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  • Analytical Chemistry and Spectroscopy  (23)
  • 42.75
  • 2000-2004  (2)
  • 1985-1989  (21)
  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 8 (1985), S. 82-84 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary column ; Mass selective detector, MSD ; Ambient air ; Nitro-PAH ; 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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  • 2
    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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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 435-440 
    ISSN: 0935-6304
    Keywords: On-line coupled HPLC-GC ; Concurrent solvent evaporation ; Loop-type Interface ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Concurrent solvent evaporation using the loop-type HPLC-GC interface requires that the GC oven temperature be above the eluent boiling point at the given carrier gas inlet pressure in order to prevent eluent flowing into the GC capillary column. Corresponding oven temperatures representing minimum oven temperatures for eluent transfer were experimentally determined for solvents and solvent mixtures of interest for use as HPLC eluents. Evaluation of eluents for concurrent evaporation is discussed. Recommended lengths of uncoated column inlets (pre-columns) are derived from the mechanisms involved in solvent evaporation. Temperatures listed as minimum column temperatures for concurrently evaporating HPLC eluents are also useful for estimating maximum applicable column temperatures when working with the conventional retention gap or partially concurrent solvent evaporation techniques in coupled HPLC-GC.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 4
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The structure of the inner core region (L-glycero-D-mannoheptose/2-keto-3-deoxy-D-mannooctulosonic acid region) of lipopolysaccharides from Salmonella minnesota rough mutants was investigated. Using conventional methods (neutral sugar analysis, Smith degradation and methylation analysis) combined with gas chromatography/mass spectrometry (GC/MS) of higher oligosaccharides (up to tetrasaccharide), the linkages of the core sugars of lipopolysaccharides from S. minnesota rough mutants, strains R4 (Rd2P-), R7 (Rd1P-) and R5 (RcP-) were determined as: with R representing H in R4, L-glycero-D-mannoheptopyranosyl in R7, and D-glucopyranosyl-(1→3)-L-glycero-D-mannoheptopyranosyl in R5, respectively. In addition, it is shown that heterogeneity within the neutral sugar part of these lipopolysaccharides is low.
    Additional Material: 4 Ill.
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  • 5
    ISSN: 0935-6304
    Keywords: Gas chromatrography, GC ; Capillary columns ; Splitless and on-column injection ; Interlaboratory study ; Chlorobiphenyl congeners ; Internal standards ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The Community Bureau of Reference has organized a collaborative interlaboratory project to improve the analytical protocol for some specific chlorobiphenyls (CBs) within the European Community (EC). A series of test procedures were prescribed to optimize the gas chromatographic conditions for splitless and on-column injection, which substantially improved the quality of data. Important parameters included the initial column and injector temperatures and the choice of the polarity of the stationary phase. In a study with cleaned eel-fat extracts, coefficients of variation for reproducibility CV(R) ranging from 11 to 24% at the 0.04-0.3 mg/kg level per CB congener were obtained. No significant difference could be found between splitless- and on-column injection.
    Additional Material: 4 Tab.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 515-517 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary column ; Electron impact mass spectrometry ; Linear retention indices ; Dinitrofluoranthenes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This paper reports the retention indices of eighteen of the possible twenty-five dinitrofluoranthene isomers.
    Additional Material: 1 Ill.
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  • 7
    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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  • 8
    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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  • 9
    ISSN: 0935-6304
    Keywords: Comprehensive two-dimensional gas chromatography ; thermal desorption modulator ; temperature programming ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---In comprehensive two-dimensional gas chromatography, two individual separations are coupled by means of a rotating thermal desorption modulator interface. The injection pulse introduced via the interface onto the second column should be as short as possible. Parameters affecting the modulator operation are studied. In the set-up used in this study, the temperature of the second column can be programmed independently from that of the first column. Optimization of the second-dimension separation to minimize peak broadening and maximize resolution is discussed and an elegant approach to determine second-dimension retention times using a non-constant modulation frequency is demonstrated. The high separation power of the comprehensive system is demonstrated by the analysis of technical and biota samples containing chlorinated biphenyls and toxaphene.
    Additional Material: 7 Ill.
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  • 10
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Detection limits ; Trace analysis ; Narrow bore columns ; Wide bore columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The need for faster and more efficient separations of complex mixtures of organic compounds by gas chromatography has led to the development of small inner diameter open tubular columns. Owing to their decreased plate height, extremely narrow peaks are obtained. When differently sized columns with equal plate numbers are compared, injection of a fixed amount of a solute will give the highest detector signals for the smallest bore columns. When P is defined as the ratio of the column inlet and outlet pressures, it can be seen from theory that under normalized chromatographic conditions the minimum detectable amount (Qº) for a mass flow sensitive detector increases proportionally to the square of the column diameter for P = 1. In the situation of greater interest in the practice of open tubular gas chromatography where P is large, a linear relationship is derived between Qº and the column diameter.It is a widespread misunderstanding, however, that narrow bore capillary columns should be used for this reason in trace analysis. If a fixed relative contribution of the injection band width to the overall peak variance is allowed, a decreased plate height drastically restricts the maximum sample volume to be injected. It is shown that the minimum analyte concentration in the injected sample (Cº) is inversely proportional to the column inner diameter when a mass flow sensitive detector is used. For actual concentrations less than Cº, sample preconcentration is required. The effect of peak resolution and selectivity of the stationary phase in relation to Cº and Qº will be discussed as well. The validity of the given theory is experimentally investigated. Minimum analyte concentrations and minimum detectable amounts are compared using columns with different inner diameter.
    Additional Material: 8 Ill.
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