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  • 1
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Chlorinated and oxygenated cyclohexene derivatives detected in methylene chloride extracts of chlorinated drinking water were demonstrated to be artifacts produced during sample preparation. Commercial methylene chloride contains cyclohexene as a preservative, and this reacted during the extraction/concentration process to produce microgram amounts of chlorocyclohexene, 2-chlorocyclohexanol, trans-1,2-dichlorocyclohexane, cyclohexenone and cyclohexenol. Quantitative analysis indicated that over 90% of the initial cyclohexene was consumed during the process. Dechlorination of drinking water with sodium arsenite significantly reduced but did not eliminate cyclohexene artifact formation.
    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 19 (1996), S. 403-408 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Cryogenic trapping ; Capillary ; Focusing ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Cryogenic trapping of solutes leads to narrowing of the chromatographic band. By placing the trap at the end of a capillary column, it is possible to study the effectiveness of the trap in terms of producing a sharpened elution profile. The trap may be heated by supplementary heating, but here convective heating from the GC oven is employed simply by turning off the cryogenic coolant. It is estimated that it takes about 50 s for the trap to heat up sufficiently to allow trapped solute to be remobilized, although this depends upon the oven temperature and thermal mass of the trap. It can also be shown that the more volatile solutes mobilize faster from the trap in this particular mode of operation. The recovery of trapped components shows that there is essentially quantitative trapping, and the solutes are trapped just at the leading edge of the trap.
    Additional Material: 4 Ill.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 620-622 
    ISSN: 0935-6304
    Keywords: Multidimensional gas chromatography ; comprehensive two-dimensional gas chromatography ; kerosene analysis ; cryogenic modulation ; 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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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 235-238 
    ISSN: 0935-6304
    Keywords: Cryogenic modulation ; LMCS ; GC×GC ; multidimensional GC ; comprehensive gas chromatography ; petroleum analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: No abstract
    Additional Material: 4 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 622-626 
    ISSN: 0935-6304
    Keywords: Multidimensional capillary chromatography ; Polychlorinated biphenyls ; PCBs ; Congener ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Multidimensional chromatography was used to resolve the specific chlorobiphenyl (CB) congeners 28, 52, 101, 118, 138, 153, and 180 in technical aroclor standards. Single column analysis of polychlorinated biphenyls (PCBs) results in co-elution of key congeners with other components in the mixture; therefore using two columns of different selectivity was necessary to enhance the resolution achievable on just one column. The HT8 column (8% phenylpolycarborane-siloxane phase) has been reported to have specific selectivity characteristics for improved PCB separation. When coupled with a BPX5 column (5% phenylpolysiloxane-silphenylene phase), it has been shown here to provide unambiguous identification of 7 marker compounds which are used to monitor PCB occurrence and distribution. All seven marker CBs are present in aroclor 1254, and by adjusting the size of the heartcut window, it was possible to obtain resolution of the marker congeners from other congeners. Single column analysis is unable to achieve this result. This offers an alternative to GC-MS analysis.
    Additional Material: 3 Ill.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 253-258 
    ISSN: 0935-6304
    Keywords: Comprehensive gas chromatography ; cryogenic modulation ; semi-volatile aromatics ; thermal sweeper ; peak widths ; peak asymmetries ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The two current technologies for achieving comprehensive gas chromatography (GC×GC) - the thermal sweeper and the cryogenic modulator - are compared in an interlaboratory study using a multicomponent semi-volatile aromatic compound sample. The same column set (phases, film thickness, dimensions of columns) and conditions of oven temperature program were used. Carrier gas flow settings however were different for the data reported here. The thermal sweeper has a longer overall length due to the extra ca. 30 cm length of narrow bore tubing used for the modulator/accumulator section. Data reveal that the two methods behave in an analogous manner in respect of delivering GC×GC results, with key peak parameters of peak widths and symmetry measures showing good correlation. Retention time dissimilarity on the first dimension columns in the two systems arises from different flow rates used, however the second column retention is similar, and this is due to the resulting different elution temperatures that peaks elute on the first dimension in each system. Overall, the two approaches to GC×GC appear to produce equivalent results within the scope of the application studied. Each system does have its experimental limitations; the thermal sweeper has what may be called a ‘thick film effect’, where at high temperature it can be difficult to sufficiently trap the migrating bands in the accumulator column, and the pulsing of solutes in the cryogenic system may suffer from a ‘thick wall effect’ if a column with too thick a wall dimension is used at low oven temperature.
    Additional Material: 4 Ill.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 281-284 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Time-switched detectors ; UV detection ; Fluorimetric detection ; Vitamin A ; Vitamin E ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An HPLC method utilizing a UV and a fluorimetric detector linked in series is described. By use of a simple integrator-controlled time-switched relay, analysis of serum vitamin A and E is accomplished on the same chromatogram and at optimum sensitivity for each detector. A single internal standard (retinyl acetate) monitored only by the UV detector permits measurement of both vitamins over a wide linear range. Precision of the assays is satisfactory, both on a within-day and on a day-to-day basis. Recoveries of both vitamins are virtually 100% whilst sensitivity is 2 μg/L (retinol) and 0.05 mg/L (α-tocopherol).
    Additional Material: 4 Ill.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 13 (1990), S. 287-289 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Oleic acid ; Free fatty acids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 9
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The syntheses of 2′-O-succinyl, 2′-O-succinyltyrosinyl methyl ester and 2′-O-succinyliodotyrosinyl methyl ester derivatives of a cyclic nucleotide, derivatives necessary for the successful development of a specific radioimmuno-assay, are described. Fast atom bombardment with collision-induced dissociation and mass-analysed ion kinetic energy spectroscopy were used to verify the positions of substitution and the retention of the 3′,5′-cyclic phosphate moiety. Comparison of spectra produced after different iodination times permitted the optimization of the reaction conditions.
    Additional Material: 6 Ill.
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  • 10
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ion-to-neutral conversion at surfaces is found to be complementary to that with gas-phase targets for neutralization-reionization mass spectrometry and to yield high-energy neutral species. With an Ag surface deposited on an in-line Si substrate, neutralization-reionization efficiencies of 0.01% are achieved using 9.8 keV CH4+·, with the neutral CH4 receiving a median internal energy of 14 eV; with a conventional target of K vapor, the efficiency is 0.4% with a neutral energy of 8.2 eV expected from their ionization energy difference. The energy deposition can be increased by increasing the potential that deflects ions into the surface; in this way ∼15% of CH4 neutral species can be given 〉20 eV of internal energy. Product abundances from CH4 dissociation provide a useful estimate of the distribution of energy values deposited in neutralization.
    Additional Material: 4 Ill.
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