Fast supercritical fluid chromatography using capillaries packed with nonporous particles |
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Authors: | Y Shen M L Lee |
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Institution: | (1) Department of Chemistry and Biochemistry, Brigham Young University, 84602 Provo, UT, USA |
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Abstract: | Summary Packed columns containing microparticles provide high column efficiency per unit time and strong retention characteristics
compared with open tubular columns, and they are favored for fast separations. Nonporous particles eliminate the contribution
of solute mass transfer resistance in the intraparticle void volume characteristic of porous particles, and they should be
more suitable for fast separations. In this paper, the evaluation of nonporous silica particles of sizes ranging from 5 to
25 μm in packed capillary columns for fast supercritical fluid chromatography (SFC) using neat CO2 is reported. These particles were first deactivated using polymethyl-hydrosiloxanes and then encapsulated with a methylphenylpolysiloxane
stationary phase. The retention factors, column efficiencies, column efficiencies per unit time, separation resolution, and
separation resolution per unit time for fast SFC were determined for various length capillaries packed with various sizes
of polymerencapsulated nonporous particles. It was found that 15 μm nonporous particles provided the highest column efficiency
per unit time and resolution per unit time for fast packed capillary SFC. Under certain conditions, separations were completed
in less than 1 min. Several thermally labile silylation reagent samples were separated in times less than 5 min.
Presented at the 21st ISC held in Stuttgart, Germany, 15th–20th September, 1996 |
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Keywords: | Supercritical fluid chromatography Fast analysis Packed capillary columns Nonporous particles |
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