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Synthesis of novel stationary phases for use in gas and supercritical fluid chromatography

Posted on:1994-06-07Degree:Ph.DType:Thesis
University:Brigham Young UniversityCandidate:Reese, Shawn LaddFull Text:PDF
GTID:2471390014992431Subject:Chemistry
Abstract/Summary:
The purpose of this study was to develop and test new stationary phases for gas and supercritical fluid chromatography. Nine new isomeric cyanobiphenyl substituted polysiloxanes were synthesized and tested. For 0.2 mm i.d. columns, efficiencies were as high as 5100 p/m. Thermal stabilities were near 300{dollar}spcirc{dollar}C for all of the isomers, except one. Three new multisubstituted biphenyl polysiloxane stationary phases were also synthesized with efficiencies as high as 4000 p/m for 0.2 mm i.d. columns, and thermal stabilities were near 300{dollar}spcirc{dollar}C. The new substituted biphenyl phases showed selectivities comparable to commercially available stationary phases. Six new chiral stationary phases were also synthesized. These phases show unique selectivity for resolving selected racemic diols, and lactones. Efficiencies for a 0.2 mm i.d. column were less than 1000 p/m, except the oxazolines which were near 2000 p/m. Molecular modeling was conducted to provide insights into the selectivity of the cyanobiphenyl stationary phases. The synthesis and characterization of these materials are given.
Keywords/Search Tags:Stationary phases, Supercritical fluid chromatography, Thermal stabilities were near 300{dollar}spcirc{dollar}c
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