The results show that thermal immobilization accelerates the distribution and rearrangement of the polymer on the silica surface. However, from the time that a monolayer has been formed by self-immobilization (similar to100 days for PMOS on Kromasil silica), the thermal treatment does not alter this configuration and, thus, does not change the resulting chromatographic parameters. (C) 2003 Elsevier B.V. All rights reserved.
引用
收藏
页码:217 / 223
页数:7
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