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  • 1
    ISSN: 0935-6304
    Keywords: Gas chromatography-mass spectrometry ; Capillary columns ; Stationary phases ; Silicones ; Thermal degradation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The applicability of capillary columns for gas chromatography is often limited by stationary phase degradation at elevated temperatures. In order to achieve a better understanding of column thermostability, column bleed products have been analyzed qualitatively by gas chromatography-mass spectrometry (GC-MS). Three silicone stationary phases were studied: SE-52, SE-54, and OV-1701. Each of these was immobilized in the columns. The proportion of cyclics containing diphenyl in column bleed from SE-52 reflected to a large extent the composition of the polymer, while for SE-54 the proportion of such cyclics was unexpectedly high. The polar moiety of OV-1701, the cyanopropyl(phenyl)siloxy unit, was found to exert a highly destabilizing effect on the polymer, and the thermal degradation products consisted mainly of cyclosiloxanes containing this unit.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 0935-6304
    Keywords: Open tubular gas chromatography ; Dynamic headspace analysis ; Purge and trap ; Thermal desorption ; Reinjection ; Fourier transform infrared spectroscopy ; Volatile constituents in polymers ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An analytical system for the analysis of volatiles entrained in polymers is described. This system is based on a thermal desorption oven connected to a cold trap. After enrichment of headspace vapor, trapped material is reinjected and analyzed by open tubular gas chromatography/Fourier transform infrared spectroscopy, OTGC/FTIR. The thermal desorption oven is designed to provide different modes of sample introduction: use of a pyroprobe; insertion of a piece of quartz tubing with applied sample; or syringe injection. Headspace enrichment is carried out in a piece of fused silica capillary tubing filled with glass beads. The trap may be cooled either electrically using Peltier elements or with liquid nitrogen. A six-port rotary valve is used for flow switching between enrichment and reinjection modes. All system parameters, temperatures, and timed events, are controlled from the gas chromatograph. Dynamic headspace analysis is demonstrated as a method for polymer characterization.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
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  • 3
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Glass and fused silica capillary columns ; Coating time and efficiency ; 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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