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  • 1985-1989  (943)
  • 1890-1899
  • 1986  (943)
  • 1898
  • Analytical Chemistry and Spectroscopy  (943)
  • 101
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 35-38 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary columns ; Quantification ; Uremia ; Steroid metabolites ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Neutral steroid metabolites enriched from urine and hemofiltrate were identified by gas chromatography/mass spectrometry and quantified by capillary gas chromatography. This study included 20 healthy controls and 37 uremic patients. Before enrichment of steroids from biological material, the standard deviation of the workup procedure and subsequent derivatization into the trimethylsilyl-enol-trimethylsilyl ethers was tested and found to be 2-5% in urine and 12-17% in the more complicated workup procedure of hemofiltrate, but essentially smaller than the biological standard deviation. Compared to the 24 h urinary excretion rates of controls, the excretion rates of androsterone, etiocholanolone, and corticoid metabolites were significantly lower in uremic body fluids, while those of 11-oxygenated androstanolones, degradation products of corticoids, were enhanced in uremic urine. The ratio of corticoid metabolites to 11-oxygenated androstanolones in urine of nondialyzed uremics correlated significantly with their plasma creatinine levels.
    Additional Material: 3 Ill.
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  • 102
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 49-56 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary, columns ; Wide and narrow bore ; Cyanosilicone coatings ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The preparation of wide bore (320 μm) and narrow bore (50 μm) fused silica capillary columns is described for immobilized cyanopropyl substituted silicones containing 60 and 88% substitution. The effect of high temperature deactivation with cyanopropylcyclosiloxanes was studied with a special test mixture. Curing was achieved with dicumyl peroxide or azo-tert-butane.The columns were evaluated and compared in terms of efficiency, activity, polarity, and temperature stability. Different coating methods were compared for the narrow bore columns. The activity of the 60% cyanopropyl columns that had been immobilized with dicumyl peroxide was significantly larger than for azo-tert-butane immobilized columns. The polarity of polar columns appeared to depend greatly on column temperature and is completely different for wide and narrow bore columns.
    Additional Material: 10 Ill.
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  • 103
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 64-64 
    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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  • 104
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 252-254 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Post-column derivatization reaction ; Fluorogenic reaction ; Haloperidol ; N1-Methylnicotinamide chloride ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 5 Ill.
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  • 105
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 407-408 
    ISSN: 0935-6304
    Keywords: Planar liquid chromatography ; Overpressured layer chromatography ; Red peppers ; Quality control ; Carotenoids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 106
    Electronic Resource
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 412-414 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Zanthoxylum tessmannii (Engl.) Ayafor ; Amides ; Terpene hydrocarbons ; Alkaloids ; Medicinal plant ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 107
    Electronic Resource
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 419-420 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Ligand exchange ; Uracil derivatives ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 108
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 314-316 
    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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  • 109
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 312-313 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Fused silica capillary micro-packed columns ; Open tubular columns ; Sample capacity ; Trace analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 110
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 320-327 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Electron capture detector, ECD ; Electron capture sensitization ; Polynuclear aromatic hydrocarbons ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The electron capture detector (ECD) response to numerous aromatic hydrocarbons of low electron affinity (EA) is shown to be detrimentally affected by two processes which compete with and typically overwhelm the electron capture reactions of these molecules. It is shown that the effects of these two undesired reactions can be eliminated by the permanent addition of trimethylamine and one of several alkyl monochlorides to the detector make-up gas. These modifications of the detector gas result in greatly increased sensitivity, increased linearity, and increased reproducibility of response. A kinetic model for the ECD responses of low EA resonance capture molecules is developed which appears to explain these improvements.
    Additional Material: 7 Ill.
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  • 111
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 472-474 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Distilled-in-glass methylene chloride ; Environmental water analysis ; Sample preparation solvent ; Capillary GC/MS impurities ; Cold-on-column injection technique ; Fingertip organics ; EPA Method 625 ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Tab.
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  • 112
    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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  • 113
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 199-204 
    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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  • 114
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 242-247 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, LC ; Gradient elution ; Hydrostatic equilibrium ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Gradient elution under hydrostatic equilibrium is extended to the treatment of the case where the two liquids have different densities. Analytic expressions are derived only for the cases where both mixing chamber and reservoir have constant cross-sectional areas.As in the case where the densities of the liquids are equal, pressigned concentration gradients can be duplicated quite satisfactorily by combining a mixing chamber having a constant cross-sectional area and a reservoir having an area which changes linearly with reservoir height. A numerical example is given to illustrate the use of the derived equations.
    Additional Material: 6 Ill.
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  • 115
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 584-589 
    ISSN: 0935-6304
    Keywords: Chromatography ; Additivity of sorption energy ; Universal equation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Deviations from the additivity of energy contributions to substance sorption energies, determined on the basis of thermodynamic studies of GC behavior of homologous series of organic compounds fall into two categories: one for n-alkanes, the other for homologous series containing a functional group. A previously derived equation is proposed for homologous series, describing the deviation from the linear dependence of retention parameters with a propagating homolog n-alkyl chain. The equation permits calculation of retention parameters of homologs starting from the first member in gas-liquid, gas-solid, and liquid-liquid systems. The results prove its universal applicability.
    Additional Material: 8 Tab.
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  • 116
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 306-307 
    ISSN: 0935-6304
    Keywords: Liquid chromatography ; Fluorometric determination ; Postcolumn reaction ; o-Phthaldehyde ; Saliva bradykinin ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 117
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 335-340 
    ISSN: 0935-6304
    Keywords: Capillary gas-liquid chromatography ; Stationary-phase focusing ; Swelling ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Sample introduction using the solvent effect can lead to significant swelling of the stationary phase. The phenomenon has been studied theoretically and experimentally. The longitudinal profile of the swollen phase has been established. Swelling can affect the retention time of solutes, the shape of solute bands emerging from the inlet, and the maximum permissible sample size.
    Additional Material: 8 Ill.
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  • 118
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 535-537 
    ISSN: 0935-6304
    Keywords: Liquid chromatography ; Fused silica capillary columns ; Reverse-phase ; Nanoliter flow cell ; Column packing ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 119
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 613-617 
    ISSN: 0935-6304
    Keywords: Fused silica capillary tube isotachophoresis ; Multichannel photodiode array detector ; Cationic dye analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Isotachophoresis carried out in a 0.25 mm i.d. fused-silica capillary tube yielded high resolution, compared with that in a fluorinated ethylene-propylene polymer tube. The use of an ultraviolet-visible multichannel spectrophotometer with photodiode array as detector together with a cross flow cell (volume 0.01 μl) was investigated. The system was successfully applied to the analysis of cationic dyes such as neutral red, bismarck brown, and basic fuchsine.
    Additional Material: 6 Ill.
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  • 120
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 626-632 
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography, SFC ; Post-column restrictor ; Dead-time variation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A one-dimensional compressible flow model is used in the description of actual flow through ducts. This model serves well in the explanation and prediction of the characteristics towards signal distortion, noise, mass flow rate and influence on dead-time behavior of end-restrictors as used in supercritical fluid chromatography (SFC) with post-column detection. It was experimentally verified that tapered restrictors have a better performance than constant diameter restrictors at relatively low detection temperatures (200°C).The mass flow rate of a tapered restrictor is found to be linearly proportional to applied inlet pressure, implying the same linear dependence of the product of linear velocity and on-column density. A more than proportional rise of density will, therefore, lead to a decrease in linear velocity and vice versa. Since thermostat temperature fluctuations are directly translated into linear velocity variations, a very temperature stable thermostat has to be used.As will be discussed, this complicated dead-time dependence on applied pressure has a large effect on the chromatographic results.
    Additional Material: 7 Ill.
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  • 121
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 643-647 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography (CGC) ; Simultaneous quantitation ; Human plasma ; Glyceryl trinitrate ; Glyceryl dinitrate ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A specific, sensitive, and precise assay for simultaneous quantitation of glyceryl trinitrate (GTN) and its metabolites 1,2-and 1,3-glyceryl dinitrate (GDN) has been developed. The method involves one single extraction step with benzene, followed by evaporation at 55°C. One μl of the extract was injected onto a capillary fused silica column with trifluoropropyl as the stationary phase. The column separated all the nitrates within 17 minutes using temperature programming from 90 to 155°C. The lower limits of detection were 0.05, 0.5, and 0.1 nmol/I for GTN, 1,2-GDN and 1,3-GDN respectively. The calibration curves were linear in the concentration ranges 0.05-10.0 nmol/I (GTN), 0.5-10.0 nmol/I (1,2-GDN) and 0.1-10.0 nmol/I (1,3-GDN). Plasma concentration data from two patients receiving intravenous GTN infusion are presented.
    Additional Material: 2 Ill.
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  • 122
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 410-411 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, LC ; Temperature programming ; Carboxylic acids ; Cation exchange ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 123
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 640-643 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary column ; Chiral monoamide phase ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
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  • 124
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 652-656 
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography ; Capillary columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In cases where high efficiency is required to resolve complex mixtures of either thermally labile or nonvolatile organic compounds, capillary supercritical fluid chromatography may be the most desirable analytical method. While great strides in this new technology have been made over the last few years, several problem areas are requiring increased attention. These include sample introduction systems, pressure reduction at the end of the column, column stability in various supercritical mobile phases, and migration of polar solute molecules. This paper describes the state-of-the-art in capillary SFC with emphasis on the progress made and future needs in the solutions to these specific problems.
    Additional Material: 3 Ill.
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  • 125
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 671-675 
    ISSN: 0935-6304
    Keywords: Capillary GC ; GC-MS ; Residue analysis PCB's ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An integrated analytical procedure for polychlorinated biphenyl (PCB) multiresidues in environmental samples has been developed and applied to well-characterized samples. PCB residues are characterized and quantified using wall coated open tubular column (WCOT) gas chromatography or HRGC/MS-selected ion monitoring. An automated data system based on a Spectra Physics SP-4200 computing integrator is used to select and quantitate peaks of individual congeners and homolog groups. This procedure consistently yields results with a reproducibility within 3 percent for HRGC-ECD and 3.7 percent for HRGC/MS-SIM technique respectively.
    Additional Material: 1 Ill.
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  • 126
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 462-464 
    ISSN: 0935-6304
    Keywords: Gas liquid chromatography, GLC ; Capillary columns ; Headspace analysis ; Cuticular hydrocarbons ; Volatiles ; Insects ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 127
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 469-471 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; GC/MS ; Selected ion monitoring (SIM) ; Polycyclic aromatic compounds ; 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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  • 128
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 483-484 
    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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  • 129
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 492-501 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The use of high resolution chromatographic techniques for the determination of species of great importance in atmospheric pollution is critically reviewed. Attention has been focused on those pollutants recently recognized to be responsible for biological activity of particulate matter, acid deposition, and photochemical smog generation. The unique contribution made by capillary GC to the solution of environmental problems is demonstrated by the results obtained in the identification of several nitrofluoranthene/pyrene isomers in urban dust, industrial emissions, and automobile exhaust and by the selective determination of 2,3,7,8-tetrachlorodibenzo-ρ-dioxin in fly-ash emitted from urban incinerators. Also organic components dissolved in rain-water can be analyzed by capillary chromatography after sample enrichment on traps filled with solid sorbents. The recent availability of sampling precedures suitable for the collection of gaseous species which play an important role in acid deposition makes possible their determination by chromatographic techniques. Inorganic acids, sampled through high efficiency annular denuders to obtain discrimination between gaseous species and aerosols, can be determined by ion chromatography. Peroxyacyl nitrates, relevant to photochemical pollution, can be determined by GC combined with electron capture detection. New fields of application for high resolution chromatography are discussed.
    Additional Material: 12 Ill.
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  • 130
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 9 (1986), S. 528-530 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Reversed-phase mode ; Environmental studies ; Biphenyl 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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  • 131
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    Journal of High Resolution Chromatography 9 (1986), S. 537-538 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Reversed-phase made ; Mixing chamber ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
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  • 132
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    Journal of High Resolution Chromatography 9 (1986), S. 548-554 
    ISSN: 0935-6304
    Keywords: Gas liquid chromatography (GLC) ; Fused silica capillary columns ; Alkali flame ionization detection (AFID) ; Mass spectrometry (MS) ; Quantitation in human serum ; Ethylenediamine ; Aminophylline ; Small molecular weight amines and diamines ; m-Toluoyl derivatives ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A specific and sensitive method for the determination of ethylenediamine in human plasma is described. The aqueous sample is treated with m-toluoyl chloride, yielding the N,N′-bis(m-toluoyl) derivative of the diamine, which is extracted into dichloromethane and quantitated after “on column” methylation by capillary gas liquid chromatography with alkali flame ionization detection. The corresponding derivative of putrescine serves as internal standard. The assay is reproducible and calibration curves are linear over the concentration range 0.05 to 10 μg · ml-1. The lower detection limit is about 10 ng · ml-1. The structures of the compounds of interest eluting from the capillary column are examined by gas liquid chromatography/mass spectrometry. The assay has been applied to the analysis of ethylenediamine in plasma following the administration of aminophylline and ethylenediamine in a cross-over study to patients with bronchopulmonary diseases. The method also proves suitable for measuring other primary and secondary amines and diamines in aqueous solutions by gas liquid chromatography.
    Additional Material: 7 Ill.
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  • 133
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    Journal of High Resolution Chromatography 9 (1986), S. 577-583 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary column, FSCC ; Non-methane hydrocarbons, NMHC ; Air analysis ; On-column cryofocusing ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An analytical method for the determination of non-methane hydrocarbons (NMHC) in air was developed using simultaneously pressure and temperature programmed gas chromatography (GC) on a capillary column. The separation of C2-C10 hydrocarbons was performed in a single GC-run using a fused silica capillary column (FSCC) with a chemically bonded non-polar stationary phase (CP-Sil-5-CB). A combination of on-column cryofocusing and GC reinjection provided baseline separation of C2 hydrocarbons at subambient initial temperature (-40°C). The cryofocusing was performed on the column head immersed in liquid nitrogen. Quantitative retention of all C2-C10 hydrocarbons was achieved only when a temperature gradient is created along the cooled column section. The focused components are eluted from the column head without supplementary heating by removing the coolant. To eliminate matrix effects, the enrichment procedure was designed to remove CO2 and H2O. The detection limit was found to be 2.0 × 10-12 g propane.
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  • 134
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    Journal of High Resolution Chromatography 9 (1986), S. 593-594 
    ISSN: 0935-6304
    Keywords: Capillary GC ; HPLC ; Adulteration of cold pressed olive oil ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 135
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    Journal of High Resolution Chromatography 9 (1986), S. 600-601 
    ISSN: 0935-6304
    Keywords: Liquid chromatography ; Internal standard ; External standard ; Quantitation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Tab.
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  • 136
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    Journal of High Resolution Chromatography 9 (1986), S. 618-623 
    ISSN: 0935-6304
    Keywords: Capillary GC ; FSOT columns ; Applications ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The chromatographic performance of 10 m × 100 μm i.d. capillary columns, coated with different stationary phases, was studied. TZ-ū plots were measured at different temperature program rates. The polarity and selectivity are strongly influenced by the temperature program rate. The analysis time depends on the capacity ratio and the selectivity factor; stationary phase selection thus is an important aspect in high speed capillary GC. A number of applications is presented and the applicability of split injection is discussed.
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  • 137
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    Journal of High Resolution Chromatography 9 (1986), S. 637-640 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Headspace ; Dynamic headspace analysis ; Applications of headspace technique ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The advantages of the dynamic headspace method for the analysis of solid samples, as compared with the static head space method, are discussed. Examples of dynamic headspace analyses are given to illustrate its possibilities.
    Additional Material: 3 Ill.
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  • 138
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    Journal of High Resolution Chromatography 9 (1986), S. 647-651 
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography (SFC) ; Stationary-phase phenomena ; Mobile-phase modifier ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A significant uptake of supercritical mobile phases into immobilized stationary phases has been observed. The phase swelling effect has been evaluated hydrodynamically for SE-30, SE-54, and cyanopropyl silicone phases with respect to the mobile-phase density of supercritical butane, column temperature, and the presence of a polar retention moderator. Some kinetic and retention consequences of the swelling phenomena are discussed.
    Additional Material: 5 Ill.
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  • 139
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    Journal of High Resolution Chromatography 9 (1986), S. 676-678 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Narrow bore columns ; Wide bore thick film columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The analysis time for a given resolution is a complex function of stationary phase selectivity, column radius, and thickness of the stationary phase film. Variation of these parameters has a large effect not only on analysis time, but also on the column inlet pressure and other instrumental requirements. The minimum amount that can be reliably detected as well as the maximum sample capacity of a column are strongly related to the selected column dimensions.
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  • 140
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    Journal of High Resolution Chromatography 9 (1986), S. 666-670 
    ISSN: 0935-6304
    Keywords: Electrokinetic chromatography ; Electroosmosis ; Electrophoresis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Effects of pH, concentration of sodium dodecyl sulfate (SDS), additives, and coatings of polymers on the inner wall of fused silica tubing on electrokinetic migration were investigated with SDS solutions. The increase in SDS concentrations caused a substantial increase of the electrophoretic velocity of the SDS micelle but little affected the electroosmotic velocity veo under a constant applied voltage. No significant change in veo was observed either when the pH of the solution was varied from 5.5 to 9 or when additives such as hydroxypropyl cellulose were employed. Compared with an uncoated tube, electroosmosis became stronger in a fused silica tube coated with methyl silicone but weaker in one coated with polyethylene glycol 20M.
    Additional Material: 3 Ill.
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  • 141
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    Journal of High Resolution Chromatography 9 (1986), S. 688-692 
    ISSN: 0935-6304
    Keywords: Aza-arenes ; Retention index ; Fluorescence spectra ; Post column reaction ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Two methods are described for predicting the molecular structures of aza-arenes eluted from a capillary column. The first is based on a combination of retention indexes (RI) and a post-column reaction. The RI of an aza-arene is calculated by using the incremental contributions of some atomic groups to RI. Once the molecular weight is determined by the mass spectrum, the possible compounds are picked up, based on comparison of the observed RI with the calculated RI values and information about the intramolecular environment around the nitrogen atom obtained from the degree of peak shift resulting from interaction with Ni(II). The second is due to combination of information from fluorescence spectrometry and TLC fractionation. The fluorescence spectrum allows the identification of the fused ring system.
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  • 142
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    Journal of High Resolution Chromatography 9 (1986), S. 702-707 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Temperature programming ; Optimization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The theory which predicts the retention time, retention temperature, and peak width for any kind of multi-step TPGC and the principle of optimization has been described. Software for optimization and identification in TPGC has been developed on the basis of this theory. It has also been proven that the relationship between peak width in TPGC and the derived or “invented” retention time is similar to that between peak width and retention time in isothermal processes. The validity of the software has been proved by using it to predict retention temperature, retention time, and peak width for any kind of temperature programming and to predict the optimum temperature program for separation of a multihomolog mixture of industrial alcohols and 15 enantiomeric pairs of amino acids.
    Additional Material: 4 Ill.
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  • 143
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    Journal of High Resolution Chromatography 9 (1986) 
    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
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Fused-silica capillary columns ; Programmed-temperature (PTV) injection ; Cold on-column injection ; Triglyceride analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The capillary gas chromatographic analysis of complex naturally occurring and food-product triglyceride mixtures is accomplished qualitatively and quantitatively on columns coated with methyl and methyl-phenyl (65%) silicones using programmed-temperature split/splitless and on-column injection. Faster analysis times are achieved using elevated initial column oven temperatures with cold initial injector temperatures.
    Additional Material: 10 Ill.
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  • 145
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    Journal of High Resolution Chromatography 9 (1986), S. 747-751 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Capillary columns ; On-Column GC ; Cold-trapping effect on on-column GC ; Solvent effect on on-column GC ; Behavior of solutes and solvent ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The behavior of heavy solutes present in a sample injected on the precolumn has not been clarified in on-column injection onto gas chromatograph having a capillary column coupled to an uncoated precolumn in an oven. To investigate this point, an on-column gas chromatograph has been developed which is constructed with a heatable precolumn outside the oven. Some experiments were carried out in order to evaluate the performance. As a result, it was found that heavy solutes reach the first part of the main capillary column after the solvent has gone, resulting in sharp peaks without solvent effects. The reason why sharp peaks appear for the heavy solutes is also discussed. The cold-trapping effect has been shown to play an important role in narrowing the band width of the heavy solutes. Some of the advantages of the gas chromatograph developed are also presented.
    Additional Material: 8 Ill.
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  • 146
    ISSN: 0935-6304
    Keywords: Gas chromatography ; FID and FPD ; Azinphos-methyl, -ethyl and six metabolites ; Beta vulgaris leaves ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 147
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    Journal of High Resolution Chromatography 9 (1986), S. 708-711 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography GC-MS ; Airborne particulates ; Nitroarenes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Routine analytical methods for benzo[a]pyrene and nitroarenes in airborne particulates are presented. Benzo[a]pyrene in airborne particulates was easily analyzed by a capillary GC/NCIMS. Analysis time was about 10 min and analytical values obtained by this method agreed well with those by HPLC/spectrofluorometry. Nineteen nitroarenes were analyzed by capillary GC/FTD following a simple clean-up procedure. Fifteen out of 19 nitroarenes analyzed were mutagenic for Salmonella typhimurium TA100 and TA98, and 4 nitroarenes were carcinogenic to experimental animals.
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  • 148
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    Journal of High Resolution Chromatography 9 (1986), S. 724-724 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 149
    ISSN: 0935-6304
    Keywords: Capillary GC ; RP-HPLC ; CP-MAS NMR ; Deactivation methods ; Hexamethyldisilazane ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of Cab-O-Sil, a highly dispersed vitreous quartz, with hexamethyldisilazane (HMDS) was studied in the temperature range 380-500°C, using 29Si solid state NMR and other techniques. Such studies are of importance in view of deactivation procedures of fused silica at high temperatures in capillary GC.The commonly accepted reaction equation: \documentclass{article}\pagestyle{empty}\begin{document}$$ \left({{\rm Me}_{\rm 3} {\rm Si}} \right)_2 {\rm NH } + {\rm 2}\equiv {\rm SiOH} \to {\rm 2} \equiv {\rm SiOSiMe}_{\rm 2} + {\rm NH}_{\rm 3} $$\end{document} predominates only below ca. 400°C. Above ca. 400°C the intermediate cleavage product Me3SiNH2 reacts with surface silanol groups to form ≡SioSiMe2NH2 + CH4. At higher temperatures these groups may ultimately form (≡SiO)3SiNH2 groups (analogously to the formation of bi-and tridentate linkages starting from ≡SiOSiMe3 groups), but (≡SiO)3SiNH2 groups are also directly formed at lower temperatures, simultaneously with the ≡SiOSiMe3 groups, probably by reaction with siloxane bridges: \documentclass{article}\pagestyle{empty}\begin{document}$$ {\rm Me}_3 {\rm SiNH}_2 + \equiv {\rm SiOSi} \equiv\; \to \;\equiv SiNH_2 + \equiv SiOSiMe_3 $$\end{document}.The reactions of the trimethylsilylamine part of HMDS with Cab-O-Sil were confirmed by an independent series of silylations using N,N-dimethyltrimethylsilylamine instead of HDMS. The presence of amino groups as ≡SiNH2 was confirmed by FT-IR. This may be one of the reasons why very high temperature silylation with disilazanes does not provide a satisfactory deactivation of fused silica GC columns: the active ≡SiOH groups are “replaced” by active ≡SiNH2 groups. However, such a material may be of interest in LC. Silylation with silazanes at ca. 350°C in humid atmosphere and/or after extensive hydroxylation (leaching) of the surface should yield sufficiently deactivated surfaces with a rather well defined surface structure.
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  • 150
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    Journal of High Resolution Chromatography 9 (1986), S. 761-762 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Glass capillary columns ; Surface deactivation ; Diphenyl phenylmethyl silicone ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 151
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    Journal of High Resolution Chromatography 9 (1986), S. 768-768 
    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 9 (1986), S. 765-767 
    ISSN: 0935-6304
    Keywords: Reversed-phase HPLC ; Alkaline-earth metals ; Chelating resin ; Dodecyliminodiacetic acid ; Dynamic coating ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 153
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    Journal of High Resolution Chromatography 9 (1986), S. 3-3 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 154
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    Journal of High Resolution Chromatography 9 (1986), S. 4-17 
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography ; Applications ; Practical information ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The general topic of supercritical fluid chromatography (SFC) is introduced, and historical aspects of its development are discussed. The physical properties of supercritical fluids, gases and liquids are tabulated. SFC is compared and contrasted with the classical forms of chromatography - gas chromatography (GC) and high performance liquid chromatography (HPLC). The selectivity of SFC, GC, and HPLC are discussed and compared. Instrumentation employed for supercritical fluid chromatography is depicted. A wide variety of SFC applications are introduced. New examples of the use of SFC for analysis of a variety of complex oligomeric mixtures indcluding polypropylene glycol, polysiloxanes, fluorocarbon oligomers (i.e. -3M's fluoro-chemical surfactant Fluorad 171, and Kel-F) and high molecular weight normal alcohols are shown. The use of SFC for separation of mono-, di-, and triglycerides at low operating temperatures is described. Lastly, the use of SFC for separations of complex hydrocarbon mixtures from liquid fuels, polycyclic aromatic hydrocarbons, synthetic alpha-olefins, and petroleum functional group separations are depicted.
    Additional Material: 23 Ill.
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  • 155
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    Journal of High Resolution Chromatography 9 (1986), S. 57-58 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, LC ; Cation exchange ; Dicarboxylic acids ; Monocarboxylic acids ; Cyanovaleric acid ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
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  • 156
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    Journal of High Resolution Chromatography 9 (1986), S. 61-63 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; HPLC accessories ; Rotary sampling valves ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 6 Ill.
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  • 157
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    Journal of High Resolution Chromatography 9 (1986), S. 69-72 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Programmed-temperature (PTV) injection ; Cold on-column injection ; Triglycerides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The performance of split and splitless programmed-temperature (PTV) injection is compared to cold on-column and hot (classical) split injection for the analysis of triglycerides on an apolar capillary gas chromatographic column. Quantitative accuracy and precision of PTV injection are determined for a synthetic mixture of triglycerides relative to cold on-column injection.
    Additional Material: 2 Ill.
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  • 158
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    Journal of High Resolution Chromatography 9 (1986), S. 95-101 
    ISSN: 0935-6304
    Keywords: Coupled HPLC-capillary GC ; Concurrent solvent evaporation ; Retention gap ; Solvent effects ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A technique is proposed which allows introduction of very large volumes of liquid (10 ml were tested) into capillary columns equipped with short (1-2 m long) retention gaps. It is based on concurrent solvent evaporation, i.e. evaporation of the solvent during introduction of the sample. The technique presupposes high carrier gas flow rates (at least during sample introduction) and column temperatures near the solvent boiling point. The major limitation of the method is the occurrence of peak broadening for solutes eluted up to 30°, in some cases up to 100°, above the injection temperature. This is due to the absence of solvent trapping and a reduced efficiency of phase soaking. Therefore, use of volatile solvents is often advantageous. Application of the concurrent solvent evaporation technique allows introduction of liquids which do not wet the retention gap surface. However, the method is still not very attractive for analysis of aqueous or water-containing solutions (reversed phase HPLC).
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  • 159
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    Journal of High Resolution Chromatography 9 (1986), S. 117-119 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, LC ; Gas chromatography, GC ; Fused silica open tubular columns ; Column preparation ; On-column fluorescence detection ; Capacity factors ; Polysiloxane stationary phases ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 5 Ill.
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  • 160
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    Journal of High Resolution Chromatography 9 (1986), S. 302-303 
    ISSN: 0935-6304
    Keywords: Normal phase HPLC ; Polycyclic aromatic compounds ; Double bond equivalents ; Cyano/amino bonded silica ; Selectivity ; Molecular conformation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 161
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    Journal of High Resolution Chromatography 9 (1986), S. 310-311 
    ISSN: 0935-6304
    Keywords: Gas-liquid chromatography, GLC ; Propoxylation of acetic acid ; Identification ; Quantitative analysis ; 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 9 (1986), S. 341-344 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Fused silica columns ; Peak splitting ; Christmas tree peaks ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Fluctuating thermal gradients are recognized as a distinct source of peak splitting in capillary column gas chromatography. In this study, the influence of analyte signal level, temperature oscillation amplitude, and oscillation frequency on splitting are quantitatively examined. Stable gradients are also considered. A simple, effective method is proposed for virtually eliminating thermal peak splitting in isothermal capillary GC analysis.
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  • 163
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    Journal of High Resolution Chromatography 9 (1986), S. 355-355 
    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 9 (1986), S. 358-360 
    ISSN: 0935-6304
    Keywords: Liquid chromatography ; Ion-pair RP HPLC ; Stable nitroxyl radicals ; Salt effect ; UV, RI detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
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  • 165
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    Journal of High Resolution Chromatography 9 (1986), S. 364-365 
    ISSN: 0935-6304
    Keywords: HPLC ; 3μm packings ; Reverse-phase ; Frit materials ; Acidic mobile phases ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 166
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    Journal of High Resolution Chromatography 9 (1986), S. 421-422 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 167
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    Journal of High Resolution Chromatography 9 (1986), S. 479-480 
    ISSN: 0935-6304
    Keywords: High-performance liquid chromatography, HPLC ; Alkaline phosphatase, AP ; Lactate dehydrogenase, LD ; γ-Glutamyltransferase ; γ-GT ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 168
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    Journal of High Resolution Chromatography 9 (1986), S. 698-702 
    ISSN: 0935-6304
    Keywords: Capillary column gas chromatography ; Microwave-induced plasma emission spectrophotometric detector ; Photodiode array spectrophotometer ; Element-specific detector ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A microwave-induced plasma emission spectrophotometric detector (MIPD) was used as an element-specific detector for capillary column gas chromatography. The atmospheric pressure microwave helium plasma generated with an original device called a SURFATRON was used as an atomization and excitation source. Combining a photodiode array spectrophotometer with the above system made the emission spectrophotometric detector very powerful. A wide range of spectra could be instantly monitored without any mechanical device.However, the spectrum of atmospheric helium emission plasma was complicated by the presence of air around the plasma discharge. An on-line background correction scheme was developed to handle such complicated spectra.
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  • 169
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    Journal of High Resolution Chromatography 9 (1986), S. 131-132 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 170
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    Journal of High Resolution Chromatography 9 (1986), S. 145-153 
    ISSN: 0935-6304
    Keywords: Capillary columns ; Supercritical fluid chromatography ; Supercritical fluid chromatography-mass spectrometry ; SFC-MS ; Thermally labile compound analysis ; Heavy molecular weight compound analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Capillary supercritical fluid chromatography and its combination with mass spectrometry (SFC-MS) is an important analytical methodology for the analysis of thermally labile and high molecular weight compounds. The mass spectrometer provides sensitive and highly selective detection for the chromatographic effluent. The same physical-chemical properties of supercritical fluids that provide important chromatographic advantages are also important for the transport and gas phase introduction of analyte molecules into the mass spectrometer. The low mobile phase flow rates of small diameter (〈 100 μm i.d.) capillary columns allow the total chromatographic effluent to be introduced with conventional, but often slightly modified, ion source configurations for quadrupole mass spectrometers with either electron impact (EI) or chemical ionization (CI) detection. The full range of CI reagents can also be used to obtain additional selectivity and complementary structural data. The instrumentation and operating parameters for capillary SFC-MS methods are described. The applicability and usefulness of various SFC-MS analysis methods are demonstrated using a variety of samples.
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  • 171
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    Journal of High Resolution Chromatography 9 (1986), S. 175-177 
    ISSN: 0935-6304
    Keywords: Capillary column ; Supercritical fluid chromatograph, SFC ; Commercial dyes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: High resolution separations of selected commercial azo, aniline, and anthraquinone dyes by capillary column supercritical fluid chromatography (SFC) are demonstrated. Supercritical n-pentane was used as a mobile phase and provided efficient separations of multi-functional, polar disperse dyes with molecular weights up to approximately 700 daltons.
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  • 172
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    Journal of High Resolution Chromatography 9 (1986), S. 172-174 
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography ; Mass spectrometry ; Capillary column ; SFC/MS ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A benchtop SFC/MS system is described which utilizes supercritical carbon dioxide in a 50 micron diameter open tubular column interfaced directly to an unchanged commercially available benchtop capillary GC/MS system equipped with a chemical ionization (CI) source. A small amount of methane reagent gas was admitted co-axially to a capillary restrictor at the exit of the capillary chromatographic column. This make-up gas served as the CI reagent gas and appeared to optimize the sensitivity of the system while providing abundant (M+1) ions for the analytes investigated in this study. Good chromatographic intergrity was obtained for the GC/MS test compound, decafluorotriphenylphosphine (DFTPP), but the capillary restrictor appeared to cause some tailing of the ion current profiles resulting from low nanogram levels of caffeine and some fatty acid esters. Improvements in the SFC/MS capillary restrictor interface and the pumping system of the benchtop GC/MS system should increase the capability of this system for future applications.
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  • 173
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    Journal of High Resolution Chromatography 9 (1986), S. 189-192 
    ISSN: 0935-6304
    Keywords: Capillary SFC ; Triglycerides ; Resolution ; Column temperature ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 5 Ill.
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  • 174
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    Journal of High Resolution Chromatography 9 (1986), S. 209-212 
    ISSN: 0935-6304
    Keywords: Capillary supercritical fluid chromatography, SFC ; Derivatization ; Sugars ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Direct analysis of polar solutes by supercritical fluid chromatography (SFC) has been somewhat limited because the mobile phases in common use are all relatively nonpolar. Derivatization is demonstrated as a viable means for facilitating the SFC separation of sugars. Oligo- and polysaccharides containing up to 18 glucose units are completely resolved by capillary SFC.
    Additional Material: 4 Ill.
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  • 175
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    Journal of High Resolution Chromatography 9 (1986), S. 218-223 
    ISSN: 0935-6304
    Keywords: High performance planar chromatography, HPPLC ; Preparative anticircular chromatography (PACH) ; Sample collection ; Quantification ; Silica Gel (20 × 20 and 10 × 10 cm) plates ; RP-18 (20 × 20 and 10 × 10 cm) plates ; Unsaponifiables from plant lipids ; Fatty acid methyl esters ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A preparative anticircular chromatography (PACH) device was constructed to elucidate different applications of separation problems as well as to compare different sample collection techniques in this particular PLC mode. An anticircular PC apparatus had to be established which allowed the utilization of 20 X 20 cm thin-layer plates as well as sampling positioning at any given radius. Typical solvent migration times were 8-12 minutes and ca. 8-10 ml of solvent was needed for an entire 20 cm plate. It was shown that peak broadening effects due to diffusion during long migration could be avoided in the same way as for analytical anticircular PLC on 10 X 10 plates. On the other hand, longer migration distances allow increased resolution, in turn allowing higher sample loads, particularly in the case of trace compound enrichment. A full description of the apparatus is given, including the sampling device.Different sample collection techniques were tried and evaluated, including the through-flow technique by on-line center collection for plate washing as well as classical scraping-off of interesting zones. Further evaluation of the method included quantification and evaluation of consistency by UV/VIS scanning after spot-visualization. Several application examples are given to illustrate the efficiency of the preparative anticircular PLC-system.
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  • 176
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    Journal of High Resolution Chromatography 9 (1986), S. 261-262 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 177
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    Journal of High Resolution Chromatography 9 (1986), S. 278-280 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Stationary-phase focusing ; Sample size ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Equations have been derived to predict the extent to which the sample size may be increased, without decreasing the column performance, by stationary-phase focusing at sub-ambient temperatures. Under favorable circumstances the sample size may be enhanced several hundredfold.
    Additional Material: 1 Ill.
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  • 178
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    Journal of High Resolution Chromatography 9 (1986), S. 281-284 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Time-switched detectors ; UV detection ; Fluorimetric detection ; Vitamin A ; Vitamin E ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An HPLC method utilizing a UV and a fluorimetric detector linked in series is described. By use of a simple integrator-controlled time-switched relay, analysis of serum vitamin A and E is accomplished on the same chromatogram and at optimum sensitivity for each detector. A single internal standard (retinyl acetate) monitored only by the UV detector permits measurement of both vitamins over a wide linear range. Precision of the assays is satisfactory, both on a within-day and on a day-to-day basis. Recoveries of both vitamins are virtually 100% whilst sensitivity is 2 μg/L (retinol) and 0.05 mg/L (α-tocopherol).
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  • 179
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    Journal of High Resolution Chromatography 9 (1986), S. 400-404 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Multidimensional GC ; Macrobore WCOT and PLOT columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Multidimensional GC (MDGC) with macrobore WCOT and PLOT columns has shown several benefits: (1) Higher flow rates, which are used, makes possible the use of common valves as the switching device; (2) very simple system configurations are possible; (3) because the columns have relatively large capacity, the TCD can be used to measure both organic and inorganic components; (4) micropacked or open tubular columns are precolumns which provide a wide range of selectivity; (5) both precolumn and analytical columns can be operated at the same flow rate without splitting of the sample. Four rapid sample analyses: (1) Oxygenates in gasohol; (2) natural gas; (3) refinery gas; (4) hydrocarbon types in naphtha, have been developed and performed on a less complex and economical gas chromatograph.
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  • 180
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    Journal of High Resolution Chromatography 9 (1986), S. 415-416 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Ion exclusion ; Peak identification ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Tab.
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  • 181
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    Journal of High Resolution Chromatography 9 (1986), S. 429-430 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 182
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    Journal of High Resolution Chromatography 9 (1986), S. 466-468 
    ISSN: 0935-6304
    Keywords: HRGC/FTIR ; Essential oils ; Unresolved peaks ; Monoterpenes ; Vapor phase IR spectra ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 183
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    Journal of High Resolution Chromatography 9 (1986), S. 481-482 
    ISSN: 0935-6304
    Keywords: Glass-silica capillary joining ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 184
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    Journal of High Resolution Chromatography 9 (1986), S. 477-479 
    ISSN: 0935-6304
    Keywords: Liquid chromatography, HPLC ; Column switching liquid chromatography ; Fluorescence detection ; 9-Anthryldiazomethane ; Saliva ; Prostaglandin ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
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  • 185
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    Journal of High Resolution Chromatography 9 (1986), S. 607-608 
    ISSN: 0935-6304
    Keywords: Racemic resolution ; Chiral cavities ; Polymer imprinted with template ; Chiral stationary phases ; Temperature effect in racemic resolution ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 186
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    Journal of High Resolution Chromatography 9 (1986) 
    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 9 (1986), S. 657-661 
    ISSN: 0935-6304
    Keywords: Capillary GC ; GC/MS ; Sampling techniques ; Arson debris ; Urban air ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Sample enrichment technology and instrumental sensitivity are no longer limiting factors in arson debris analysis. When pyrolyzed, petroleum based composite materials may produce artifacts. Urban air is another major source of interference since some of the components typically found in air, in particular alkylated aromatic hydrocarbons, are customarily used as indicators for the presence of gasoline. It is suggested to replace qualitative analysis with a quantitative approach, taking the sample matrix into consideration.
    Additional Material: 5 Ill.
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  • 188
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    Journal of High Resolution Chromatography 9 (1986), S. 692-698 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Fused silica capillary column ; Organochlorine insecticide residues ; Arable soils ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Electron capture gas chromatography with three chemically bonded fused-silica capillary columns (CB-FSCs), OV-17, OV-1701, and SE-52, was performed to evaluate peak separability of 28 organochlorine insecticides and related compounds. Relative retention times and relative peak heights to aldrin were measured and calculated. OV-17 CB-FSC showed the best separability among the three CB-FSCs employed and was applied to analysis of extracts from several soil samples with minimum clean-up procedure. The chromatograms obtained demonstrated steady baseline tracings free of interference. Residue data from soil samples were also tabulated.
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  • 189
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    Journal of High Resolution Chromatography 9 (1986), S. 718-718 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 190
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    Journal of High Resolution Chromatography 9 (1986), S. 719-720 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 191
    ISSN: 0935-6304
    Keywords: Analysis of high molecular weight compounds ; Gas chromatography Versus supercritical fluid chromatography ; Aluminum clad fused silica capillary columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Samples, representative of certain classes of “high molecular weight” and/or less volatile substances, were analyzed by gas chromatography utilizing a new generation of aluminum clad flexible fused silica glass capillary columns containing thin films of a methyl polysioxane stationary phase capable of being operated isothermally to 400-425°C and temperature programmed to 425-440°C. The results obtained here were compared with those described in the literature discussing the latest advances in Supercritical Fluid Chromatography (SFC) in the analysis of precisely the same types of samples. In all instances, the gas chromatographic method provided superior speed of analysis, superior column efficiency, and superior resolution of the component bands. This was due to fundamental factors, favoring the diffusivity of the solutes in both the gas and liquid phases in this process at these high temperatures. Under these circumstances, it is thought that the strength of SFC mainly lies in the analysis of thermally labile samples until the advocates of this technique make more definitive strides in the handling of still higher molecular weight substances well beyond the newly expanded range of gas chromatography.
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  • 192
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 193
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    Journal of High Resolution Chromatography 9 (1986), S. 763-764 
    ISSN: 0935-6304
    Keywords: Capillary liquid chromatography ; Cellulose acetate fiber column ; Alcohols separation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 194
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    Biological Mass Spectrometry 13 (1986) 
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 195
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    Biological Mass Spectrometry 13 (1986), S. 167-170 
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The interaction of nucleic acid bases with the alkylating antitumour drug thiotepa has been studied by field ionization mass spectrometry. The possibility of interaction between all four DNA bases and thiotepa in neutral aqueous solutions was demonstrated. The analysis of the data for different methylated bases made it possible to elucidate some sites of alkylation - N(1)(Cyt), N(3)(Thy), N(9)(Ade) - which are compared with data on other alkylating agents available from the literature.
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  • 196
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    Biological Mass Spectrometry 13 (1986), S. 181-186 
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Gas chromatographic/mass spectrometric techniques using chemical ionization have been employed to characterize the fungicide dichlofluanid and its major metabolite. The results have indicated some unusual fragmentation pathways for perhalogenmethylmercapto compounds. Use of deuterated ammonia as reagent gas has permitted a comparative assessment of protonation and exchangeable hydrogens within the major fragment ion structures. Resultant structural information has been employed to confirm residue findings in strawberries at the low part-per-million level.
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  • 197
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    Biological Mass Spectrometry 13 (1986), S. 199-204 
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Positive- and negative-ion mass spectra of five glycoconjugates were obtained using laser desorption/Fourier transform mass spectrometry. These were the glycoalkaloids α-solanine and α-tomatine and the steroid glycosides gitoxin, lanatoside A and digitonin. Doping with KCl yielded both potassium- and chloride-attachment ions. Few fragment ions were observed for these species, with the exception of digitonin, although the negative-ion spectra showed relatively more fragmentation than the positive-ion spectra. All major fragments appeared to arise from losses of sugar groups due to cleavages at the glycosidic linkages. This contrasted sharply with the behavior of the malto-oligosaccharides studied in this laboratory.
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  • 198
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    Biological Mass Spectrometry 13 (1986) 
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 199
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    Biological Mass Spectrometry 13 (1986), S. 231-236 
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Capillary column ammonia chemical ionization mass spectrometry was investigated as a technique for the characterization of a number of organophosphorus chemical warfare agents and simulants, since electron impact ionization provides little or no molecular ion information for these compounds. The effects of source temperature, source pressure, electron energy and electron emission were investigated in order to optimize ammonia chemical ionization conditions. Source temperature was found to have a dramatic effect on the chemical ionization mass spectra acquired. Abundant [M + NH4]+ and/or [M + H]+ quasimolecular ions were usually observed at lower source temperatures for the selected compounds under positive ion chemical ionization conditions, along with a number of characteristic fragmentation ions. Full-scan mass spectra were obtained for 1--2 ng of analyte during the capillary column ammonia chemical ionization operation. The sensitivity, molecular ion information afforded and lack of background interference ions associated with this technique make it a good candidate for the confirmation of organophosphorus chemical warfare agents and simulants.
    Additional Material: 6 Ill.
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  • 200
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    Biological Mass Spectrometry 13 (1986), S. 1-14 
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The negative and positive ion fast atom bombardment mass (FAB) spectra and fast atom bombardment mass-analysed ion kinetic energy/collision-activated dissociation (MIKE/CAD) spectra of triterpenic saponins (triterpenic glycosides) are reported. That ionization technique is well suited to the analysis of natural mixtures of these compounds. Identification and sugar sequences can be obtained from the conventional MIKE and MIKE/CAD spectra. It is shown that the negative FAB mass spectra with polyethylene glycol 200 as the matrix give more information than positive spectra for this family of compounds. The negative ion FAB mass spectra show intense deprotonated molecular peaks [M - H]- which shift to [M + Cl]- in a polyethylene glycol 200/NH4Cl matrix. The positive ion FAB mass spectrometry with glycerol/NaCl as a matrix gives spectra characterized by an enhanced sodium cationized molecular ion [M + Na]+.
    Additional Material: 8 Ill.
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