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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 11 (1988), S. 626-632 
    ISSN: 0935-6304
    Keywords: PTV splitless injection ; Splitless injection ; Large sample volumes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: PTV splitless injection cannot compete with on-column injection as far as simplicity, reliability, and accuracy of quantitative analysis is concerned. However, PTV splitless injection is attractive for trace analysis of samples containing high concentrations of involatile sample by-products. Maximum injection volumes are limited by the amount of liquid that can be retained within the PTV injector chamber and are around 20-30 μl injected at once. Solvent evaporation must be carried out in such a way that injector overflow is avoided.
    Additional Material: 4 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. 658-659 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Ferrule particle ; Column performance ; Column installation ; 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 13 (1990), S. 803-810 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Uncoated precolumns ; Solvent peak ; Porosity of capillary surfaces ; Deactivation methods ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Many uncoated precolumns, and to a lesser extent separation columns, strongly retain some of the solvent. Retarded release of such solvent elevates the baseline after the solvent peak and causes ugly “humps” of eluted solvent as the temperature is increased. The problem is probably a result of retention by a porous surface, e.g. surfaces obtained by leaching or hydrothermal treatment of capillaries prior to silylation. It is assumed that other problems with capillary columns can be explained by the same mechanism, including: a kind of adsorption including apolar compounds, and “ghost” peaks as well as “memory” effects. Fused silica capillaries are superior to glass, but even for these special procedures are required in order to achieve thorough deactivation of the internal surface without introducing porosity.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 14 (1991), S. 212-214 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Uncoated precolumn ; Water-resistant deactivation ; Coupled LC-GC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 13 (1990), S. 540-546 
    ISSN: 0935-6304
    Keywords: PTV Injection ; Vapor overflow ; Sample introduction at reduced pressure ; Evaporation rates ; Large sample volumes ; Coupled LC-GC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The concept of a GC solvent evaporation technique is outlined that involves a modified Programmed Temperature Vaporizing (PTV) injector. The vapor overflow technique is intended for introducing samples in large volumes of solvent by syringe injection of strongly diluted samples or by coupled LC-GC. The liquid is introduced into a packed vaporizing chamber kept above the solvent boiling point at a pressure which is near or below ambient. The carrier gas is essentially switched off. Evaporation and discharge of the solvent vapors occurs by expansion of the vapors, driven by the solvent vapor pressure. For transferring the sapmple into the column, the carrier gas is switched on again and the vaporizing chamber heated.Compared to PTV solvent split injection, vapor overflow offers the following advantages: It automatically optimizes operational parameters, therefore facilitating its application. Losses of volatile materials are minimized by a minimal flow rate through the injector.Vapor overflow is a promising technique for transferring watercontaining eluents in coupled LC-GC since no wettability is required and leaching of pre-column surfaces is avoided.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 14 (1991), S. 207-210 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Cyclodextrin stationary phases ; Dilution of cyclodextrins ; Chiral resolution ; Glass capillary columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 11 (1988), S. 560-565 
    ISSN: 0935-6304
    Keywords: LC/GC ; Concurrent solvent evaporation ; Solvent effects ; Co-solvent effects ; Large sample volumes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Co-solvent effects are applied to allow use of concurrent solvent evaporation for applications requiring analysis of compounds eluted less than some 50° above the column temperature during sample introduction, i.e. at oven temperatures below some 100-120°C. Required conditions such as GC even temperature, concentration of the co-solvent and length of the uncoated pre-column (retention gap) are studied theoretically as well as experimentally for the case of n-heptane as co-solvent in n-pentane.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 12 (1989), S. 721-726 
    ISSN: 0935-6304
    Keywords: Coupled LC-GC ; Partially concurrent eluent evaporation ; Evaporation rates ; Early solvent vapor exit ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Partially concurrent eluent evaporation presupposes an eluent evaporation rate in the GC pre-column that approaches the LC flow rate. Discharging the vapors through the whole GC column, evaporation rates reach 10-30 μl/min, i.e. are suitable just for LC flow rates typical for packed capillary LC columns. With an early vapor exit, evaporation rates are increased to 100-200 μl/min (under extreme conditions to some 800 μl/min), thus fitting the LC flow rates of 2 mm i.d. columns.Evaporation rates were measured for a standard set of pre-columns and conditions. The dependence of the evaporation rate on temperature, inlet pressure, carrier gas, and internal diameter of the retaining pre-column are discussed in order to allow the design of a GC system producing a desired evaporation rate.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 18 (1995), S. 573-578 
    ISSN: 0935-6304
    Keywords: Large sample volumes ; Vaporizing chambers ; Evaporation rates ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The suitability of some chambers for sample evaporation at high input flow rates (〉100 μl/min) was studied by visual experiments. The chambers were at temperatures far above the solvent boiling point in order to achieve the heat transfer required. Shooting liquid owing to violent evaporation, flooding of the chamber as a result of cooling, and excessively high vapor pressure causing backflow into the gas supply system were found to be the limiting factors. Fused silica capillaries into which a piece of wire or polyimide-free fused silica capillary had been inserted were found to be suitable for the vaporization of “easy” solvents, such as alkanes (up to some 1.7 ml/min), but packed beds were required to achieve favorable evaporation of dichloromethane or methanol/water (up to some 800 and 300 μl/min, respectively).
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 14 (1991), S. 558-559 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Coupled LC-GC ; Contamination of solvent ; “Ghost” peaks ; “Fingerprints” ; 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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