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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 14 (1991), S. 235-240 
    ISSN: 0935-6304
    Keywords: High speed capillary GC ; Metal capillary cold traps ; Thermal decomposition of analytes ; Effect of carrier gas ; Quantitative analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Thermal decomposition of some hydrocarbon and chlorinated hydrocarbon compounds in metal capillary tubes used in an inlet system for high speed gas chromatography has been investigated. The metal tube is cooled to about -75°C by a flow of cold nitrogen gas in order to focus a vapor sample cryogenically. A capacitive discharge power supply is then used to heat the metal tube resistively in order to revaporize the sample and introduce it to the separation column as a plug 5-10 ms wide. The effects of tube temperature, tube material, sample vapor residence time, and type of carrier gas on thermal cracking are described. Use of a copper-nickel alloy tube resulted in less cracking than either pure platinum or pure nickel. Cracking is more significant with hydrogen as carrier gas than with helium. Cracking also increases with increasing sample residence time in the hot tube. Quantitative sample injection with minimum decomposition can be obtained for a variety of aliphatic and aromatic hydrocarbons and chlorinated hydrocarbon compounds.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 13 (1990), S. 674-678 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Vacuum backflush ; Repetitive analysis ; Vapor stream analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A vacuum-pump-operated backflush system has been developed for applications involving high-speed, repetitive GC analysis of gas streams containing ppm and ppb levels of organic vapor. The system uses an injector capable of cryofocusing and a relatively short length of 0.25-mm i.d. fused silica column for the separation of relatively simple mixtures of volatile compounds. Analysis times typically are in the 5-10 s range, and backflush times are in the 2-5 s range. Gases from the flame ionization detector are used as the backflush carrier gas, and no modification of the detector is necessary. A procedure is described which allows the average gas velocity to be measured during backflush operation. The minimum backflush time is directly proportional to the analysis time and to the square of the column length, making this system most useful with short columns and short analysis times.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 225-234 
    ISSN: 0935-6304
    Keywords: Tunable column ensembles ; high speed GC ; comprehensive two-dimensional GC ; time of flight ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---A series-coupled ensemble of two capillary GC columns of different selectivity with an adjustable pressure at the column junction point is used to obtain tunable selectivity for high-speed GC and GC/TOFMS. An electronic pressure controller with a 0.1-psi step size is used to obtain numerous computer-selected unique selectivities. System configurations for conventional, atmospheric-pressure outlet operation with flame ionization detection and for vacuum-outlet operation with photoionization detection are described for GC-only experiments. Polydimethylsiloxane is used as the non-polar column and polyethylene glycol (atmospheric outlet) or triflouropropylpolysiloxane (vacuum outlet) is used as the polar column. For GC/TOFMS experiments, 5% phenyl polydimethylsiloxane was used as the non-polar column, and polyethylene glycol was used as the polar column. The time-of-flight mass spectrometer can acquire up to 500 complete mass spectra per second. Since spectral continuity is achieved across the entire chromatographic peak profile, severely overlapping peaks can be spectrally deconvoluted for high-speed characterization of completely unknown mixtures. For mixture components with significantly different fragmentation patterns, spectral deconvolution can be achieved for chromatographic peak separations of as little as 6.0 ms. This can result is very large peak capacity for time compressed (not completely resolved) chromatograms. The use of columns with tunable selectivity allows for precise peak-position control, which can result in more efficient utilization of available peak capacity and thus further time compression of chromatograms. The limits of tunability and deconvolution are tested for near co-elutions of different classes of hydrocarbon compounds as well as for more multi-functional mixtures.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
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