ISSN:
0935-6304
Keywords:
Supercritical fluid chromatography, SFC
;
Deactivation
;
Gas chromatography, GC
;
Small diameter capillary columns
;
Organosilicon hydrides
;
Chemistry
;
Analytical Chemistry and Spectroscopy
Source:
Wiley InterScience Backfile Collection 1832-2000
Topics:
Chemistry and Pharmacology
Notes:
Small diameter fused silica capillary columns (50-75 μm i.d.) were deactivated at relatively low temperatures (250-300°C) with a mixture of polymethylhydrosiloxanes and several lowmolecular-weight organosilicon hydrides. Reproducible surface deactivations of highest quality were achieved with the polymethylhydrosiloxane (PMHS) reagent. Deactivations performed with PMHS via dynamic coating with neat or diluted reagent were evaluated by gas chromatography. Deactivations achieved with organosiloxane mono-, tri-, and tetrahydrides were also evaluated and compared. Low-molecular-weight organosilicon hydride deactivations were less time consuming and required lower head pressures for filling and coating columns with the reagent. Critical surface tensions of capillary surfaces modified with PMHS and the low-molecular-weight organosilicon hydrides gave support to the dehydrocondensation reaction between silica surface silanols and silyhydride bonds of the reagents. Slopes from Zisman plots indicated that coverage of the surface ranged from highest for the polymer (PMHS) to lowest for the monomers (TMS and PMDS). Efficiency measurements showed the influence that surface modification had on the uniformity and stability of the coated capillary columns. Well-deactivated capillary columns permitted the chromatography of polar solutes using supercritical carbon dioxide as mobile phase.
Additional Material:
5 Ill.
Type of Medium:
Electronic Resource
URL:
http://dx.doi.org/10.1002/jhrc.1240090904
