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  • 1990-1994  (7,463)
  • 1925-1929
  • Analytical Chemistry and Spectroscopy  (7,463)
  • 101
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 868-868 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 102
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 103
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 20-21 
    ISSN: 0935-6304
    Keywords: Capillary GC ; GC-MS ; Gorse pyrolytic oil ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Thermochemical conversion of biomass produces solid charcoal, gaseous fuels, and condensable oils. Because these oils vary widely in composition depending on the cellulosic feedstock and the operating conditions used, analysis of the oils is necessary in order to determine the best ways of utilizing or disposing of them. The major components of the organic oil from pyrolysis of gorse have been characterized by capillary gas chromatography - mass spectrometry. A qualitative study of the aqueous oil from the same source has also been attempted.
    Additional Material: 2 Tab.
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  • 104
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 25-30 
    ISSN: 0935-6304
    Keywords: GC ; Dynamic headspace analysis ; Capillary columns ; Flavor ; Volatile flavor compounds ; Dairy products ; Cheese ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The aim of this study was to test the suitability and performance of various stationary phases and column dimensions for dynamic headspace gas chromatography of food aromas. The trials were performed using an aqueous test mixture containing thirty seven volatile flavor components of intense aroma, and a sample of ripe Swiss Emmental cheese.The best performance with both samples was obtained with a capillary column coated with a thick film of polydimethylsiloxane. This column resolved the greatest number of compounds in the cheese sample and resulted in the overlapping of one pair of peaks only from the test mixture. Because of its other advantages, i. e. high capacity owing to its film thickness, and insensitivity to the high moisture content of some samples or traces of oxygen in the carrier gas, the polydimethylsiloxane column appears suitable for the analysis of the volatile and highly polar compounds present in complex mixtures such as food aroma.
    Additional Material: 2 Ill.
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  • 105
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 31-36 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Graphitized carbon black ; Carbon layer open tubular columns ; Column polarity ; Retention times prediction ; Programmed temperature GC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The polarity of carbon layer open tubular (CLOT) columns coated with a layer of non-porous graphitized carbon black (Carbopack B) modified with an appropriate amount of polar polyglycol liquid phase has been evaluated and compared with that of standard polar (Supelcowax-10) and non-polar (SPB-1) bonded phase open tubular columns. The efficiency and selectivity were measured at various temperatures and the polarity of the columns was evaluated by use of McReynolds' constants and the difference in apparent carbon number, ΔC of linear alkanes and alcohols. The polarity of the CLOT column was found to depend on temperature, and changing the analytical conditions therefore enabled the separation of compounds of different polarity whose reciprocal position and resolution were affected by temperature. The application of calculation methods which enable programmed temperature retention times to be predicted from isothermal data was also found to be possible when the polarity of the CLOT column changes with temperature.
    Additional Material: 7 Ill.
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  • 106
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 47-48 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 107
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 48-48 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 108
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography (CGC) ; Enantioselective separations ; (2,3,6-Tri-O-methyl)cyclodextrins ; Enantiomeric excess determination ; 2,3-Isopropylidene-1,2,3-cyclohexanetriol derivatives ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Capillary GC on permethyl α-, β-, and γ-cyclodextrins has been applied to separate and quantify the enantiomers of some 2,3-iso-propylidene-1,2,3-cyclohexanetriol derivatives. Quantitative CGC data are compared to those obtained with chiral shift 1H NMR.
    Additional Material: 2 Ill.
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  • 109
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 98-98 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 110
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 107-108 
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Polyacrylamide ; Hydrophobic interaction ; Electrokinetic chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 111
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 556-556 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 112
    ISSN: 0935-6304
    Keywords: HRGC-MS ; Thermal desorption ; Cryofocusing ; Air analysis ; Indoor and outdoor air ; Polar and non-polar hydrocarbon ; Volatile organic compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 113
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 607-608 
    ISSN: 0935-6304
    Keywords: Ion Chromatography, IC ; Interference ; Fluoride ; Carbonate ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
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  • 114
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 609-612 
    ISSN: 0935-6304
    Keywords: Capillary zone electrophoresis (CZE) ; Chiral separation ; Separation of enantiomers ; Acidic chiral compounds ; Dextrins ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 7 Ill.
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  • 115
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 647-650 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Ambient headspace ; Modified autosampler ; Residual organic volatiles ; Blood alcohol ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A GC autosampler designed for liquid injection was modified for static headspace sampling. The modification was very simple and involved replacement of the standard 10-μL syringe with a 100-μL gas-tight syringe. Liquid samples (0.2-1.0 mL) were placed in 2-mL vials, normally used for liquid sampling and an aliquot of the head-space above the liquid was withdrawn and injected into the GC. All parts of the sampling system were at ambient temperature. The system was found to be useful for several applications. Among those discussed in this paper are determination of ethanol in the blood or urine of individuals suspected of driving while intoxicated, residual organic solvents in pharmaceuticals, and screening of effluent waters from industrial plants for acrylonitrile.
    Additional Material: 3 Ill.
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  • 116
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 668-668 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 117
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 668-668 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 118
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 674-675 
    ISSN: 0935-6304
    Keywords: Large volume splitless injection ; Vapor overflow technique ; Batching oil from jute bags ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 119
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 120
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 792-794 
    ISSN: 0935-6304
    Keywords: Splitless injection of large volumes of water ; Vapor overflow technique ; Triazines ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Conditions were optimized for the introduction of large volumes of drinking water by splitless injection with vapor overflow, experimenting with the determination of triazines. No co-solvent was added, and the maximum injection volume was 400 μl. A vapor outlet beyond a coated precolumn was used to discharge water vapors released belatedly from the packing. Using alkali flame ionization detection (AFID), detection limits were around 0.5 μg/l.
    Additional Material: 4 Ill.
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  • 121
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 797-798 
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Semiconductor laser ; Fluorescence ; Captopril ; Derivatization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 122
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 801-802 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 123
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 124
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 814-820 
    ISSN: 0935-6304
    Keywords: Sulfur ; GC-AED ; Atmosphere ; Gases ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The atomic emission detector (AED) has been found to be a sensitive and selective instrument for analysis of atmospheric sulfur gases by capillary gas chromatography. It was possible to determine atmospheric dimethyl sulfide at concentrations below 0.3 nmol/m3 typical of the remote marine environment in winter. Sample analyses from the Australian Baseline Air Pollution Station, Cape Grim, are used to illustrate this.In comparison with other sulfur-specific detectors previously used for this work, the AED has been found to exhibit the best combination of specificity and sensitivity. A configuration comprising a series of valves, gas calibration loops, and a cryogenic trap prior to the GC-AED was used for sample analysis. Standard addition of sulfur hexafluoride was found to assist determination of carbonyl sulfide, as it could be used to take into account the magnitude of signal quenching from coeluting gases. The AED was also found to be a selective detector for the direct injection of water-soluble dimethyl sulfide oxidation products.
    Additional Material: 7 Ill.
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  • 125
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 827-830 
    ISSN: 0935-6304
    Keywords: HPLC ; Fluorimetric detection ; UV detection ; Proteins of animal origin ; Lysinoalanine ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This work suggests an HPLC method for qualitative and quantitative determination of Nε(2-amino-2-carboxyethyl)-L-lysine (LAL). LAL was released from total hydrolysates of various proteins of animal origin and derivatized with dansyl chloride. The performance of two different columns, Spherisorb 3S TG and μ-Bondapack C18, was compared; better resolution and quantitative response were obtained with the former. The mobile phase was a mixture of 0.01 M phosphate buffer (pH 7) and acetonitrile. Linear response and quantitative repeatability were tested for both detectors used (UV-Vis set at 254 nm; fluorimetric set at λex(max) = 360 nm and λem(max) = 525 nm).For LAL standard the minimum detectable amount was 0.05 ng, whereas for LAL in actual samples the amount was 0.5 ng (40 μg/g of analyzed proteins). Good analytical repeatability was obtained, resulting in CV % of 4.7 and 3.8 for UV and fluorimetric detectors, respectively. LAL recovery was determined using both detectors; the values obtained were 94 % (fluorimetric) and 92 % (UV). Greater noise levels were observed with the fluorimetric detector and its higher sensitivity could not, therefore, be fully utilized. The highest amounts of LAL were found in the casein (2816 μg/g) and cooked albumin (615 μg/g) samples.
    Additional Material: 3 Ill.
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  • 126
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 851-858 
    ISSN: 0935-6304
    Keywords: High resolution gas chromatography ; Chlorinated hydrocarbons ; Polychlorinated biphenyls ; PCB indicator congeners ; Coelution ; Toxic PCB congeners ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Eighty one polychlorinated biphenyls (PCBs) and nineteen chlorinated pesticide standards have been analyzed on a newly developed apolar high resolution gas chromatography (HRGC) column. Emphasis was placed on the determination of PCB indicator congeners which are part of national regulations, and of toxic coplanar PCB congeners.The new column enables almost unambiguous quantification of the PCB indicator congeners (PCB 138 can be separated from both PCB 163 and PCB 164; PCB 28 and PCB 31 were also separated and no coelution was observed for PCB 52, PCB 118, and PCB 180). The new column furnished better results than CP-Sil 8 for the analysis of PCB indicator congeners in a sample of seal blubber.
    Additional Material: 4 Ill.
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  • 127
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 839-850 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Chemometry ; Fourier analysis ; Multicomponent mixture chromatograms ; PCB analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Aroclor and Aroclor mixture chromatograms obtained using temperature programmed high resolution capillary GC coupled with mass spectrometric selective detection have been investigated by Fourier analysis developed for the study of multicomponent chromatograms. The experimental autocorrelation function (EACF), i.e. peak shape and position correlation, showed a retention - structure pattern which could be associated with both the type of Aroclor and the ion used for selective ion monitoring (m/z value). In particular, o-m and m-m isomerization effects were singled out by EACF analysis. By fitting EACF with previously developed theoretical models, it was possible to characterize a specific Aroclor in terms of the number of PCB congeners present in it. The results obtained agreed closely with the typical Aroclor content. For the Aroclor mixture, the distribution of inter-distance between successive peaks was derived. The two first distribution moments obtained agreed with those derived from retention data reported in the literature. The consequences on the separation performance, i.e. the number of singlets, doublets, etc. in the chromatogram, are discussed.
    Additional Material: 9 Ill.
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  • 128
    ISSN: 0935-6304
    Keywords: Enantioselective gas chromatography ; Cyclodextrin derivatives ; Polychlorinated pesticides ; Polychlorinated biphenyls (PCBs) ; Pyrethroid insecticides/Allethrin ; Organophosphorus pesticides/Acephate, Malaoxon ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The enantiomers of the polychlorinated polycyclic xenobiotics heptachlor, cis- and trans-chlordane, cis- and trans-heptachlorepoxide, oxychlordane, and bromocyclen have been resolved by gas chromatography with selectively substituted cyclodextrins. The order of elution of these compounds and of α-hexachlorocyclohexane (α-HCH) was determined by comparison with enantiomerically enriched reference compounds obtained by preparative enantioselective gas chromatography.A separation of the eight stereoisomers of the pyrethroid insecticide allethrin into seven peaks was achieved. Both trans-diastereomers were separated into their enantiomers and the order of elution could be determined by comparison with commercially available (S)-bioallethrin and trans-bioallethrin. Also one cis-diastereomer was separated, wheras the other cis-isomer could not be resolved. In addition 15 out of 19 stable atropisomeric polychlorinated biphenyls with 5, 6 and 7 chlorine substituents, some chiral organophosphorus pesticides, including acephate and malaoxon and the herbicide bromoacil were separated.
    Additional Material: 10 Ill.
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  • 129
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    Journal of High Resolution Chromatography 17 (1994), S. 867-867 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 130
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 868-868 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 131
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 759-764 
    ISSN: 0935-6304
    Keywords: Supercrirtical fluid extraction (SFE) ; Modified carbon dioxide in SFE ; Liquid trapping ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A polarity test mix consisting of acetophenone, N,N-dimethylaniline, naphthalene, 2-naphthol, and n-tetracosane was spiked onto sand and extracted with carbon dioxide modified with acetonitrile, methanol, or toluene. The extracts were collected in chloroform, hexane, methanol, or a mixed collection solvent consisting of equal parts chloroform-hexane-methanol. The mixed collection solvent which showed excellent recoveries for pure CO2, had the worst recoveries of all the collection solvents with modified CO2. Overall hexane was the best collection solvent studied for these analytes under these extraction conditions.
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  • 132
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    Journal of High Resolution Chromatography 17 (1994), S. 773-778 
    ISSN: 0935-6304
    Keywords: High performance liquid chromatography ; Amino-zirconia sorbents ; Carbohydrates ; Pulsed amperometric detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of non-porous, microspherical zirconia-based stationary phases with surface bound amine functionality have been introduced and evaluated in hydrophilic interaction chromatography (HILIC) of underivatized, neutral carbohydrates and anion exchange chromatography of nucleotides using pulsed amperometric detection and ultraviolet detection, respectively. Three aminopropyl alkoxysilane compounds were used in the surface modification of the non-porous zirconia support, namely 3-aminopropyltrimethoxysilane (monoamine), N-(2-aminoethyl)-3-aminopropyltrimethoxysilane (diamine), and trimethoxysilylpropyldiethylenetriamine (triamine). Due to the relatively low specific surface area of the non-porous zirconia support used in this study (ca. 7.3 m2/g), zirconia with surface coating of the triamine type yielded the best results as far as the separations of chitooligosaccharides and maltooligosaccharides are concerned. Since a non-porous zirconia could be readily modified with amine functionality via Zr—O—Si bonds, it is expected that all the three aminopropyl alkoxysilane compounds would yield satisfactory results with porous zirconia microparticles because of their much higher specific surface areas. Although the non-porous zirconia exhibited some limitations, the present study has demonstrated that microspherical zirconia particles are suitable supports for the production of polar sorbents for HILIC of carbohydrates. Another surface modification, which involved the activation of the zirconia surface with aldehyde groups followed by reductive amination with tetraethylenepentamine, was also evaluated. Although this chemistry would in principle yield sorbents with higher concentration in amine groups, the conversion of the majority of the primary amine groups of the tetraethyle-nepetamine molecules to secondary amine functions in the course of the reductive amination reaction have provided a stationary phase that did not afford satisfactory resolution for carbohydrates. However, this same stationary phase behaved as a weak anion exchanger and allowed the high resolution separation of nucleoside-5′-mono-, -di-, and triphosphates. Overall, the results obtained with zirconia-based hydrophilic sorbents paralleled those obtained on amino-silica bonded phases.
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  • 133
    ISSN: 0935-6304
    Keywords: Enantioselective gas chromatography ; Enantioselective supercritical fluid chromatography ; Immobilized chiral stationary phases ; Modified cyclodextrin ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Heptakis(2,6-di-O-methyl-3-O-pentyl) (2-O-methyl-6-O-oct-1-enyl-3-O-pentyl)-γ-cyclodextrin was immobilized to narrow-bore fused silica capillaries after selective modification. One tert-butyldimethylsilyl group was introduced into octakis-(2-O-methyl-3-O-pentyl)-γ-cyclodextrin in order to get a pure monofunctionalized cyclodextrin derivative. During synthesis the tert-butyldimethylsilyl group was replaced by an anchoring group to bind the cyclodextrin to a polysiloxane. After thermal immobilization of the modified polysiloxane this new chiral stationary phase was applied in GC and SFC. High efficiency separations were obtained in GC. In SFC very polar compounds could be chromatographed at low temperatures resulting in higher separation factors as compared to GC.
    Additional Material: 6 Ill.
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  • 134
    ISSN: 0935-6304
    Keywords: Block polysiloxanes ; Functionalized polysiloxanes ; Chiral polysiloxanes ; Enantioselective stationary GC phase ; Polysiloxane synthesis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Trifluoroethyl ester-functionalized polysiloxanes can be prepared by block condensation of 3-dichloromethylsilyl-2-methylpropionic acid 2′,2′,2′-trifluoroethyl ester with 1,5-bis(diethylamino)hexamethyltrisiloxane or with disodium tetramethyldisiloxane-1,3-diolate. The functionalized polysiloxanes may serve as supports for a variety of selector groups; for instance, nucleophilic displacements with L-valine-t-butylamide or L-α-naphthylethylamine lead to chiral polysiloxanes in high yields and with high reproducibility. Imidazole accelerates the rate of nucleophilic displacement. Capillary columns coated with such chiral polysiloxanes exhibit high enantioselectivity and thermostability.
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  • 135
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    Journal of High Resolution Chromatography 17 (1994), S. 4-8 
    ISSN: 0935-6304
    Keywords: Micellar electrokinetic capillary chromatography (MECC) ; Cationic micelles ; DNA photoproducts ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Micellar electrokinetic capillary chromatography has been explored as an efficient and rapid method of separating the photoproducts of 2′-deoxyuridylyl-(3′-5′)-thymidine (i.e., cis-syn and trans-syn cyclobutane dimers, (6-4) photoproduct, and the related Dewar valence isomer) from normal nucleosides and nucleotides. Three cationic surfactants, dodecyl-, tetradecyl-, and hexadecyltrimethy-lammonium bromide were evaluated and the separations compared with those obtainable with the anionic surfactant, sodium dodecylsulfate. Optimum resolution of the dinucleoside monophosphate photoproducts was obtained using tetradecyltrimethylammonium bromide. By use of this detergent the photoproducts could also be separated from other normal constituents in less than 6 min at -25 kV. Dodecyl- and hexadecyltrimethylammonium bromide provided some separation between the various species but sodium dodecylsulfate did not separate the UV radiation-induced products from either the parent compound or other dinucleoside monophosphates. Increased interaction between negatively charged solutes and positively charged micelles accounts for the differences.
    Additional Material: 4 Ill.
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  • 136
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    Journal of High Resolution Chromatography 17 (1994), S. 37-42 
    ISSN: 0935-6304
    Keywords: Deactivation of GC precolumns ; Water resistance of deactivation ; OV-1701 for deactivation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Deactivation of precolumns with an ultra thin film of OV-1701 provided inertness at least equal to silylation, but better resistance to water. Dynamic coating of the raw fused silica capillary is, furthermore, much faster than the hydrothermal treatment/silylation procedure.
    Additional Material: 3 Ill.
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  • 137
    ISSN: 0935-6304
    Keywords: Chiral stationary phase ; Carbon dioxide-based mobile phases ; Dynamic chiral chromatography ; Fullerenes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Fast and efficient separations of chiral stereolabile compounds were obtained at very low temperature on a π-acid chiral stationary phase (R,R-DACH-DNB) using carbon dioxide-based mobile phases containing alcoholic polar modifiers.Furthermore, efficient separations of the newly discovered spherical carbon cluster buckminsterfullerene (C60) and the related higher fullerenes (C70, etc.) have been performed on the same stationary phase using eluents based on either n-hexane or carbon dioxide.
    Additional Material: 6 Ill.
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  • 138
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    Journal of High Resolution Chromatography 17 (1994), S. 264-270 
    ISSN: 0935-6304
    Keywords: GC-MS ; Exhaust emissions ; Hydrocarbon emissions ; Photochemical smog ; Gasoline ; Spark-ignited engine ; Engine operating parameters, effect of ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reactivities of engine-out exhaust hydrocarbon (HC) emissions in photochemical smog formation have been determined for three fuels (isooctane, an aromatic blend, and a gasoline) in a single-cylinder, spark-ignited engine. High resolution capillary GC was used to determine the mole fractions of the exhaust hydrocarbon species. Temperature programmed chromatography on a single capillary column was sufficient to separate the major exhaust species. A library of approximately 160 hydrocarbon species was used to identify typically 90-95 % of the HC species present. GC-MS was used selectively to verify peak assignments.The effect of engine operating parameters (fuel-to-air ratio, spark timing, and speed) on reactivity was examined. Engine operating parameters affect both total emissions [g/mile] and the specific atmospheric reactivity [g ozone/g HC emissions] of these emissions. Changing the operating parameters to control total emissions may not be as effective as expected in controlling the total reactivity [g ozone/mile] of the emissions because the specific reactivity can also change simultaneously. Effects of changes in operating parameters differ significantly as the type of fuel is varied. The ability to measure exhaust hydrocarbon species emissions accurately and quickly will increase in importance as reactivity-based emissions standards come into widespread use.
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  • 139
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    Journal of High Resolution Chromatography 17 (1994), S. 390-397 
    ISSN: 0935-6304
    Keywords: On-line coupled LC-GC ; Fuel product analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A review of the analysis of petroleum fuels, oils, tars and engine exhaust particulate extracts by on-line coupled LC-GC is presented.
    Additional Material: 8 Ill.
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  • 140
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    Journal of High Resolution Chromatography 17 (1994), S. 415-426 
    ISSN: 0935-6304
    Keywords: GC/MS ; Petroleum ; Primary, secondary, and tertiary amines ; Ditrifluoroacetylation ; Trifluoroacetylation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An analytical method for differentiation of primary, secondary, and tertiary amines using exhaustive trifluoroacetylation prior to GC/MS has been developed. Using the conditions described in the report, most primary amines add two and secondary amines add one trifluoroacetyl group. In general, tertiary amines do not react. GC retention indices and relative GC/MS total ion current response factors for 102 trifluoroacetyl derivatives are reported. Examples of the application of the method to petroleum and coal liquid products are provided. Because of the limited thermal stability of the derivatives of primary amines, the method is applicable only to distillates boiling below 370 °C (700 °F).
    Additional Material: 7 Ill.
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  • 141
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    Journal of High Resolution Chromatography 17 (1994), S. 452-456 
    ISSN: 0935-6304
    Keywords: Coupled LC-GC ; Automation ; Diesel fuel analysis ; Group-type separation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Characterization of fuels by LC-GC is possible by use of automatic successive transfer (multiple transfer) of HPLC fractions to a GC via an on-column interface. This paper describes the instrumentation and the methodology for the HPLC separation of the hydrocarbons (aliphatic and aromatic) into separate groups and the on-line transfer of these groups to a capillary GC column. Two HPLC methods were used with the same valve configuration: single column (silica) with column back-flush to detector; and double column (silica and amino-bonded silica) with multiple fraction transfer and back-flush. The first method was used for the analysis of total saturated compounds and total aromatic compounds; the second was used for the separation of the one-, two-, three-, and four-ring aromatic compounds present in diesel fuels. Examples are shown of the characterization of diesel fuels, and the repeatability of the data.
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  • 142
    ISSN: 0935-6304
    Keywords: Capillary GC ; Petroleum crude oil ; Condensates ; Carbon number distribution ; Pseudocomponents ; Quality control ; Quality assurance ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A quality control scheme has been developed to achieve reproducible capillary GC characterization of crude oils and petroleum condensates. The method uses an internal standard to quantify the amount of non-eluted material in the crude oil sample. Correlation between the gas chromatographic results and actual distillation was 2 %. After repeated use, however, weekly analysis of the same standard crude oil did not give the correct composition. This was a result of discrimination, which worsened with time, as a result of leaks in the septum or the graphite ferrules. More reproducible results were obtained by performing frequent analyses of quality control samples to ensure that the gas chromatographic system was operating properly. The use of quality control charts was a convenient way of ensuring correct operation and identifying the need for corrective action on the gas chromatographic system.
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  • 143
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    Journal of High Resolution Chromatography 17 (1994), S. 503-504 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 144
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    Journal of High Resolution Chromatography 17 (1994) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 145
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Mass spectrometry ; Fatty acids ; 2-Substituted 4,4-dimethyloxazoline derivatives ; Lipids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Fatty acids from blood serum lipids and fish oil preparations are derivatized with 2-amino-2-methyl-1-propanol to form 2-substituted 4,4-dimethyloxazolines. The derivatives are separated on a 25 m × 0.25 mm FFAP column and identified by mass spectrometry using electron impact ionization. The positions of the double bonds of mono- and polyunsaturated fatty acids can be easily and reliably recognized from a characteristic fragmentation feature of the oxazolines. Several unsaturated C16 to C22 fatty acid isomers are identified whose exact structure has not been derived from the commonly used methyl esters.
    Additional Material: 3 Ill.
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  • 146
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    Journal of High Resolution Chromatography 17 (1994), S. 522-526 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Precolumns ; Solvent focusing ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In trace analysis by capillary GC it is often desirable to use larger than normal injection volumes to obtain sufficient sensitivity. This, however, results in a wider solvent peak and tailing, and may reduce column efficiency. This paper describes the use of a short length of a capillary precolumn coated with a stationary phase of polarity similar to that of the sample solvent and a film thickness greater than that of the analytical column; provided the right combination of polarities of injection solvent and liquid phases are used, the precolumn focuses the solvent band, thereby enabling the maximum injection volume to be increased without measurably reducing efficiency. Typical precolumn dimensions are 1 m length, 0.32 mm i.d., and 0.5 μm stationary phase film thickness. Using a precolumn increases the maximum injection volume up to 8 or 10 μl, or three times that appropriate for a conventional analytical column, with little or no loss in efficiency.
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  • 147
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    Journal of High Resolution Chromatography 17 (1994), S. 553-555 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Liquid - liquid extraction ; Vinegar ; Polyalcohol analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A capillary gas chromatographic method has been developed for the determination of glycerol, erythritol, arabitol, sorbitol, and inositol in vinegar. After addition of phenyl-β-glucopyranoside as internal standard, the sample was then dried and silylated. The analysis was performed both on the crude silylated sample and after liquid - liquid extraction. The repeatability of the two methods was evaluated on twenty three different types of vinegar and the extraction did not seriously affect the analysis. Extraction of the TMS-ethers enables elimination of a large number of interfering substances such as acids and polyphenols and so acts as a purification of the sample.
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  • 148
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    Journal of High Resolution Chromatography 17 (1994), S. 613-615 
    ISSN: 0935-6304
    Keywords: Glass capillary column ; Trifluoroacetylated cyclodextrin ; γ-Lactones ; δ-Lactones ; Routine quality control ; GC-MS ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 149
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    Journal of High Resolution Chromatography 17 (1994), S. 682-682 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 150
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    Journal of High Resolution Chromatography 17 (1994), S. 695-699 
    ISSN: 0935-6304
    Keywords: High resolution gas chromatography ; Sulfur chemiluminescence detection ; Chromatographic injection profile ; Gaseous injection ; Sulfur gases ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A one meter stainless steel capillary column coated with a 20μm film of polydimethylsiloxane was used to replace the Teflon gas sampling loop of a HRGC - flameless SCD system. This column trap was equilibrated with the gaseous sample and then purged with carrier gas while being sequentially, resistively heated in ten 10 cm sections. The sequential heating of the 10cm sections was timed such that the velocity of the moving heated zone was approximately the same as the velocity of the carrier gas. The thick stationary phase film served to retard the front end of the injection band while the ballistic heating accelerated the back end. The net result was focusing of the injection, which gave rise to a narrower injection profile than that obtained with the original Teflon loop.
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  • 151
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 152
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    Journal of High Resolution Chromatography 17 (1994), S. 53-55 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 153
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    Journal of High Resolution Chromatography 17 (1994), S. 49-50 
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography ; Automated injection ; Solvent venting ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 154
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    Journal of High Resolution Chromatography 17 (1994) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 155
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    Journal of High Resolution Chromatography 17 (1994), S. 57-57 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 156
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    Journal of High Resolution Chromatography 17 (1994), S. 784-791 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Polychlorinated biphenyls ; Electronic pressure programming ; Experimental design ; Optimization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The applicability of electronic pressure control and Taguchi L27 experimental design to the optimization of the gas chromatographic separation and detection of polychlorinated biphenyls has been evaluated. The influence of several experimental variables, column temperature program, carrier gas pressure program, on-column injector temperature program, and make-up gas pressure program, was studied using analysis of variance. Simultaneous optimization of sample introduction, column efficiency, and detector performance could be achieved without compromising system performance. The relationships between system performance and experimental variables were established using regression analysis. Agreement between the simulated and experimental results obtained using suggested optimum conditions demonstrated the applicability of the technique developed in this study. The improvement achieved in the chromatographic separation of PCBs is presented.
    Additional Material: 6 Ill.
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  • 157
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Atomic emission detection (AED) ; Programmed temperature vaporization (PTV) ; Nitro musks ; Human adipose tissue ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Atomic emission detection (AED) has been successfully applied to the determination of nitro musks in the fat of human adipose tissue by gas chromatography at trace concentration levels. Element specific detection with the AED combined with a clean-up procedure for nonpolar substances makes target screening analysis for lipophilic nitro aromatic compounds possible for the first time. The lack of sensitivity, especially in the AED nitrogen and oxygen trace, was compensated by higher concentration of the extracts and injection of larger sample volumes performed by cold programmed temperature vaporization (PTV) in the solvent split mode. The combination of the superior quantification properties of the atomic emission detector with large sample volume introduction makes the quantification of nitro musks down to the ppb level possible. All five nitro musks investigated exhibit linear dynamic ranges going down close to instrumental limits of detection. Moreover, organochlorine compounds could be sensitively detected in the same sample extract by the AED chlorine trace without any interferences from coeluting matrix compounds.
    Additional Material: 7 Ill.
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  • 158
    ISSN: 0935-6304
    Keywords: GC-AED ; High boiling PAC ; Peak splitting in discharge tube ; Additional make-up gas ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Peak splitting of high molecular weight polycyclic aromatic compounds originating from the microwave plasma of an atomic emission detector (AED) coupled to a GC has been described and evaluated. The influence of the solute structure, solute concentration, and physical conditions in the AED (such as detector temperature, make-up gas flow, concentration of reagent gases and distance of column end from the plasma) have been studied. An explanation is presented for peak splitting, which is based on an insufficient solute decomposition and solute mass flow in the discharge tube. Modification of the instrument by introduction of additional make-up gas applied through the transfer line has been shown to improve peak shape and solute response.
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  • 159
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    Journal of High Resolution Chromatography 17 (1994), S. 153-159 
    ISSN: 0935-6304
    Keywords: Capillary GC-MS ; Purge and trap GC-MS ; Extraction ; Solid phase extraction ; Fractionation ; Organic contaminants in municipal wastewater ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: High resolution capillary gas chromatography-mass spectrometry has been used in combination with various sample preparation methods to analyze a wide range of low molecular weight organic contaminants in municipal wastewaters. Volatile organic compounds were extracted using a purge and trap concentrator connected directly to a wide bore DB-624 capillary column. Because of the high organic load in wastewater samples, this method was preferred to the more sensitive closed loop stripping technique which suffered from competition effects and insufficient adsorbent capacity. Volatile and semi-volatile base/neutral compounds and acids were extracted with dichloromethane at pH 11 and pH 2, respectively, or were recovered using a simultaneous distillation-extraction procedure. Acidic compounds were subsequently derivatized using diazomethane methylation. Both fractions were separated with a 30m DB-5ms capillary column. Specific ionic substances (LAS, NTA, EDTA) were isolated by solid-phase extraction then derivatized with diazomethane (LAS) or acetyl chloride in n-butanol (NTA, EDTA) before GC-MS analysis.This array of techniques enabled the identification of more than 150 organic contaminants in the influent of a municipal wastewater treatment plant in northern suburban Paris. The individual concentrations of these contaminants ranged from 〈 0.1 μg/l to 5.7 mg/l.
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  • 160
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    Journal of High Resolution Chromatography 17 (1994), S. 169-173 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 161
    ISSN: 0935-6304
    Keywords: Nonaqueous solvent ; Capillary electrophoresis ; CE-electrospray-mass spectrometry ; Drug metabolism ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 162
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    Journal of High Resolution Chromatography 17 (1994), S. 184-186 
    ISSN: 0935-6304
    Keywords: Chiral capillary GC ; Linalyl acetate ; Bergamot ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 163
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    Journal of High Resolution Chromatography 17 (1994) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 164
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    Journal of High Resolution Chromatography 17 (1994), S. 197-202 
    ISSN: 0935-6304
    Keywords: GC and GC-MS ; HPLC ; SFC ; TLC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Practically all the conventional chromatographic techniques are used in the characterization of the highly complex mixtures of organic compounds occurring in fuels, heavy fractions, and crude oils. This paper surveys the techniques employed for class determination, preparative fractionation of the main classes, and determination of subgroups after class fractionation.
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  • 165
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    Journal of High Resolution Chromatography 17 (1994), S. 217-222 
    ISSN: 0935-6304
    Keywords: Size exclusion chromatography ; Gas chromatography - atomic emission detection ; Sample pretreatment ; Metalloporphyrins ; Crude oil ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Size exclusion chromatography (SEC) has been demonstrated to be an effective and reproducible sample pretreatment procedure for removal of heavy oil matrices prior to GC-AED analysis of metalloporphyrins, and for the resolution of volatile metal species into clean and defined fractions. This paper also discusses the results obtained by SEC for determination of the distribution of metallopor-phyrins in crude oils and the correlation between total metal, metal-loporphyrin, and total distillable metal content.
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  • 166
    ISSN: 0935-6304
    Keywords: Nitrogen compounds ; Alkylcarbazoles ; Analytical TLC ; Oil migration ; Crude oils ; Petroleum source rocks ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The results are reported of a range of laboratory chromatographic fractionation experiments with synthetic model compounds and a petroleum pyrrolic nitrogen fraction. Reversed phase separation of pyrrolic nitrogen compounds was governed mainly by the number of carbon atoms in the molecule, with little selectivity toward different positional isomers, whereas normal phase separation of the compounds could be explained in terms of steric effects related to alkylation position. Comparison of experimental results from model compounds with observations made previously using sets of natural samples taken from sedimentary basins clearly suggests adsorptive interactions between organic and mineral phases are involved in the compositional fractionation of pyrrolic nitrogen compounds in petroleum during migration. Detailed studies of the effects of petroleum migration on the molecular distribution of petroleum pyrrolic nitrogen compounds may provide useful, quantifiable, migration-related geochemical parameters.
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  • 167
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    Journal of High Resolution Chromatography 17 (1994), S. 501-502 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 168
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    Journal of High Resolution Chromatography 17 (1994), S. 504-504 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 169
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    Journal of High Resolution Chromatography 17 (1994), S. 509-518 
    ISSN: 0935-6304
    Keywords: Liquid - solid disk extraction ; Gas chromatography (GC) ; Phenols ; Supercritical fluid extraction (SFE) ; Water ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method combining the techniques of liquid - solid disk extraction (LSDE) and supercritical fluid elution (SFE) has been developed for the phenols regulated by the Clean Water Act. LSDE uses a disk or membrane made of polytetrafluoroethylene (PTFE) fibrils impregnated with small particles, e.g. styrene divinylbenzene (SDB) resin, to extract phenols from water. After disk extraction the retained analytes are eluted from the disk using SFE. SFE is used as an alternative to liquid solvent elution with an organic solvent. Analytes are separated, identified, and quantified using gas chromatography - ion trap detector mass spectrometry (GC-ITDMS). The method is capable of sub parts per billion detection limits, and precision of 5-28% RSD. Evaluation of various disks or membranes, such as C18-silica disks, SDB disks, and ion exchange membranes, has also been performed for the extraction of phenols from water. The results obtained from the in-situ aqueous acetylation of phenols and extraction of their acetates are quantitative. The utilization of LSDE and SFE techniques has proven to be a more effective approach than liquid - liquid extraction in minimizing air pollution and solvent waste.
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  • 170
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Atomic emission detector ; Organotin compounds ; Organolead compounds ; Organomercury compounds ; Grignard derivatization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: As part of a continuing evaluation of new analytical and sample preparation techniques conducted by the US Environmental Protection Agency (EPA), the use of capillary gas chromatography with atomic emission detection (GC-AED) for the simultaneous determination of organotin, organolead, and organomercury compounds in environmental samples was investigated. Pentylmagnesium bromide was used to pentylate ionic organotin, organolead, and organomercury compounds; the pentyl derivatives were then separated by GC and determined by AED. Several important GC-AED parameters, including the type of injector inlet, carrier gas flow rate, and helium make-up gas flow rate, were optimized for the simultaneous determination of these organometallic compounds. Their minimum detectable concentrations were approximately 1.0 to 2.5 ng/mL using a 0.5-μL on-column injection. The calibration curves exhibited good linearity between 2.5 and 2500 ng/mL for organotin and organolead compounds, and between 2.5 and 10000 ng/mL for organomercury compounds.
    Additional Material: 5 Ill.
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  • 171
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    Journal of High Resolution Chromatography 17 (1994), S. 549-552 
    ISSN: 0935-6304
    Keywords: GC/MS ; Crude oils ; Monoaromatic steroids ; Triaromatic steroids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Series of C-ring monoaromatic steroid hydrocarbons (C21, C22, C27 — C29) and triaromatic steroid hydrocarbons (C20, C21, C26 — C28) have been recognized in the aromatic hydrocarbon fraction of Alamein crude oil from the western desert, Egypt. Detection of these compounds were based on mass fragmentography of the key ions m/z 253 and m/z 231 and comparison of the mass spectra and relative retention times with literature data. The predominance of the C29 monoaromatic steroids and C28 triaromatic steroids provide further evidence for a land plant origin of Alamein oil. The results substantiate previous evidence of the occurrence of an aromatization process with increasing maturation and indicate a moderate maturity level for Alamein oil.
    Additional Material: 5 Ill.
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  • 172
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    Journal of High Resolution Chromatography 17 (1994), S. 190-190 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 173
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    Journal of High Resolution Chromatography 17 (1994), S. 567-568 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 174
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    Journal of High Resolution Chromatography 17 (1994) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 175
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    Journal of High Resolution Chromatography 17 (1994), S. 593-596 
    ISSN: 0935-6304
    Keywords: High Temperature Gas Chromatography (HTGC) ; Bis(trimethylsilyl)trifluoroacetamide ; Ethoxylated alcohols ; Ethoxylated alcohol sulfates ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Conversion of ethoxylated alcohols to trimethylsilyl derivatives and subsequent high temperature gas chromatography allowed for the determination of alkyl chain distribution, mole average degree of ethoxylation and weight percent distribution of several commercial mixtures. Repetitive derivatizations and analyses of a mixture with a vendor specified mole average degree of ethoxylation of 3.0 (Neodol 23-3), yielded an experimental result of 2.93 ± 0.05 (n = 6). Mixtures with different alkyl chain distributions and higher degrees of ethoxylation provided similar accuracy. Extension of the method to the analysis of ethoxylated alcohol sulfate raw materials and ethoxylated alcohol sulfates in dishwashing liquids is discussed.
    Additional Material: 6 Ill.
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  • 176
    ISSN: 0935-6304
    Keywords: Enantioselective GC ; Permethyl-β-cyclodextrin ; Cyclopropyl amino 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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  • 177
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    Journal of High Resolution Chromatography 17 (1994), S. 621-621 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 178
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    Journal of High Resolution Chromatography 17 (1994), S. 623-624 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 179
    ISSN: 0935-6304
    Keywords: Microwave cavity ; Post-column derivatization ; Carboplatin ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
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  • 180
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    Journal of High Resolution Chromatography 17 (1994), S. 303-307 
    ISSN: 0935-6304
    Keywords: High resolution gas chromatography ; Unsaponifiable coffee fraction ; Coffee diterpenic alcohols ; Robusta coffee determination ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The unsaponifiable lipid fractions extracted from Arabica and Robusta coffee samples were analyzed by high resolution gas chromatography (HRGC) in a polar column with a thermally stable stationary phase (TAP, Chrompack). Certain characteristic ratios among diterpenic alcohols were found to permit measurement of the amount of Robusta blended with Arabica coffee, given a minimum content of 5-10%. Determination does not appear to be influenced by geographic origin of produce or even by decaffeination.
    Additional Material: 3 Ill.
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  • 181
    ISSN: 0935-6304
    Keywords: Headspace Gas Chromatography ; Water ; Soil ; Halogenated hydrocarbons ; Aromatic hydrocarbons ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Volatile aromatic and halogenated hydrocarbons are determined in water and soil samples by equilibrium headspace gas chromatography. Simultaneous analysis is carried out in a dual column/dual detector arrangement with ECD and PID. Their determination in contaminated soil is performed with the same instrumental configuration. However, in contrast to water analysis, an increased sample temperature was found necessary for highly adsorptive soil specimens. At sample temperatures of 95 °C, recoveries near 100% have been found. Both adsorption and desorption processes were found to be strongly time-dependent.
    Additional Material: 5 Ill.
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  • 182
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    Journal of High Resolution Chromatography 17 (1994), S. 312-314 
    ISSN: 0935-6304
    Keywords: Automated on-line HPLC-HRGC ; Sweet orange oil ; Aliphatic aldehydes ; Monoterpene aldehydes ; Sesquiterpene aldehydes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The application of a new method, computer-controlled on-line HPLC-HRGC, to the analysis of the components of sweet orange oil has enabled the determination of aldehydes without interferences. HPLC was used to separate the oil aldehydes into three fractions, aliphatic aldehydes, sesquiterpene aldehydes, and monoterpene aldehydes. These fractions were transferred automatically to the GC, where the individual aldehydes were separated into well resolved chromatographic peaks.
    Additional Material: 3 Ill.
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  • 183
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    Journal of High Resolution Chromatography 17 (1994), S. 325-334 
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Repeatability of electroosmotic flow ; Silica capillary tubes ; Column pretreatment ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The influence of a number of factors, such as the nature of the buffer, the presence of additives therein, the manufacturing conditions, and the pretreatment of the capillary, on the magnitude and repeatability of the electroosmotic flow (EOF) in silica capillary tubes has been investigated. It was established that the nature of the buffer plays the most significant role in respect of the stability and magnitude of EOF, whereas the conditions used for manufacture and pretreatment of the tubing are less important. The EOF obtained using buffers consisting of tris(hydroxymethyl)aminomethane and ethylenediamine was more repeatable than that obtained using pure phosphate buffers. Buffer additives such as sodium dodecylsulfate, 1-butanol, sodium salts of 1-pentanesulfonic acid and 1-heptanesulfonic acid, altered the magnitude of the EOF only, not its repeatability.
    Additional Material: 8 Ill.
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  • 184
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    Journal of High Resolution Chromatography 17 (1994), S. 343-346 
    ISSN: 0935-6304
    Keywords: High performance thin layer chromatography ; Platinum metal 8-hydroxyquinolinates ; Polar stationary phases ; Retention, effect of mobile phase ; Sample preparation ; Optimization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: High performance thin layer chromatography has been used to separate all the platinum metal 8-hydroxyquinolinates on polar stationary phases. The dependence of Rf values on the composition of mobile phases prepared from chloroform - tetrahydrofuran or chloroform - alcohol mixtures has been investigated. Retention was found to be partially dependent on alcohol chain length in chloroform - alcohol systems. The results obtained from TLC are dependent on the method of sample preparation used for the analyte.
    Additional Material: 7 Ill.
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  • 185
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    Journal of High Resolution Chromatography 17 (1994), S. 350-352 
    ISSN: 0935-6304
    Keywords: Supercritical fluid extraction ; Supercritical fluid derivatization ; C18 adsorbent ; Capillary GC ; Polar compounds ; Phenoxycarboxylic 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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  • 186
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    Journal of High Resolution Chromatography 17 (1994) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 187
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    Journal of High Resolution Chromatography 17 (1994), S. 373-389 
    ISSN: 0935-6304
    Keywords: GC ; Natural gas analysis ; Sulfur components ; Selective enrighment ; Sulfur selective detection ; Calibration ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: More stringent environmental regulations as well as higher demands presently being imposed on the sulfur content of natural gas feed-stocks for chemical processes necessitate the development of new analytical procedures for sulfur determination in natural gas. Only analytical procedures based on gas chromatography can meet the sensitivity and accuracy requirements dictated by environmental regulation institutions and modern chemical industry. The complexity of the natural gas matrix as well as the extremely low concentration levels at which the sulfur species occur make the development of these analytical methods a true challenge. In this review the three steps common for analytical methods for trace analysis in complex matrices, i.e. pretreatment, chromatographic separation, and detection, are discussed in detail. Possible methods for calibration of the system are discussed in the final section.Various techniques to determine sulfur in natural gas are described. Depending on the application, the most suitable system has to be selected. For example, for on-line application in a hazardous area a simple and rugged system is required, i.e. a simple gas chromatograph with a flame photometric detector, while for laboratory application a more complex instrument including preconcentration, column switching, and more exotic detection systems could be more suitable. Therefore it is crucial to define the requirements of the instrument at an early stage and use the information in this review article to develop/select a dedicated instrument/procedure for the problem at hand.
    Additional Material: 17 Ill.
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  • 188
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    Journal of High Resolution Chromatography 17 (1994), S. 398-406 
    ISSN: 0935-6304
    Keywords: High temperature GC ; Pyrolysis ; Hydrocarbons ; Waxes ; High molecular weight hydrocarbons (C40—C100) ; Asphaltenes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: For the past two or three decades geochemists have been concerned with the analyses and characterization of compounds, generally hydrocarbons, ranging from C1—C40. Significant amounts of information have resulted from these studies which have been extremely useful in many geochemical and environmental studies. However, in the past two or three years the commercial development and availability of high temperature gas chromatography columns has lead to the investigation of the occurrence and distribution of high molecular weight hydrocarbons (HMWHC), and other compounds, in the carbon number range C40—C100, present in oils, waxes, bitumens and rock extracts. The ability to study these compounds represents a major advance in organic geochemistry. In some samples these compounds may represent the bulk of the organic components but prior to development of the high temperature columns it was impossible to study their distributions.This paper will review advances that have occurred in terms of the application of high temperature gas chromatography (HTGC) to the analyses of fossil fuel samples and discuss the possible origin and significance of these compounds that have been identified. In addition, some of the potential problems involved in the analyses of these compounds will also be discussed.
    Additional Material: 5 Ill.
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  • 189
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    Journal of High Resolution Chromatography 17 (1994), S. 439-451 
    ISSN: 0935-6304
    Keywords: Analysis of phenolic compounds ; Trifluoroacetate esters of phenols ; Polycyclic hydroxyaromatics ; Dihydroxyaromatics ; Petroleum and synfuels ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The GC-MS characteristics of trifluoroacetate esters of phenolic compounds are discussed. Linear temperature programmed retention indices and total ion current MS response factors of over 120 phenolic esters are reported.The main GC advantages from analysis of trifluoroacetate esters as compared to plain phenols are enhanced volatility and improved resolution. For example, the elution temperature of a given phenol is typically 50 °C greater than that of the corresponding trifluoroacetate ester. Also, while retention of compounds with two trifluoroacetate groups is only moderately greater than mono esters, underivatized dihydroxy compounds are very difficult to elute from any GC column. Complete resolution of isomeric C0-, C1- and C2-alkylphenol esters is readily achieved on conventional fused silica GC columns; resolution of the corresponding underivatized compounds requires specialized GC columns with low temperature limits.In general, mass spectra of trifluoroacetate esters are more characteristic of a given structure than those of the corresponding phenols and may be more rigorously interpreted towards structural elucidation. A table in the report summarizes some of the more important spectral features used in compound identification.Example applications in analysis of coal-, shale- and petroleum-derived materials are presented. Selected ion monitoring is used to determine individual phenolic components in whole distillates; reconstructed ion chromatograms are used to illustrate distributions of selected species as a function of fuel storage and thermal stress.
    Additional Material: 8 Ill.
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  • 190
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    Journal of High Resolution Chromatography 17 (1994), S. 457-462 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Flame photometric detector ; Pyrolyzer ; Sulfur boiling point distribution ; Light cycle oils ; Exponential dilution flask ; Low sulfur diesel ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method has been developed to determine the boiling point distribution of sulfur compounds in light cycle oils (LCO'S). The method chosen for this analysis was GC with a flame photometric detector (FPD) and pyrolyzer. Tests were carried out to evaluate the recovery efficiency, repeatability, and accuracy of the method. Repeatabilities within 2% were obtained. The recovery of benzothiophenes and dibenzothiophenes was close to 100%; this was important because these are the major sulfur components in LCO's. No hydrocarbon or solvent interferences were observed with the use of the pyrolyzer, even for a 95% solvent level. Comparison with results from other techniques showed that the method accurately determined the levels of sulfur compounds in the LCO boiling point range.
    Additional Material: 10 Ill.
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  • 191
    ISSN: 0935-6304
    Keywords: Isotope ratio monitoring-Gas Chromatography-Mass Spectrometry (irm-GC-MS) ; Compound specific isotope analysis (CSIA) ; Pyrolysis ; Stable carbon isotopes ; Kerogen ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This study describes the application of isotope ratio monitoring gas chromatography- mass spectrometry (irm-GC-MS) for compound-specific stable carbon isotopic analysis of aliphatic hydrocarbon and phenolic products from flash pyrolysis (800 °C, 20s) of natural biopolymers and sedimentary kerogens. As part of this work, we provide a detailed description of the analysis of complex samples, including approaches for peak integration, data handling and correction for derivative carbons. Several aliphatic and aromatic biopolymers are analyzed by irm-GC-MS in order to establish relationships between the isotopic signatures of pyrolysis products and those of their parent macromolecules. We also analyze a select group of kerogens and kerogen precursors of different ages and biopolymer compositions to evaluate the applicability of combined pyrolysis/irm-GC-MS to complex geochemical mixtures. Our findings suggest that, in spite of the wide degree of heterogeneity, the isotopic values of individual aliphatic and phenolic pyrolysis products determined by irm-GC-MS can be related to the isotopic composition of the total organic carbon in kerogens and used to trace its biological sources. This study also highlights the need for optimum chromatographic separation in order to fully realize the potential of compound specific isotope analyses.
    Additional Material: 10 Ill.
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  • 192
    ISSN: 0935-6304
    Keywords: Crude oils ; Organic sulfur ; Desulfurization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Five crude oils with varying sulfur contents (0.1 - 4.7%) were characterized on a molecular level for organically-bound sulfur. Aromatic fractions were analyzed by GC-(MS) and asphaltene and polar fractions were analyzed by flash pyrolysis-GC-(MS). The polar fractions were also desulfurized with Raney Ni and the hydrocarbons formed were analyzed by GC-MS. Major sulfur compounds in the aromatic fractions were identified as alkylbenzo- and alkyldiben-zothiophenes. The flash pyrolyzates of the asphaltene contained alkylthiophenes and alkylbenzothiophenes as major compounds, depending on the thermal maturity of the oil. Generally, the sulfur-rich crude oils contained relatively more sulfur compounds. The flash pyrolyzates of polar fractions contained a variety of sulfur compounds (alkylthiolanes, alkylthianes, terpenoid sulfides, alkylbenzothiophenes) with substantial differences between different crude oils. Raney Ni desulfurization of the polar fraction yielded hydrocarbons dominated by n-alkanes, but isoprenoid alkanes, n-alkylcyclohexanes, mid-chain methylalkanes, tricyclic terpanes, hopanes and steranes were also present. These hydrocarbons show a potential to fingerprint crude oils since their distribution patterns are more characteristic than those of the hydrocarbons present in the saturated hydrocarbon fraction.
    Additional Material: 15 Ill.
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  • 193
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    Journal of High Resolution Chromatography 17 (1994), S. 537-542 
    ISSN: 0935-6304
    Keywords: Metal-ammonia complexes ; Electroosmosis ; Field strength ; Diuretics ; Resolution ; Capillary length ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The counter ion in CZE separation systems affects resolution, effective field strength and electroosmosis. Alkali metals (lithium, sodium, potassium, and cesium), the ammonium ion, and several complexes of metals with ammonia ([Ag(NH3)2]+, [Cu(NH3)4]2+, [Zn(NH3)4]2+, [Cd(NH3)4]2+, [Ni(NH3)6]2+, and [Co(NH3)6]2+) have been studied for their effect on the separation of diuretics. With the alkali metals the electroosmotic flow velocity decreased and the effective field strength and resolution increased as the hydrated radius of the alkali metal decreased.All the metal-ammonia complexes except that with silver greatly reduced the electroosmotic flow velocity (Veo) and had only a slight effect on the effective field strength (Eeff). Because these complexes had a negligible effect on the ionic strength of the buffer, they enabled high separating power to be maintained during the separation, and hence the use of more energy in the separation system. This yielded better resolution of the compounds, but the analysis time was then compromised.A simultaneous reduction in capillary length and Veo while maintaining the high voltage enabled increased resolution without an increase in analysis time. The ability to control Veo by adding small concentrations (〈 100 μM) of metal complexes to the buffer solution makes it possible to adjust the analysis time and capillary length independently while employing high separation power.
    Additional Material: 5 Ill.
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  • 194
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    Journal of High Resolution Chromatography 17 (1994), S. 603-606 
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography ; Lanthanide β-diketonates ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The chromatographic behaviors of lanthanide chelates of acetylacetone (ACAC), trifluoroacetylacetone (TFA), thenoyltrifluoroacetone (TTA), dipivaloylmethane (THD), 6,6,7,7,8,8,8-heptafluoro-2,2-dimethyl-3,5-octanedione (FOD), and the thenoyltrifluoroacetonepyridine (TTA·Py) adduct were investigated using packed column supercritical fluid chromatography. Mobile phases consisting of neat and alcohol modified CO2 were used with a phenyl packed stationary phase. Lanthanide complexes of ACAC, THD, and FOD were shown to have better chromatographic performance compared to the corresponding chelates with TFA, TTA, and TTA·Py. In particular, TTA complexes such as Eu(TTA)3 showed characteristic thermal decomposition in the mobile phase at elevated temperature. In addition, retention behavior was found to be a temperature dependent function of volatility and solubility for all chelates studied.
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  • 195
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    Journal of High Resolution Chromatography 17 (1994), S. 616-618 
    ISSN: 0935-6304
    Keywords: HPLC ; MEKC ; Diode-array detection ; Flavonoid analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 5 Ill.
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  • 196
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    Journal of High Resolution Chromatography 17 (1994), S. 622-622 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 197
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    Journal of High Resolution Chromatography 17 (1994) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 198
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    Journal of High Resolution Chromatography 17 (1994), S. 643-646 
    ISSN: 0935-6304
    Keywords: High Resolution Capillary GC ; High Resolution GC-MS ; Lemon oil ; Citrus volkameriana ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The dependence of the limonene content of lemon (Citrus volkameriana) peel oil on the degree of ripeness of the fruit has been studied by using steam distillation and cold pressing to extract the oils from lemon fruit peel at different stages of maturation (green, greenish-yellow, and yellow-orange peel coloration). Samples of essential oils were analyzed by high resolution GC and GC-MS, using tetradecane as internal standard for quantitation. Forty components were detected; thirty eight were positively identified by comparison of their mass spectra (El, 70 eV) and Kováts retention indexes (determined using a non-logarithmic scale on capillary columns coated with both polar (DB-Wax) and non-polar (DB-1) stationary phases) with those of standards and with data reported in the literature. The limonene concentration reached a maximum level of 79.4% when the fruit was in the intermediate maturation stage characterized by greenish-yellow coloration.
    Additional Material: 4 Ill.
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  • 199
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    Journal of High Resolution Chromatography 17 (1994), S. 639-642 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Chiral stationary phase ; Chirasil-Val ; Cyclodextrins ; Perfluoroacylation ; Enantiomeric separation ; Amino alcohols ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Racemic amino alcohols have been separated as perfluoroacylated derivatives by gas chromatography using either improved Chirasil-Val or heptakis(2,6-di-O-methyl-3-O-pentyl)-β-cyclodextrin as stationary phase. Using Chirasil-Val all the amino alcohols investigated were separated to baseline (α values between 1.03 and 1.08) whereas only a few amino alcohols were resolved on the modified cyclodextrin column. The enantioselectivity obtained on the latter phase was, however, significantly higher.The separations were performed as trifluoroacetyl, pentafluoropropionyl, and heptafluorobutyryl derivatives and the chiral discrimination observed for the different derivatives was significantly different for both stationary phases.In oder to obtain a better understanding of the separation mechanism, the Gibbs-Helmholtz parameters Δ(R,S)ΔH° and Δ(R,S)ΔS° were determined. The most extraordinary result was obtained for the trifluoroacetyl derivative of allo-threoninol. In addition to the order of elution of the enantiomers being the opposite of that for the other compounds, the separation seems to be entropy controlled (the sign Δ(R,S)ΔH° is positive), i.e. the separation improved at higher temperatures.
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  • 200
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 662-664 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Sorbent cartridge ; Medium-chain fatty acids ; Fatty acid ethyl esters ; Beer analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A modification of a procedure by Hage [1] is proposed for the gas chromatographic evaluation of the content of free medium-chain fatty acids and related ethyl esters in beer. The method involves extraction of free fatty acids and ethyl esters by SPE using C18 bonded phase columns, derivatization of free fatty acids and related ethyl esters with diazomethane, and GC analysis using an SP-2340 capillary column. The results obtained have shown the method to be rapid and highly reproducible. The technique has been compared with other methods used for determination of free fatty acids.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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