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  • General Chemistry  (354)
  • Gas chromatography  (6)
  • Coupled LC-GC  (5)
  • Atomic and molecular processes in external fields, including interactions with strong fields and short pulses
  • Atomic and molecular structure and dynamics
  • Surface physics, nanoscale physics, low-dimensional systems
  • Wiley-Blackwell  (365)
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Keywords
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  • 1
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Separation of polychloro biphenyls ; Separation of organochlorine pesticides ; Splitless automated injection ; Residue level ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Complicated PCB mixtures can be separated in individual compounds using glass capillary gas chromatography, (GC)2. Depending on extraction and clean-up procedure it is also possible to separate and determine organochlorine pesticides at the same time.This (GC)2 technique can be used to determine the contents of individual chlorinated biphenyls in milk products and animal feedstuffs and in the analysis of complicated extracts of soil and vegetable material.Practical aspects concerning connection of the capillary, automatic splitless injection, repeatability of the retention time, quality of the column with respect to separation and adsorption and degradation of DDT are discussed.The detection of individual chlorinated biphenyls is possible at the ppb level in fats and vegetable materials, using an extraction and clean-up procedure, based on saponification of the sample.Preliminary results for milk, obtained from several areas, are shown.
    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 3 (1980), S. 298-298 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary, glass ; Closing technique for static coating ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 11 (1988), S. 106-110 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Tandem capillaries ; Charcoal trapping ; Soil fumigants ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Soil fumigants, like 1,3-dichloropropene and metham-sodium (forming methyl isothiocyanate) diffuse into the atmosphere, thus presenting a hazard to people in the surroundings. A method is described in which a large volume (50 μl) of extractant, used to desorb the compounds from charcoal, is injected into a GC, equipped with two capillary columns. By way of Deans switching, the solvent is separated from the compounds of interest. Modification of a GC sampler makes unattended analyses possible.
    Additional Material: 2 Ill.
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  • 4
    ISSN: 0935-6304
    Keywords: Capillary GC ; Coupled LC-GC ; Large injection volumes ; Trace analysis ; Aqueous samples ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This paper describes the design of a new, versatile, and low-cost on-line LC-GC interface that allows the fast and reliable introduction of large sample volumes onto a capillary GC column. The sample introduction procedure consists successively of: evaporation of the entire sample (LC fraction), selective removal of the solvent and simultaneously cold-trapping of the solutes, splitless transfer of the solutes to the GC column, on-column focusing, GC separation and detection. Quantitative and qualitative aspects of various experimental parameters are evaluated and optimum conditions are reported. The applicability of the method is demonstrated on a synthetic aqueous sample of chlorinated pesticides.
    Additional Material: 15 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 13 (1990), S. 157-161 
    ISSN: 0935-6304
    Keywords: Coupled LC-GC ; Partially concurrent solvent evaporation ; Trace enrichment ; Surface water ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The feasibility of using ethyl acetate for the desorption of trace pollutants from a liquid chromatographic precolumn on-line into a diphenyltetramethyldisilazane-deactivated retention gap and, subsequently analysis by means of capillary gas chromatography has been demonstrated. First 5% of methanol are added to the water sample to prevent sorption of analytes onto parts of the preconcentration system. About 1 ml of this aqueous sample is injected onto a precolumn containing a polymeric stationary phase, using water-methanol (95:5, v/v) for transport and clean-up. The precolumn is desorbed with ethyl acetate and a fraction of 75 μl is injected on-line into the retention gap; separation is then achieved on a capillary CP Sil 19 column. No breakthrough of the test compounds was observed in the preconcentration step. The recovery was quantitative and the response obtained with flame ionization detection was linear in the range 0.1-100 ng/ml. The effect of varying the sorption flow rate on the recovery was studied. The system was applied to the analysis of river water.
    Additional Material: 6 Ill.
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  • 6
    ISSN: 0935-6304
    Keywords: Coupled LC-GC ; Retention gap ; LC trace enrichment ; Aqueous samples ; Organic pollutants ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Trace enrichment for the GC analysis of a series of chlorinated pesticides and polychlorinated biphenyls (PCBs) in aqueous samples has been achieved through a simple on-line technique involving sorption on an LC micro-precolumn followed by direct elution into a gas chromatograph with hexane. A 5-m retention gap coupled to the capillary GC column served as the recipient of a relatively large sample volume (ca. 100 μl) introduced into the GC. Partially concurrent solvent evaporation during sample introduction allowed a large sample capacity. Recoveries of more than 95% were observed for the majority of the compounds studied. Using 1.0 ml aqueous samples, detection limits of less than 1 ppt were found. The applicability of the developed method was demonstrated for a river water sample.
    Additional Material: 7 Ill.
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  • 7
    ISSN: 0935-6304
    Keywords: Polar solvents ; Coupled LC-GC ; Partially concurrent solvent evaporation ; Trace enrichment ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Coupling column liquid chromatography and gas chromatography on-line is becoming more important in analytical chemistry. Especially when large amounts of polar solvents can be introduced into the gas chromatograph without any problem, the technique will offer new possibilities. With a DPTMDS retention gap, evaporation rates and flooded zones of some solvents have been determined. Two modes of operation using partially concurrent solvent evaporation conditions are discussed: (1) injecting a sample via a loop of an LC valve followed by introduction into the gas chromatograph with an LC pump; (2) trace enrichment on a precolumn followed by on-line desorption with n-propanol into the gas chromatograph. Preliminary results for a splitter system, inserted between the retention gap and the analytical column which allows a considerable increase of the evaporation rate are also presented.
    Additional Material: 4 Ill.
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  • 8
    ISSN: 0935-6304
    Keywords: Coupled LC-GC ; Retention gap ; Variable splitter ; Partially concurrent solvent evaporation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A system is described which accelerates the solvent evaporation rate in the retention gap. The evaporation is due to a saturation effect of the carrier gas stream, and a considerable increase in evaporation rate is obtained by inserting a split outlet between the retention gap and the capillary separation column in the gas chromatograph. By varying the backpressure of the spliter device, the flow rate through the retention gap can be adjusted and so too the evaporation rate. The evaporation process was monitored by inserting a dectecter in the split outlet line. The technique was applied to the on-line LC trace enrichment/GC analysis of water containing a mixture of polycyclic aromatic hydrocarbons.
    Additional Material: 4 Ill.
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 18 (1995), S. 19-27 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Large volume injection ; PTV injectors ; PTV splitless injection ; PTV solvent split injection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Temperature programmable injectors with liner diameters ranging from 1 to 3.5 mm are evaluated and compared for solvent split injection of large volumes in capillary gas chromatography. The liner dimensions determine whether a large sample volume can be introduced rapidly or has to be introduced in a speed controlled manner. The effect of the injection technique used on the recovery of n-alkanes is evaluated. Furthermore the influence of the liner diameter on the occurrence of thermal degradation during splitless transfer to the analytical column is studied. Guidelines are given for the selection of the PTV liner internal diameter best suited for specific applications.
    Additional Material: 9 Ill.
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  • 10
    ISSN: 1434-193X
    Keywords: Asymmetric synthesis ; Nitrogen heterocycles ; N-Acyliminium ions ; PCP site ligands ; Pharmacological enantioselectivity ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new method for the asymmetric synthesis of 1-substituted tetrahydroisoquinolines is presented. It is based on stereoselective addition reactions of organometallic compounds to the intermediate N-acyliminium ion 6, which is provided with an N-acyl group as a chiral auxiliary. In addition reactions with organomagnesium and organozinc reagents diastereoselectivities from 70:30 to 95:5 (for 7/8) were observed with the zinc reagents in general leading to markedly improved stereoselectivities. By catalytic hydrogenation of 7 and 8 and after removal of the chiral auxiliary the target compounds 11 and 12 were obtained. The enantiomerically pure 11c-g and 12c-g (ee 〉 99 %), 1-aryl-tetrahydroisoquinolines, were evaluated for their affinity to the PCP [1-(1-phenylcyclohexyl)piperidine] binding site of the NMDA (N-methyl D-aspartate) receptor. In each case the enantiomers 11 exhibited a higher affinity than those of 12, with the potencies of the enantiomers differing by a factor of 4 (11/12g) to 27 (11/12c). The absolute configuration of the more potent enantiomers 11 is in accordance with the stereochemical requirement found for FR115427 (3) which is a close analogue.
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