Synthesis and characterization of endcapped C18 stationary phases using a silica hydride intermediate.

Synthesis and characterization of endcapped C18 stationary phases using a silica hydride intermediate.
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使用二氧化硅中间体合成和表征封端 C18 固定相。

DOI:
10.1016/s0021-9673(02)00014-6
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发表时间:
2002
期刊:
Journal of chromatography. A
影响因子:
--
通讯作者:
Yu,RaymondJ
Yu,RaymondJ
中科院分区:
--
文献类型:
--
作者:
Pesek,JosephJ;Matyska,MariaT;Yu,RaymondJ

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The effect of endcapping on an octdecyl bonded phase synthesized by the silanization/hydrosilation method is investigated. The endcapping reagent is a 1:1 molar ratio of trimethylchlorosilane (TMCS) and hexamethyldisilizane (HMDS). Two approaches for endcapping are possible for this synthetic method that produces a silica hydride intermediate: bonding of TMCS–HMDS after silanization (on the hydride intermediate) or after hydrosilation (on the C18product stationary phase). The use of TMCS–HMDS is designed to eliminate the few remaining silanols on the silica hydride intermediate. The endcapping process is characterized spectroscopically by diffuse reflectance infrared Fourier transform (DRIFT),29Si cross polarization magic angle spinning nuclear magnetic resonance spectroscopy (CP-MAS-NMR) and13C-CP-MAS-NMR. The octadecyl bonded phases are characterized chromatographically by measuring the capacity factors of several hydrophobic and basic test solutes as well as the separation factors among various solute pairs. Finally, long-term stability tests are done on both products at high and low pH.
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