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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 506-514 
    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
    Library Location Call Number Volume/Issue/Year Availability
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 378-384 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Deactivation ; Phenylhydrosiloxanes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In this work, an investigation of new organosilicon hydride reagents with phenyl functional groups for deactivation and surface modification of fused silica capillary columns is described. Different reagents were tested for their ability to deactivate the fused silica surface, and actual critical surface tension measurements were made using the capillary rise method. The deactivation procedure required lower optimum temperatures than conventional methods. Deactivated capillaries and coated capillary columns were prepared and tested for reproducibility, efficiency, and surface inertness towards basic and acidic compounds at the low nanogram level.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    Library Location Call Number Volume/Issue/Year Availability
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