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  • 1
    ISSN: 1612-1112
    Keywords: Deactivation of columns ; Capillary gas chromatography ; Capillary supercritical fluid chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary In order to prevent plugging during deactivation of small diameter (50 μm i.d.) capillary columns for gas and supercritical fluid chromatography, various high temperature deactivation methods were employed. Pure hexamethyldisilazane and hexamethyldisiloxane (a substitute for D4) were dynamically coated on the column, while a film (0.05 μm) of OV-101 was statically coated, before high temperature (450°C) treatment. Excellent deactivated columns were obtained, and no significant difference in column activity was observed using any of these three methods.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 329-332 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Fused silica capillary columns ; Deactivation ; Polymethylhydrosiloxanes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 128-136 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Coating of capillaries, static and dynamic ; Rayleigh instability ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The film of stationary phase on the wall of a capillary column and that of the phase solution during both static and dynamic coating is subject to Rayleigh instability, which is quite independent of so-called wettability. A theory is developed which shows that the logarithmic growth rate of Rayleigh instabilities is proportional to the surface tension and to the third power of the film thickness, and inversely to the viscosity and to the fourth power of the capillary diameter. Determination of the variation of the viscosities of stationary phase solutions with concentration in coating solvents, and the variation of the viscosities of neat stationary phases with temperature, both revealed that heating and/or diluting changed the viscosities of phases with π-electron-containing, groups much more than for polydimethylsiloxanes. Rayleigh instability is therefore more important during coating of phenyl-containing phases such as OV-17, and later during column operation. The efficiencies of capillary columns of different diameters coated with a number of phases under different conditions of temperature and coating rate, and then operated at different temperatures were in good agreement with the predictions of the theory.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
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  • 4
    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
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  • 5
    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
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 11 (1988), S. 113-118 
    ISSN: 0935-6304
    Keywords: Static coating ; Biphenyl polysiloxane ; Capillary columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Static coating of phenyl and biphenyl polysiloxane stationary phases on 50 μm i.d. open tubular capillaries was studied. The influence of coating solvents and coating temperatures on the viscosities and surface tensions of the polymer stationary phases and their coating solutions was determined. A measure of the Rayleigh instability paralled the observed coating efficiencies.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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