Synthesis and characterization of a novel stationary phase, Si-Zr/Ti(PMTDS), based upon ternary oxide support for high performance liquid chromatography
A new stationary phase based on the thermal immobilization of poly(methyltetradecylsiloxane) (PMTDS) on silica particles coated with a mixture of zirconia and titania was prepared and evaluated for the chromatographic separation of test mixtures. The spherical particles were characterized by elemental analysis, SEM, FTIR and 29Si NMR. The physicochemical properties of PMTDS phase supported on Si-Zr/Ti were intermediate between PMTDS phases supported on titanized silica and zirconized silica. The chromatographic performance of Si-Zr/Ti(PMTDS) phase was similar to PMTDS phases based on metal oxide coated silica having only one metal oxide and the preparation of a Si-Zr/Ti(PMTDS) phase allowed evaluation of the effect of each oxide, zirconia and titania, on the separation process and on the stability of the immobilized polymer phase. The hydrolytic stability of Si-Zr/Ti(PMTDS) stationary phase was similar to the Si-Ti(PMTDS) phase, improving the chemical stability of the silica-based PMTDS phase by about 100%.
| Main Authors: | , , |
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| Format: | Digital revista |
| Language: | English |
| Published: |
Sociedade Brasileira de Química
2013
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| Online Access: | http://old.scielo.br/scielo.php?script=sci_arttext&pid=S0103-50532013000900016 |
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| Summary: | A new stationary phase based on the thermal immobilization of poly(methyltetradecylsiloxane) (PMTDS) on silica particles coated with a mixture of zirconia and titania was prepared and evaluated for the chromatographic separation of test mixtures. The spherical particles were characterized by elemental analysis, SEM, FTIR and 29Si NMR. The physicochemical properties of PMTDS phase supported on Si-Zr/Ti were intermediate between PMTDS phases supported on titanized silica and zirconized silica. The chromatographic performance of Si-Zr/Ti(PMTDS) phase was similar to PMTDS phases based on metal oxide coated silica having only one metal oxide and the preparation of a Si-Zr/Ti(PMTDS) phase allowed evaluation of the effect of each oxide, zirconia and titania, on the separation process and on the stability of the immobilized polymer phase. The hydrolytic stability of Si-Zr/Ti(PMTDS) stationary phase was similar to the Si-Ti(PMTDS) phase, improving the chemical stability of the silica-based PMTDS phase by about 100%. |
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