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  • Articles  (19)
  • Chemistry  (18)
  • Capillary gas chromatography  (2)
  • Fused silica capillary columns  (2)
  • 1
    ISSN: 1612-1112
    Keywords: Crosslinked phenyl silicones ; Capillary gas chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Methyl(phenyl)silicones offer useful selectivities when used as stationary phases in gas chromatography (GC). Such phases have, however, hitherto been of restricted importance in capillary GC due to the lack of phases having a viscosity high enough to ensure stationary phase film stability. Further, to utilize fully the possibilities of a methyl(phenyl)silicone capillary column, it must also possess high efficiency and a high degree of deactivation. In this work, the preparation of soda-glass capillary columns coated within situ cured methyl(phenyl) and methyl(tolyl)-silicones is presented. Vulcanization was made possible by the introduction of some vinyl substitution in the gum to be cured: tolyl-containing gums could be cured without the presence of vinyl groups. In addition, fused silica capillary columns coated with OV-1701 were prepared. The columns show a coating efficiency of above 80%, a thermal stability up to 320 °C and a high degree of deactivation. Their utility is demonstrated by the separation of samples containing polynuclear aromatics, antidepressants and some potent mutagens.
    Type of Medium: Electronic Resource
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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.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 213-217 
    ISSN: 0935-6304
    Keywords: Capillary supercritical fluid chromatography ; Injection system ; Polycyclic aromatic compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A sample introduction system for capillary supercritical fluid chromatography, which allows the dissolution of the sample in the supercritical mobile phase before being introduced into the column, was constructed and evaluated. Supercritical n-pentane was shown to solvate high-molecular-weight polycyclic aromatic compounds that could not be solvated using typical liquid solvents. In addition, split injection of a supercritical fluid solution was found to be more reproducible than split injections of a liquid solution. The potential of such an injection system was demonstrated, although further developments are needed in order to make the technique of practically utility.
    Additional Material: 3 Ill.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 527-528 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Surface deactivation ; High temperature silylation ; Cyclic trifluoropropylsiloxanes ; Improved surface wettability ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 4 (1981), S. 578-579 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Crosslinked silicones ; Peroxide-initiated vulcanization ; Trifluoropylsilicone ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 6
    ISSN: 0935-6304
    Keywords: Capillary columns ; Gas chromatography, GC ; Stationary phases ; Liquid crystal ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Mesomorphic biphenylcarboxylate esters were coupled via flexible aliphatic hydrocarbon spacers to a polysiloxane backbone. The influence of spacer length, percent mesomorphic substitution, and crosslinking of the stationary phase on liquid-crystalline transition temperatures and on chromatographic performance was investigated. Unique selectivity and good efficiency over a wide temperature range for gum and cross-linked liquid-crystalline phases were demonstrated by the separation of various isomeric polycyclic aromatic compounds.
    Additional Material: 4 Ill.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 741-747 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Fused silica capillary columns ; Deactivation ; Cyanopropylhydrosiloxanes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method is described for surface deactivation and modification of fused silica capillary columns with a cyanopropyl-containing reagent. The deactivation procedure involved a dehydrocondensation reaction between a bis(cyanopropyl)methylhydropolysiloxane reagent and surface silanol groups at an optimum temperature of only 250°C. Actual critical surface tension measurements were made using the capillary rise method. Excellent deactivation for acidic and basic compounds at the low ng level, and wettability for nonpolar and polar polysiloxane stationary phases were obtained. A procedure was developed to remove acidic impurities that are present in polar stationary phases.
    Additional Material: 5 Ill.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 632-650 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 8 Ill.
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  • 9
    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.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 652-656 
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography ; Capillary columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In cases where high efficiency is required to resolve complex mixtures of either thermally labile or nonvolatile organic compounds, capillary supercritical fluid chromatography may be the most desirable analytical method. While great strides in this new technology have been made over the last few years, several problem areas are requiring increased attention. These include sample introduction systems, pressure reduction at the end of the column, column stability in various supercritical mobile phases, and migration of polar solute molecules. This paper describes the state-of-the-art in capillary SFC with emphasis on the progress made and future needs in the solutions to these specific problems.
    Additional Material: 3 Ill.
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