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  • Analytical Chemistry and Spectroscopy  (2,913)
  • Inorganic Chemistry  (1,340)
  • 1995-1999  (2,036)
  • 1990-1994  (2,217)
  • 1950-1954
  • 1995  (2,036)
  • 1991  (2,217)
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  • 1995-1999  (2,036)
  • 1990-1994  (2,217)
  • 1950-1954
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  • 101
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 18 (1995), S. 272-272 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 102
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 18 (1995) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 103
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 18 (1995), S. 277-278 
    ISSN: 0935-6304
    Keywords: History of chromatography ; Moses ; Pliny the Elder ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Indications that already in the Ancient World, methods based on chromatographic principles were utilized, are discussed. As pointed out, they had little to do with chromatography.
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  • 104
    ISSN: 0935-6304
    Keywords: Cyclodextrins ; Multidimensional GC ; Isotope ratio ; Adulteration ; Flavors ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This work presents two techniques for testing for the adulteration of flavors. One uses multidimensional gas chromatography on cyclodextrin derivatives to separate chiral compounds, the other uses isotope ratio mass spectrometry coupled with gas chromatography to determine stable isotope ratios. Applications to fruits and plants for the food and perfume industry are introduced.
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  • 105
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 18 (1995), S. 286-288 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Citrus juices ; Adulteration ; Oligosaccharides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method is described for the detection of citrus juices adulterated by addition of industrial sugar products. The oligosaccharides maltotriose (DP3) and maltotetraose (DP4), both of which are absent from the natural sugar profile of citrus fruits, serve as markers. The sample preparation method includes clean-up on a solid phase ODS cartridge, fractionation of DP3 and DP4 carbohydrates by LC on aminopropyl silica gel, and derivatization of the collected sugars to form the oxime-trimethylsilyl derivatives. Capillary GC analysis is performed on a 30 m × 0.32 mm i.d. polydimethylsiloxane fused silica column applying cool on-column injection and FID detection. The detection limit for maltotriose and maltotetraose is about 1 mg l-1. Several orange and grapefruit juices were evaluated on their authenticity. Adulteration with crystalline sugar products cannot be detected with the described procedure.
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  • 106
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 18 (1995), S. 289-294 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Supercritical fluid chromatography ; FT-IR spectrometry ; Characterization ; Silicones ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Materials used in the manufacture of silicone breast prostheses were analyzed by supercritical fluid chromatography (SFC) and high temperature gas chromatography (GC) coupled with direct deposition FT-IR detection. The chromatographic resolution and deposition quality were found to be unsatisfactory for SFC/FT-IR; however, high temperature GC/FT-IR produced excellent results. The chromatograms and spectra obtained allowed for the identification of poly-dimethyl silicones and mono-, di-, and tri-diphenylsubstituted poly-dimethyl silicones. An automated method of baseline correction was developed that allowed functional group chromatograms due to molecules containing Si-phenyl bonds to be constructed without significant interference from Si-methyl bonds despite the fact that the Si-C stretching mode of Si-phenyl bands overlapped significantly with the strong bands due to Si-CH3 groups.
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  • 107
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    Journal of High Resolution Chromatography 18 (1995), S. 378-380 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 108
    ISSN: 0935-6304
    Keywords: Capillary GC ; Equilibrium headspace sampling ; Tenax TA trapping ; Thermal desorption ; TD-GC-MS ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Volatile compounds from biodegradable household waste and infected building materials have been studied by dynamic or equilibrium headspace sampling and concentration on Tenax TA followed by thermal desorption and HRGC-MS. Equilibrium headspace sampling was also used to study vegetables stored for 14-18 days at ambient temperature. Over 200 compounds were tentatively identified. The concentration of organic sulfur compounds from garden waste was high enough to contribute to respiratory problems of waste handling personnel. Nitriles, alkyl nitro compounds, and alkyl nitrates were isolated from radish and carrot samples at low concentrations (10-50 ppb). Air monitoring in waste handling working environments may be required to ensure the safety of personnel. Branched aliphatic aldehydes, carboxylic acids, esters, and 2-alkanones were found in the headspace of the infected building materials, indicating that volatile compounds may be useful for detection of microbial growth in buildings.
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  • 109
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 18 (1995), S. 381-383 
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Preconcentration-CE ; Drug metabolites ; Peptides ; On-line sample concentration ; Analyte stacking ; Transient isotachophoresis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 110
    ISSN: 0935-6304
    Keywords: Capillary Electrophoresis ; Mass spectrometry ; Preconcentration-CE ; Transient isotachophoresis ; Peptide mixture ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 111
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 18 (1995), S. 387-388 
    ISSN: 0935-6304
    Keywords: Size exclusion chromatography ; Gasoline additives ; Evaporative light-scattering detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 112
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    Journal of High Resolution Chromatography 18 (1995), S. 389-391 
    ISSN: 0935-6304
    Keywords: HPLC ; Optical resolution ; Chiral phase ; Substituted amylopectin tris(phenylcarbamate) derivatives ; Benzodiazepines ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 113
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    Journal of High Resolution Chromatography 18 (1995), S. 392-392 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 114
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    Journal of High Resolution Chromatography 18 (1995) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
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  • 115
    ISSN: 0935-6304
    Keywords: High-speed GC ; Electron capture detector (ECD) ; Detection limits ; PCBs ; Pesticides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In this work the combination of high-speed narrow-bore capillary GC with electron capture detection is evaluated. The make-up gas flow rate is a key parameter in the successful coupling of narrowbore columns and ECD detection. The make-up flow has to be as high as possible to eliminate peak tailing caused by the large detection cell volume. The sensitivities at these elevated make-up flow rates (400 to 1000 ml/min), measured for some pesticides like HCB and dieldrin, were very good. Detection limits for these compounds of 0.1 pg were obtained, resulting in minimum detectable concentrations of approximately 0.2 ppb. The performance of the system is illustrated by several high-speed analyses of environmentally relevant samples of PCBs and pesticides.
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  • 116
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    Journal of High Resolution Chromatography 18 (1995), S. 417-421 
    ISSN: 0935-6304
    Keywords: Microwave extraction of PCBs ; Water samples ; Low ng/L concentration ; ECD quantitation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The microwave energy produced by a high intensity microwave oven was used to extract polychlorinated biphenyls (PCB) from water samples. This static method was compared with liquid-liquid extraction to determine the optimum and limiting conditions in extraction processes. The sample size and sample container shape determine the temperature profiles in the sample. Using a 500 mL sample size, the detection limit is in the low ng/L range when an electron capture detector is employed.
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  • 117
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    Journal of High Resolution Chromatography 18 (1995), S. 319-322 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Atomic emission detection ; Elemental response ; Compound independent calibration ; 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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    Journal of High Resolution Chromatography 18 (1995), S. 326-326 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 119
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    Journal of High Resolution Chromatography 18 (1995) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 120
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    Journal of High Resolution Chromatography 18 (1995), S. 329-329 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 121
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    Journal of High Resolution Chromatography 18 (1995), S. 343-347 
    ISSN: 0935-6304
    Keywords: GC ; Window diagrams ; Optimization of mixed phases ; On-line chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Window diagrams that optimize for the separation of only one or a few components in a complex mixture are applied to on-line process analysis when speed of analysis is more important than a complete separation of all components in the sample. A window diagram based on retention indexes is the most useful for quickly evaluating the feasibility of a given pair of phases. The one with the most useful output is one based on partition ratios, as this can be used directly with the columns in hand. A PC-based spreadsheet program with integral specific retention volume data for the common liquid phases is described as a tool for selecting the optimum ratio of lengths for the columns in hand.
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  • 122
    ISSN: 0935-6304
    Keywords: Natural gas analysis ; Sulfur components ; Sulfur selective detection ; Universal detectors ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In the present contribution, the performance of a number of commercially available selective and universal detectors that can be used in the analysis of sulfur components in natural gas is evaluated in terms of sensitivity, selectivity, reproducibility, quenching effect, stability, and compound dependence of the sulfur response. Investigated detectors include the sulfur chemiluminescnce, the flame photometric, the electron capture, the mass spectrometric, the thermal conductivity, and the flame ionization detector. The sulfur chemiluminescence detector was found to have the best overall performance, e.g., low picogram amounts of sulfur can be detected accurately and the linear dynamic range is more than five orders of magnitude. After careful optimization, the sulfur response of this detector was found to be almost compound independent. All other detectors, including the flame photometric and the electron capture detector, have more or less compound dependent responses.
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  • 123
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    Journal of High Resolution Chromatography 18 (1995), S. 353-358 
    ISSN: 0935-6304
    Keywords: Chiral stationary phase ; Fluorocarbinol ; HPLC ; Enantiomeric separation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A chiral stationary phase (CSP) derived from anthrone is quite effective for the chromatographic resolution of the enantiomers of a wide variety of compounds. Denoted CSP 4, the phase is a chiral 2,2,2-trifluoro-1-(9-anthryl)ethanol tethered to silica by an elevencarbon-atom chain at the 10-position of the anthryl ring. CSP 4 typically provides greater enantioselectivity than its fluoroalcohol predecessor and is synthetically much more accessible.
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  • 124
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    Journal of High Resolution Chromatography 18 (1995), S. 348-352 
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Enantiomers ; Cyclodextrin polymer ; Organic modifiers ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Enantiomeric separation of some basic compounds, namely selegiline, amphetamine, and clenbuterol, was studied by capillary electrophoresis using an uncharged β-cyclodextrin polymer added to the background electrolyte at pH 2.5. Both complexation and resolution were influenced by the concentration of the chiral polymer confirming our previous results obtained in our earlier work for a wide number of pharmaceutical compounds. In this further study, we examined the influence of different organic additives to the background electrolyte on the enantioselectivity of the chiral selector, also using an extended number of analytes. In most cases, the use of an organic additive resulted in a decrease of resolution. However opposite to that, in some cases, e.g. ephedrine, the organic solvent proved to be essential to achieve enantiomeric resolution. Furthermore the influence of the capillary temperature on the resolution of the analytes was evaluated. Increase of temperature had a deleterious effect on the resolution of the enantiomers. For ephedrine, however, relatively high temperature (50 °C) proved to be advantageous, for the resolution of the optical isomers.
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  • 125
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    Journal of High Resolution Chromatography 18 (1995), S. 359-362 
    ISSN: 0935-6304
    Keywords: Derivatization of hydroxycarbamates ; Polar compounds in water ; Chemical ionization mass spectrometry ; n-Hexyl chloroformate ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A rapid and effective procedure, developed for the determination of polar compounds in water, has been applied to hydroxycarbamates. In few minutes, it is possible to perform a catalyzed derivatization of such compounds directly in the aqueous medium, using n-hexyl chloroformate. Extraction with n-hexane and injection into a benchtop GC-MS system are the only two further steps to complete the analysis. Chemical ionization proved to be more effective than electron impact to produce valuable mass spectra in terms of selectivity and sensitivity. Linear quantitative responses were demonstrated over a two-order-of-magnitude range. The minimum detectable concentration was 3 ppb for acetohydroxamic acid and 10 ppb for hydroxyurethane, obtained from Po river water samples spiked with the two hydroxycarbamate standards.
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  • 126
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    Journal of High Resolution Chromatography 18 (1995), S. 367-372 
    ISSN: 0935-6304
    Keywords: Fluvalinate residues ; Honey ; Gas chromatography-atomic emission detection (GC-AED) ; Gas chromatography-mass spectrometry (GC-MS) ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Two hyphenated techniques, gas chromatography-mass spectrometry and gas chromatography-atomic emission detection, have been used to identify the degradation products of the acaricide fluvalinate in a methanol solution of the commercially available formulation Mavrick, as well as in honey from beehives treated with this product. The major degradation products were 2-chloro-4-trifluoromethylaniline (I), methyl 2-[2-chloro-4-trifluoromethylaniline]-3-methylbutanoate (II), N-(2-chloro-4-trifluoromethyl-phenyl)valine (III), and 3-phenoxybenzaldehyde (IV). Fluvalinate in honey is gradually degraded, 3-phenoxybenzaldehyde being the most abundant residue.
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  • 127
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    Journal of High Resolution Chromatography 18 (1995), S. 452-454 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 128
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    Journal of High Resolution Chromatography 18 (1995), S. 455-455 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 129
    ISSN: 0935-6304
    Keywords: High Resolution GC and GC/MS ; Elsholtzia blanda chemotypes ; Elsholtzia communis ; Perilla frutescens chemotypes ; Essential oil compositions ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 130
    ISSN: 0935-6304
    Keywords: Benzotriazole ; Poly(vinyl chloride) ; Supercritical Fluid Chromatography ; Supercritical Fluid Extraction ; Tinuvins ; Internal standardization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 131
    ISSN: 0935-6304
    Keywords: Solid-phase microextraction ; Accelerants ; Fire debris ; Arson analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The current method of choice for the extraction of flammable or combustible liquid resides from fire debris samples is passive headspace concentration using activated charcoal strips (ACS) for adsorption of the liquid residues followed by elution with carbon disulfide or other suitable solvent. Presently, we report a new technique based on headspace solid-phase microextraction which has been successfully applied to the identification of a wide range of accelerants commonly seen in arson analysis. The SPME technique developed is simple, inexpensive, rapid, and eliminates the use of the highly flammable and toxic solvent carbon disulfide. Results using this SPME method have been directly compared to results obtained via the ACS technique for light, medium, and heavy petroleum distillates as well as gasoline. All of the accelerants studied were accurately identified by the SPME method with equal or greater sensitivity compared to the ACS method.
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  • 132
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    Journal of High Resolution Chromatography 18 (1995), S. 659-664 
    ISSN: 0935-6304
    Keywords: Capillary zone electrophoresis ; Electrokinetic chromatography ; Enantiomer separation ; Binaphthyl compounds ; Cyclodextrin ; Bile salt ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The capillary electrophoretic (CE) separation of the enantiomers of three binaphthyl compounds is investigated. Several CE modes such as cyclodextrin (CD) modified capillary zone electrophoresis (CZE) (CD-CZE), micellar electrokinetic chromatography (MEKC), cyclodextrin electrokinetic chromatography (CD-EKC), etc. are employed for the simultaneous enantiomer separation of the three solutes. The successful separation was achieved by combining two modes, in other words by using more than two chiral selectors. A development of the CE enantiomer separation is demonstrated for the binaphthyl compounds. The enantioselectivity of binaphthyl compounds is alo briefly discussed.
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  • 133
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    Journal of High Resolution Chromatography 18 (1995), S. 510-510 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
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  • 134
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    Journal of High Resolution Chromatography 18 (1995), S. 513-513 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
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  • 135
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    Journal of High Resolution Chromatography 18 (1995), S. 667-669 
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Chemiluminescence ; Indirect detection ; Amino acids ; Peptide ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 136
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    Journal of High Resolution Chromatography 18 (1995), S. 685-691 
    ISSN: 0935-6304
    Keywords: On-line LC-GC-MS ; PCBs ; Non-ortho CBs ; Human blood plasma ; Dinitroanilinopropyl modified silica ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method for the determination of non-, mono- and di-ortho substituted polychlorinated biphenyls in human blood plasma is presented. The non-ortho CBs are isolated from the bulk of PCBs by HPLC on a dinitroanilino-propyl silica column and collected as a heart-cut fraction that is transferred on-line to GC-MS utilizing concurrent solvent evaporation technique. The on-line coupling serves to lower the limit of determination and to partly automate the sample clean-up. The di- and mono-ortho CBs are analyzed by off-line GC-ECD using two different columns. Sample pre-treatment is performed by extraction with organic solvents and fractionation on silica gel. A high reproducibility and an absolute over-all recovery of approximately 70 % is demonstrated. The method is applied to samples of blood from 5 individuals. All the samples demonstrated a similar relative concentration profile. It was also shown that three CB congeners (CB 126, CB 156 and CB 170) contributed to the major part of the toxic equivalent quantity of the PCB content in the blood.
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  • 137
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    Journal of High Resolution Chromatography 18 (1995), S. 695-698 
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Tetracycline ; Antibiotics ; Related substances ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tetracycline was separated from its main impurities 4-epitetracycline, anhydrotetracycline, 4-epianhydrotetracycline, chlortetracycline, and demethyltetracycline by capillary electrophoresis. Systematic method development was performed in which following parameters were consecutively optimized: type and pH of the buffer, buffer concentration, type and concentration of organic modifier, voltage and temperature. Qualitative and quantitative aspects of the method are compared with liquid chromatography.
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  • 138
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    Journal of High Resolution Chromatography 18 (1995), S. 705-708 
    ISSN: 0935-6304
    Keywords: Capillary GC-MS ; Metabolism ; Oxabolone ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The metabolism of oxabolone cipionate, 17-(3-cyclopentyl-1-oxopropoxy)-4-hydroxyestr-4-en-3-one, a synthetic anabolic steroid, was investigated in man, the cumulative urinary excretion and the metabolism of the compounds being studied by GC-MS in both electron impact and chemical ionization modes. After administration by injection to volunteers, five different metabolities were detected in urine. The metabolites and the parent compound were detected in urine up to a week after administration.
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  • 139
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    Journal of High Resolution Chromatography 18 (1995), S. 635-642 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Emission control ; Humid samples ; Adsorptive sampling ; Hydrophobic adsorbents ; Thermal desorption ; Volatile organic compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Adsorptive enrichment on hydrophobic adsorbents, thermal desorption, and capillary gas-chromatographic analysis have been used to determine volatile organic compounds in extremely humid stack-gas emissions from the residential burning of brown-coal briquets. One hundred and fifty two compounds were identified and quantified. Quantitative emission factors were determined for the identified individual compounds in relation to the amount of the fuel used. These factors enable a first assessment of the pollution of the city of Leipzig with volatile organic compounds resulting from the burning of indigenous lignite.
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  • 140
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    Journal of High Resolution Chromatography 18 (1995), S. 630-634 
    ISSN: 0935-6304
    Keywords: GC ; Enantiomer separation ; Thermal stability ; Chiral stationary phase ; Metal capillary column ; Glass capillary column ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A chiral stationary phase prepared by bonding L-valine-t-butylamide to XE-60 has been coated on glass and metal capillaries. The performances of the chiral glass and metal columns were equivalent to those of commercial fused silica capillary columns. The thermal stability of the glass column was examined up to 280°C. It was found that no appreciable change in separation factor (α value) was observed up to 230°C. The α values gradually decreased between 240 and 260°C, and enantiomer separation was no longer achieved at 280°C. It was concluded that the allowable upper limit temperature of the chiral stationary phase is between 230 and 240°C in the isothermal mode, and ca 260°C in temperature-programmed mode.
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  • 141
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    Journal of High Resolution Chromatography 18 (1995), S. 760-760 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
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  • 142
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; High performance liquid chromatography ; Alkyl-nitrile phases ; Lipid oxidation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 143
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    Journal of High Resolution Chromatography 18 (1995), S. 647-652 
    ISSN: 0935-6304
    Keywords: GC-MS ; PCB Substitute ; Waste mineral oil ; Ugilec 141 ; Dichlorobenzyldichlorotoluenes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: After the restrictions on production and use of PCBs, Ugilec 141, a technical mixture of dichlorobenzyldichlorotoluenes (DBDTs), has been used as a PCB substitute in hydraulic systems. In the Netherlands, the production, import and use of Ugilec 141 has been forbidden since 1988. A method has been developed for the analysis of Ugilec 141 in waste mineral oils to control waste oil import and processing.The method development was based on modification of procedures for the analysis of PCBs in oil and dioxins in fatty matrices and analysis was performed with gas chromatography with mass spectrometry. For sample clean-up, several combinations of column chromatography with activated carbon, alumina, and silica gel have been tested to obtain extracts free from matrix interferences. An internal standard of 13C-labeled DBDT was examined to check recoveries from the clean-up procedures. Quantification was performed by comparison with the six most abundant peaks of an external Ugilec 141 standard mixture. Validation experiments showed a linear range from 0.25 to 60 mg Ugilec 141 kg-1 oil, a reproducibility of 3% and a limit of determination of 0.25 mg Ugilec 141 kg-1 waste oil.The method was applied in a survey of 70 samples of waste mineral oils from producers all over the Netherlands; this revealed levels below the limit of determination and one positive sample with a concentration of 5.7±0.1 mg Ugilec 141 kg-1 oil. In an inspection inquiry, one contaminated oil was found containing 116 ± 9 g Ugilec 141 kg-1 oil.
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  • 144
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    Journal of High Resolution Chromatography 18 (1995), S. 666-666 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
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  • 145
    ISSN: 0935-6304
    Keywords: HPLC ; Reversed phase ; 4-Methyl-5-vinylthiazole ; Phenolic derivatives ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 146
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    Journal of High Resolution Chromatography 18 (1995), S. 725-726 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Column technology ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 147
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    Journal of High Resolution Chromatography 18 (1995) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
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  • 148
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    Journal of High Resolution Chromatography 18 (1995), S. 753-756 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Electronic flow controller ; Advanced flow controller (AFC) ; Pressure programming ; Flow programming ; Automatic optimization ; Split injection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An electronic gas-flow controller system called Advanced Flow Control (AFC), which controls not only carrier gas pressure at the column inlet but also the total gas flow including the split flow, was designed and evaluated. BASIC programming of repetitive analyses of standard mixtures under varied split ratios and pressure programs allowed automated optimization of those conditions for the desired column loading and resolution between adjacent peaks.
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  • 149
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    Journal of High Resolution Chromatography 18 (1995), S. 757-759 
    ISSN: 0935-6304
    Keywords: CGC, ECD ; Ammonia, nitrogen ; Chlorophenols, nitro-aromatic compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The effect of ammonia on the electron capture detector (ECD) response has been investigated. Nitrogen with different ammonia concentrations (5-20%) was used as make-up gas. Compared to pure nitrogen, the ECD response decreased when the ammonia concentration in the make-up gas was 5%. However, the response increased when the ammonia concentration was 20%. The response factor of 4-chlorophenol increased 4 fold when ammonia was 20%. Also, di- and tri-chlorophenols increased by 30-50%. The nitroaromatic compounds responses increased by about 2-3.7 times with 20% ammonia in the make-up gas. The signal-to-noise (S/N) increased when 20% ammonia in nitrogen was used as make-up gas compared to pure nitrogen. Also, the detector linearity increased by 50% with ammonia.
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  • 150
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Solid phase microextraction ; Aqueous phase derivatization ; Tin-selective FPD ; Organotin speciation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 151
    ISSN: 0935-6304
    Keywords: Capillary GC ; Milkfat triglycerides ; PTV split and cold on-column ; Quantitation ; 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 18 (1995), S. 776-780 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography, mass spectrometry ; Purge and trap ; Apple juices ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 153
    ISSN: 0935-6304
    Keywords: GC ; Stationary phases ; Cyanobiphenyl phase ; Polychlorinated biphenyls ; Reference Materials ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A novel p,p-cyanobiphenyl stationary phase (p-cyanobiphenyl, p-allyloxy methylpolysiloxane) has been evaluated for the GC investigation of polychlorinated biphenyls (PCBs). Several PCB congeners which coelute on the phases typically used for PCB analysis (e.g. 5% phenyl methylpolysiloxane) are separated on the p,p-cyanobiphenyl phase, including the hexachlorobiphenyl congeners PCB 163, PCB 164, and PCB 138. In this work, a p,p-cyanobiphenyl stationary phase was used to measure selected PCB congeners in two Standard Reference Materials (SRMs) available from the National Institute of Standards and Technology (NIST), and two Certified Reference Materials (CRMs) available from the Community Bureau of Reference (BCR). The materials analyzed were SRM 1588, Organics in Cod Liver Oil; SRM 1945, Organics in Whale Blubber; CRM 349, Chlorobiphenyls in Cod Liver Oil; and CRM 350, Chlorobiphenyls in Mackerel Oil. Concentrations are reported for several PCB congeners which coelute on the 5% phenyl methylpolysiloxane, including PCB 163 and PCB 164.
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  • 154
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    Journal of High Resolution Chromatography 18 (1995), S. 97-100 
    ISSN: 0935-6304
    Keywords: HPLC ; Gradient elution ; Cyano bonded phase ; Polymerized vinyl alcohol bonded phase ; Plant tissue ; Potato ; Lipid classes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The wide range of lipid classes found in plant tissues, including simple lipids, glycolipids, and phospholipids, have been resolved by gradient high performance liquid chromatography with evaporative light-scattering detection. The lipids from potato tubers were used to optimize the separations. Adsorption chromatography with silica gel gave disappointing results for the plant glycolipids. Much better separations were obtained with chemically bonded stationary phases, e.g. those with propionitrile or polymeric vinyl alcohol as the functional moiety. With careful calibration, good reproducibility was possible. Only highly acidic lipids such as phosphatidylserine still present some problems.
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  • 155
    ISSN: 0935-6304
    Keywords: High resolution capillary GC ; High resolution GC-MS ; Essential oil analysis ; Ylang-ylang oil composition ; Cananga odorata ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Volatile secondary metabolites from Colombian ylang-ylang flowers were obtained by combined steam distillation - solvent extraction. The samples were analyzed by high resolution gas chromatography with flame ionization, nitrogen/phosphorus, or mass spectrometric detection. The chemical composition of the oils extracted from flowers at different stages of development differed both qualitatively and quantitatively. The generation of total volatile metabolites, light oxygenated compounds in particular, increased markedly during flower maturation. In this work the quality of the ylang-ylang essential oils was studied as a function of flower maturity.
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  • 156
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    Journal of High Resolution Chromatography 18 (1995), S. 105-107 
    ISSN: 0935-6304
    Keywords: Analytical methodology ; Positional isomers ; Silver and silver compounds ; Triglycerols ; Liquid chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Silver ion chromatography, utilizing two commercially available HPLC columns connected in series, was used to separate a variety of triacylglycerol positional isomers. The isomers had a fatty acid composition of ABA and AAB, where A and B were fatty acids containing zero to three double bonds. Isocratic solvent systems of 0.5% to 1.0% acetonitrile in hexane were used to separate the triacylglycerol isomers. This methodology can be used to rapidly determine the isomeric purity of synthesized or isolated triacylglycerols and to isolate specific positional isomers.
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  • 157
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    Journal of High Resolution Chromatography 18 (1995), S. 108-110 
    ISSN: 0935-6304
    Keywords: GC/Atomic Emission Detection (GC/AED) ; Reformulated gasolines ; Selective analyses of oxygenates ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A GC method for the determination of oxygenated additives in reformulated gasolines (RFG) is described. The method uses on-column injection and atomic emission selective detection of oxygenates using the 777 nm NIR emission line. Detection limits are approximately 10 ppm oxygen. Results compared well with other techniques, such as GC/FTIR.
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  • 158
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Poly(dimethyl diphenyl siloxane) phases ; Temperature program optimization ; Organophosphorus and organonitrogen pesticides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The CGC analysis of 25 organophosphorus and organonitrogen pesticides was optimized on two different stationary phases, namely a 5% diphenyl dimethyl silicone (SE-54 type) and a 50% diphenyl dimethyl silicone (OV-17 type) by selecting the best temperature program conditions, using computer simulation.
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  • 159
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    Journal of High Resolution Chromatography 18 (1995) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 160
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    Journal of High Resolution Chromatography 18 (1995), S. 141-151 
    ISSN: 0935-6304
    Keywords: Chlorobiphenyl congeners ; Isomer specific capillary column gas chromatography ; Stationary phases ; Single column and multi-column techniques ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: High resolution gas chromatography has greatly changed the field of polychlorinated biphenyl (PCB) analysis. From a rough estimation of the total PCB concentration on packed column GC, the development of commercially available fused silica capillary columns in the late 1970s and early 1980s has advanced the analysis of PCBs to a point where they can be accurately measured as separated congeners. The state-of-the-art of PCB analysis in the 1990s is routine isomer-specific analysis with multi-column techniques using long (〈50 m) narrow (〉 0.25 mm) columns. A broad spectrum of commercially available stationary phases have been completely characterized with regard to their PCB elution profiles.
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  • 161
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    Journal of High Resolution Chromatography 18 (1995), S. 161-166 
    ISSN: 0935-6304
    Keywords: Solid phase microextraction (SPME) ; High-speed gas chromatography ; Headspace solid phase microextraction ; BTEX ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Solid phase microextraction (SPME) was used as the sample introduction technique for high-speed isothermal GC. An injector dedicated for SPME fiber injection was designed and built. The injector was operated in two modes, continuously heated and flash heated. The latter mode proved to be better for high-speed separations. The injector was then used for sample introduction in separation of BTEX. When sampling directly from water with a fiber having a 56 μm thick poly(dimethylsiloxane) coating, the BTEX components were separated under isothermal conditions in ca. 18 s. A fiber with a thinner coating (15 μm) enabled the separation to be completed in ca. 12 s when sampling from headspace. In both cases the results were highly reproducible, as measured by the estimated values of the relative standard deviation.
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    Journal of High Resolution Chromatography 18 (1995), S. 266-266 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 163
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    Journal of High Resolution Chromatography 18 (1995), S. 267-268 
    ISSN: 0935-6304
    Keywords: HPLC ; Rape seeds ; Rapeseed meal ; Phytic acid ; Inositol phosphates ; 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 18 (1995), S. 269-270 
    ISSN: 0935-6304
    Keywords: Micellar electrokinetic chromatography (MEKC) ; Rhei Rhizoma ; Aurantii Fructus Immaturus ; Magnoliae Cortex ; Hsiao-cheng-chi-tang ; Bioactive components ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 165
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    Journal of High Resolution Chromatography 18 (1995), S. 15-18 
    ISSN: 0935-6304
    Keywords: Ozone removal ; Potassium iodide ozone trap ; Artifact formation ; Organic iodine compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Trace atmospheric gases have been sampled using potassium-iodide-based reactant traps for ozone removal. GC-MS analysis revealed the presence of organic iodine compounds which were present neither in the atmosphere nor as contaminants of the materials used, but more likely arose from reactions of organic gases or aerosols sampled with reactive iodine or hypoiodite released from reaction of ozone with potassium iodide in the traps. Losses of the individual organic trace gases measured were not, however, observed as a result of this mechanism. Several cautions in identifying unknown compounds from the atmosphere when using potassium iodide ozone traps are discussed.
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  • 166
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    Journal of High Resolution Chromatography 18 (1995), S. 28-32 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Isotope ratio MS ; GC-on-line combustion ; IRMS-ITD coupling ; GC capillary eluate splitting ; Organic acids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An isotope ratio mass spectrometer and an ion trap mass spectrometer have been coupled in parallel to one gas chromatograph. Using this arrangement both the 13C/12C ratio and the mass spectrum of a given compound can be measured simultaneously under identical gas chromatographic conditions. Although column connection fittings are employed to split the capillary eluate, chromatographic performance was barely impaired. Development of the system has been monitored by recording δ13C values of the constituents of Grob test mixture no. 2. The accuracy and reliability of system performance has also been tested.
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  • 167
    ISSN: 0935-6304
    Keywords: On-line extraction ; Large volume introduction ; Capillary gas chromatography ; Atomic emission detection ; Solvent venting ; Pesticides ; Ground water ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The on-line coupling of a liquid-liquid extraction system with capillary gas chromatography using atomic emission detection (GC-AED) has been studied. The required large volumes of about 100 μl of an iso-octane solution can be introduced into the GC-AED system by using the AED solvent vent and a solvent vapor exit in front of the capillary analytical column. Test solutions containing several pesticides were detected using the carbon, chlorine, nitrogen and sulfur channels. Analyte detectability (in concentration units) was improved significantly and low concentractions of the test compounds could be determined (1-5 ng/ml). Aqueous samples were on-line extracted and analyzed. The precision of the large-volume injection itself as well as the total extraction-GC-AED system was satisfactory (RSD of ca. 2 and 4%, respectively). As a real-life application, several ground water samples were screened.
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  • 168
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    Journal of High Resolution Chromatography 18 (1995), S. 403-412 
    ISSN: 0935-6304
    Keywords: High resolution GC ; Apolar phase ; Alkanes ; Napthenes ; Aromatics ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This paper deals with the separation of alkanes, naphthenes, and aromatic compounds in naphtha and reformate, on a newly developed apolar high resolution GC column. The selectivity of this apolar phase has been compared with those of squalane, DB-1, and SE-30. A total of 95 hydrocarbons were reliably identified, mostly by GC-MS. Repeated measurements of Kováts retention indices are presented as evidence for the reproducible manufacture of fused silica columns coated with this phase.
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  • 169
    ISSN: 0935-6304
    Keywords: cis-13-Eicosenoic Acid (Paullinic Acid) ; Cyanolipids ; Fatty acids ; GLC-MS ; NMR spectroscopy ; Oxazoline derivatives ; Paullinia elegans Sapindaceae ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The fatty acids of the total lipids, triglycerides, and the cyanolipid of Paullinia elegans (Sapindaceae) have been analyzed as their methyl esters and 4,4-dimethyloxazoline derivatives by gas chromatography-mass spectrometry. It was shown that the gas chromatographic separation of the oxazoline derivatives was sufficient to ensure the correct identification of the monoenic fatty acid positional isomers. Stereochemistry of the double bonds has been confirmed by infrared and 13C-nuclear magnetic resonance (NMR) spectroscopy. cis-13-Eicosenoic Acid (Paullinic acid) (44.4%) and cis-11-octadecenoic acid (cis-vaccenic acid) (19.8%) were found to be the main components beside other monoenoic acid positional isomers. The cyanolipid of P. elegans was identified as 2,4-dihydroxy-3-methylenebutyronitrile derivative by IR, 1H-NMR, 13C-NMR spectroscopy and was quantified by 1H-NMR spectroscopy (71.4%).
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  • 170
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    Journal of High Resolution Chromatography 18 (1995), S. 422-424 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Internal standard (IS) ; Temperature programming ; OV-17 ; m-Phenoxybenzaldehyde ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A capillary GC method employing an internal standard has been developed and successfully used for quantitative determination both of the raw materials used for the manufacture of m-phenoxybenzaldehyde and for the components of the reaction mixtures obtained at various stages of the development of the process. A complete analysis can be performed in a single temperature programmed run.
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    Journal of High Resolution Chromatography 18 (1995), S. 425-432 
    ISSN: 0935-6304
    Keywords: GC ; GC-MS ; Micro-LC ; SEC ; Crude tall-oil ; Fatty acids ; Resinic acids ; Unsaponifiable matter ; Dimers ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Chromatographic methods currently used for isolation, separation, and identification of the components of crude tall-oil have been reviewed, and their resolution and analytical methodology compared. Sample introduction by cold on-column, rather than vaporizing, injection provides good reproducibility and operational convenience for capillary GC analysis. Size exclusion chromatography for isolation followed by capillary GC-MS for identification, gave the best performance for analysis of acidic and dimeric compounds.
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  • 172
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    Journal of High Resolution Chromatography 18 (1995), S. 439-442 
    ISSN: 0935-6304
    Keywords: Electrokinetic chromatography (EKC) ; Pseudo-stationary phase ; Electroosmotic flow ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 18 (1995), S. 433-438 
    ISSN: 0935-6304
    Keywords: On-line LC-GC ; Reversed-phase HPLC ; Programmed Temperature Vaporizer (PTV) ; Sterols ; Factorial design ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An on-line reversed-phase LC-GC method involving the use of a Programmed Temperature Vaporizer (PTV) as interface is used for the rapid analysis of sterols. The experimental procedure requires only the use of commercial HPLC and GC equipments and a Rheodyne valve. The LC preseparation can be performed satisfactorily even with aqueous eluents containing up to 25% water. Factorial experimental design is applied to investigate the sensitivity achievable in the analysis with some variables (adsorbent material used in the PTV, particle size and plug length) being considered at two different levels. As a result, the sensitivty can be increased by a factor as large as 35 merely by performing the analysis under the experimental conditions giving the highest response. The use of the proposed configuration allows the transfer of up to 1050 μL from LC into the GC system, 1400 μL/min being the speed of sample introduction. The proposed procedure was succesfully applied to the analysis of real samples.
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  • 174
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    Journal of High Resolution Chromatography 18 (1995), S. 443-445 
    ISSN: 0935-6304
    Keywords: Micellar Electrokinetic Chromatography (MEKC) ; Ionic polymer ; Polycyclic aromatic hydrocarbons (PAHs) ; Alkylphenones ; Fullerenes ; 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 18 (1995), S. 446-448 
    ISSN: 0935-6304
    Keywords: Supercritical fluid extraction (SFE) ; Aqueous media ; Modifiers ; Phenoxy acids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 176
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    Journal of High Resolution Chromatography 18 (1995), S. 456-456 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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  • 177
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    Journal of High Resolution Chromatography 18 (1995) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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  • 178
    ISSN: 0935-6304
    Keywords: Supercritical fluid extraction ; Series-coupled column gas chromatography ; Chemometric classification ; Semivolatile flavor compounds ; Cinnamon ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Solvent-assisted supercritical fluid extraction is superior to Soxhlet extraction, solvent extraction at reflux, and simultaneous setam distillation solvent extraction for the isolation of semivolatile compounds from the cinnamons of commerce. Optimized extraction conditions are described using carbon dioxide at 300 atm and 70°C to extract 0.5 g of powdered cinnamon mixed with 4.5 g of anhydrous sodium sulfate to which 1.0 ml of acetonitrile was added at the start of the sequential 30 min static and 30 min dynamic extraction. The semivolatile compounds were collected by solvent trapping in ethyl acetate and analyzed directly by series coupled-column gas chromatography after filtration and partial solvent evaporation. Twenty-one compounds identified by mass spectrometry were quantified in twenty-four samples of cinnamon and cassia purchased in Sri Lanka, Korea, United Kingdom, and the United States of America. True cinnamon is easily distinguished from cassia by the presence of eugenol, absence of δ-cadinene, much lower amounts of coumarin, and larger amounts of benzyl benzoate. Principal component analysis using the relative composition of the twelve major semivolatile compounds provides a clear distinction between true cinnamon and cassia as well as useful interspecies differences which can be used for further classification.
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  • 179
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    Journal of High Resolution Chromatography 18 (1995), S. 483-489 
    ISSN: 0935-6304
    Keywords: Supercritical-Fluid Extraction (SFE) ; Supercritical-Fluid Chromatography (SFC) ; Recovery ; Optimization ; Retention Data ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The possibility of using supercritical-fluid chromatographic retention data for examining the effects of operational parameters, such as pressure and flow rate, on the extraction characteristics in supercritical-fluid extraction (SFE) was investigated. A model was derived for calculating the extraction efficiency in SFE from retention data and peak shapes measured in supercritical-fluid chromatography (SFC). By performing the SFC experiments at the same pressure and temperature as the SFE extractions using the SFE extraction cell as the SFC column, an accurate prediction of extraction efficiencies could be made. Finally, the effects of matrix composition and analyte concentration on extraction efficiency were studied.
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  • 180
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    Journal of High Resolution Chromatography 18 (1995), S. 490-494 
    ISSN: 0935-6304
    Keywords: Capillary gas-chromatography ; Splitless injection discrimination ; Electronic pressure programming ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Hydroxylated polychlorobiphenyls (polyhydroxy-PCBs) are subjected to severe discrimination effect when they are introduced into a capillary gas chromatograph by splitless injection. This effect can be considerably reduced by using a pulsed pressure injection to favor sample transfer and by further programming the eluent gas pressure during the GC run. By multistep gas pressure programming, splitless injection provides analytical performances and chromatograms for (poly)hydroxy-PCBs closely resembling those obtained by on-column injection, whose use is generally discouraged with real environmental samples. Among the six model compounds studies, the dihydroxy congeners exhibit the best results.
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  • 181
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    Journal of High Resolution Chromatography 18 (1995), S. 500-500 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Topics: Chemistry and Pharmacology
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  • 182
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    Journal of High Resolution Chromatography 18 (1995), S. 501-503 
    ISSN: 0935-6304
    Keywords: High resolution GC-MS ; Mass spectrometry ; Anise oil ; Catalytic transformation ; Zeolite Y ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 183
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    Journal of High Resolution Chromatography 18 (1995), S. 504-506 
    ISSN: 0935-6304
    Keywords: High-temperature gas chromatography (HTGC) ; Capillary columns, fused silica ; Base leaching ; Poly(dimethyl/diphenyl)siloxane ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 184
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    Journal of High Resolution Chromatography 18 (1995) 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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  • 185
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    Journal of High Resolution Chromatography 18 (1995), S. 525-534 
    ISSN: 0935-6304
    Keywords: Natural gas analysis ; Sulfur components ; Adsorption-purge-thermal desorption ; Programmed temperature vaporizer ; Ultra-thick film apolar capillary column ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Determination of trace concentrations of sulfur components in natural gas is a true analytical challenge. Only analytical procedures based on gas chromatography can meet the sensitivity and accuracy requirements dictated by environmental regulation institutions and modern chemical industry. In the present contribution the sample pretreatment and chromatographic separation steps have been evaluated and optimized based on the use of a flamebased sulfur chemiluminescence detector (SCD) for target compound detection.The proposed instrument consists of a programmed temperature vaporizing (PTV) injector employing a liner packed with Chromosorb 104, a 4 μm thick film apolar column and a flame-based SCD. Using a 13 mL sample loop the detection limit achievable with the new method is 3 μg S/m3. The precision of replicate measure. ments is generally in the range of 5-15% relative standard deviation. Lower detection limits can be achieved by preconcentrating larger sample volumes, e.g. 100 mL.
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  • 186
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    Journal of High Resolution Chromatography 18 (1995), S. 535-539 
    ISSN: 0935-6304
    Keywords: Coupled LC/GC ; Solid phase extraction ; Automated SPE/GC ; Co-solvent effect ; NP-pesticides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In order to meet the requirements of analyzing very low concentrations of pesticides in water (typically at 0.1 μg/l or less), samples have to be concentrated prior to GC-analysis. Samplie pre-concentration by off-line methods based on solid phase extraction (SPE) or liquid-liquid extraction are very time consuming and cumbersome. Moreover, the quantitative performance of the analytical method as a whole in terms of accuracy and reliability is seriously hindered by elaborate, manually performed sample pre-treatment steps. This paper describes an automated method based on solid phase extraction and capillary gas chromatography. The technique was applied for the analysis of 31 polar organophosphorus and organonitrogen pesticides. A commercially available HPLC/GC instrument is modified, using the LC-part for solid phase extraction. The sample, of which only a few ml's is required to obtain sufficiently low detection limits, is delivered by a robotic large volume autosampler. After solid phase extraction and elution, the eluate is transferred into the GC via a so called “loop type interface”. In this paper the instrumentation and analytical methodology is described, as well as the main validation results. The quantitative performance (i.e. recovery and repeatability) of the most polar solutes like metamitron and dimethoate appears to be better than obtained with off-line SPE as a result of the more beneficial ratio between the amount of sorbent and the sample volume. As the loop-type interface causes losses of the most volatile compounds, a co-solvent is added. This co-solvent provides sufficient trapping capacity in the capillary pre-columns to allow quantitative analysis of even the most volatile pesticides. Moreover a better separation of early eluting compounds is also established.
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  • 187
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Capillary zone electrophoresis ; Micellar electrokinetic capillary chromatography, MECC, MEKC ; Selectivity optimization ; Systematic method development ; Multi-parameter optimization ; Iterative regression design ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An iterative regression design has been used in the optimization of selectivity in capillary zone electrophoresis and micellar electrokinetic capillary chromatography. This strategy, initially developed for HPLC, is modified in respect of the choice of the parameter(s) and the parameter space and the description of the migration behavior of (charged) solutes in capillary electrophoresis. The six test solutes could not be fully resolved by adjusting the pH in a free zone system but the simultaneous two-parameter optimization of the pH and the concentration of surfactant resulted in baseline separation of all the solutes. Further improvement may be obtained when distorted peak shapes are also considered at the level of the parameter choice and the criterion.
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  • 188
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    Journal of High Resolution Chromatography 18 (1995), S. 582-586 
    ISSN: 0935-6304
    Keywords: Allergen ; Wasp venom ; Phleum pratense and Betula verrucosa pollen ; Capillary electrophoresis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A CE method has been developed for the analysis of wasp venoms and pollen extracts of Phleum pratense and Betula verrucosa. Various electrolyte systems can be used but the best separation and reproducibility are attained in 0.15 mol/l phosphoric acid, pH 1.8. UV photometric detection at 190 nm is sufficiently sensitive for determination of the polypeptides and glycoproteins contained in these materials (the detection limit for phospholipase A2 is 0.4 ng). The allergens from wasp venoms and pollen extracts yield characteristic electropherograms which can be used for control of the allergen production. Modification of capillary wall with poly(ethylhydroxy methacrylate) causes a decrease in the migration times and the separation efficiency is retained.
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  • 189
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    Journal of High Resolution Chromatography 18 (1995), S. 593-596 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Temperature programming ; Retention simulation ; Compound identification ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Conversion of Kováts retention indices on a given stationary phase into the thermodynamic parameters of compounds on a given column leads to a simplified method for retention simulation in isothermal, linear, and multi-ramp temperature programmed capillary gas chromatography. The influence of numerical methods used in the computation, the temperature coefficient of Kováts indices, and the experimental factors such as isothermal temperatures selected in the measurement of n-alkanes, column characterization and sample overloading, on the reproducibility and accuracy of simulation were discussed and examined. When the column used is properly characterized, the error between the simulated values and the experimental data is within ± 0.5 index unit or less than ± 1% of retention time.
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    Journal of High Resolution Chromatography 18 (1995) 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
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  • 191
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    Journal of High Resolution Chromatography 18 (1995), S. 721-724 
    ISSN: 0935-6304
    Keywords: Packed column supercritical fluid chromatography ; Capillary supercritical fluid chromatography ; Large volume injection ; Solvent elimination ; Solid-phase injection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 18 (1995), S. 573-578 
    ISSN: 0935-6304
    Keywords: Large sample volumes ; Vaporizing chambers ; Evaporation rates ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The suitability of some chambers for sample evaporation at high input flow rates (〉100 μl/min) was studied by visual experiments. The chambers were at temperatures far above the solvent boiling point in order to achieve the heat transfer required. Shooting liquid owing to violent evaporation, flooding of the chamber as a result of cooling, and excessively high vapor pressure causing backflow into the gas supply system were found to be the limiting factors. Fused silica capillaries into which a piece of wire or polyimide-free fused silica capillary had been inserted were found to be suitable for the vaporization of “easy” solvents, such as alkanes (up to some 1.7 ml/min), but packed beds were required to achieve favorable evaporation of dichloromethane or methanol/water (up to some 800 and 300 μl/min, respectively).
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  • 193
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    Journal of High Resolution Chromatography 18 (1995), S. 579-581 
    ISSN: 0935-6304
    Keywords: Deactivation ; Packed column SFC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Residual adsorptive activity of reversed phase (RP) column packings used in supercritical fluid chromatography (SFC) can be significantly reduced by a dynamic in-situ silanization with diphenyltetramethyldisilazane (DPTMDS). RP-materials thus deactivated were characterized both chromatographically and by solid-phase 29Si NMR.
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  • 194
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    Journal of High Resolution Chromatography 18 (1995), S. 643-646 
    ISSN: 0935-6304
    Keywords: Gas chromatography/Mass spectrometry ; Chiral GC ; Deuterium-labeled compounds ; Hexachlorocyclohexane ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Perdeuterated α-1,2,3,4,5,6-hexachlorocyclohexane (α-PDHCH) was synthesized and isolated in pure form. α-PDHCH was baseline separated from unlabeled α-HCH by high resolution gas chromatography on different stationary phases. α-PDHCH was also resolved into its enantiomeric forms by application of a chiral GC phase. Furthermore, chiral chromatography of a mixture of labeled α-PDHDH and unlabeled α-HCH resulted in four peaks. Standard solutions of α-PDHCH are recommended both as recovery standard for sample clean-up and as internal standard for the quantitation of chlorinated hydrocarbons with GC/MS or GC/ECD in environmental samples.
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    Journal of High Resolution Chromatography 18 (1995), S. 784-784 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 196
    ISSN: 0935-6304
    Keywords: Solid-phase microextraction ; Distribution coefficients ; Drinking water ; Equilibration ; Temperature dependency ; VOC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Solid-phase microextraction (SPME) has been applied to the quantitative analysis of 60 volatile organic compounds (VOCs) in drinking water. Equilibration curves for the partitioning of the VOCs between the fiber coating and fortified water obtained at 20, 50, and 80 °C are found between the theoretical curves for completely agitated and non-agitated samples. Two important factors for the amount adsorbed by the SPME fiber coating are the extraction time and the fiber coating/water distribution coefficient, KFW. Both depend on the sample temperature, but in a counteracting manner: Increasing the temperature shortened the equilibration times, especially for the heavier VOCs, but also lead to lower KFW values, and consequently a lower sensitivity of the method. KFW values are determined for 33 of the VOCs at 40, 60, and 80°C and the heats of adsorption,-ΔH, are calculated. The nature of the adsorption is found to be exothermic which explains the decreasing sensitivity of the method with increasing temperature. Detection limits were typically from 20 ng/l to 200 ng/l, except for the very light VOCs with which detection difficulties were encountered. For all of the VOCs the linear range extended from the lowest concentration at which they were actually detected to at least 5 mg/l. The precision, 3% average standard deviation when an internal standard was used, was satisfactory for most quantitative routine analysis. SPME was also applied to head-space (HS) analysis of drinking water through the coupled equilibrium between water/head-space/fiber coating. HS-SPME is demonstrated to have shorter equilibration times than SPME directly from the water and equal sensitivities, except for the very light VOCs. Water samples from a drinking water plant contaminated in the low μg/l range with 1,1,1-trichloroethane, trichloroethene and tetrachloroethene were analyzed. There seems to be a reasonable agreement between results obtained by SPME and purge & trap. It is concluded that SPME has a great potential for drinking water analysis.
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    Journal of High Resolution Chromatography 18 (1995), S. 653-658 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Mass spectrometry ; Fragrance analysis ; Cosmetics ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A gas chromatographic (GC)-mass spectrometric (GC-MS) method has been developed for the routine analysis of 11 fragrance substances in cosmetics: cinnamic alcohol, cinnamic aldehyde, eugenol, hydroxy citronellal, α-amyl cinnamic aldehyde, geraniol, isoeugenol, coumarin, dihydrocoumarin, citronellal and citral. Methods for sample preparation of various types of cosmetic products, prior to GC analysis, have also been developed and proved to be rugged. Detection limits of all of target fragrance substances were approximately 1 ppm. Calibration curves of the target fragrance substances analyzed by GC were found to be linear in the investigated concentration range, 0.005% - 0.50%. The recoveries of the target fragrances from various types of cosmetic products were 80% - 116% and the relative standard deviations of the quantitative analysis of the target fragrance substances were within 5%.
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  • 198
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    Journal of High Resolution Chromatography 18 (1995), S. 675-678 
    ISSN: 0935-6304
    Keywords: Capillary zone electrophoresis (CZE) ; Stacking effect ; Cationic surfactant ; Cr(VI) ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 18 (1995), S. 692-694 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Intestinal permeability ; Urine ; Sugars ; Lactulose ; Mannitol ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Alteration of intestinal permeability towards compounds like sugars is an indication of abnormalities observed in some diseases. Measurement of the dual sugar absorption of lactulose and mannitol is a non-invasive test of intestinal permeability. The use of this test is however limited by difficulties in the analysis of sugars in urine at low concentrations. In this study we have developed an analytical procedure for quantitative assay of the lactulose-mannitol pair in urine by high resolution gas chromatography. The minimum detectable amounts are 7.5 pg for lactulose and 4.4 pg for mannitol. The calibration curves are linear in the range of 100-6400 mg L-1. Recoveries are within the range 86-102 % for mannitol and 84-105 % for lactulose.
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  • 200
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    Journal of High Resolution Chromatography 18 (1995), S. 699-704 
    ISSN: 0935-6304
    Keywords: Multidimensional GC ; Multidimensional GC-MS ; Thermal desorption cold trap injector ; Flavor ; Fragrance ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The Thermal desorption Cold Trap injector (TCT) was used as a part of modified multidimensional GC (MDGC) or MDGC mass spectroscopy (MS) systems. These systems were based on a preparative GC (GC1), an analytical GC (GC2), or GC-MS and the TCT. The TCT was mounted on the GC2 or GC-MS. Analysis was carried out as follows: first, the volatile compounds heart-cut after separation on the GC1 column were adsorbed onto the Porapak Q column out of the GC1 oven. This Porapak Q column was then coupled to the TCT, and the volatile compounds adsorbed on the Porapak Q were thermally desorbed, cold trapped, and injected onto an analytical column in the GC2 or GC-MS. Repeatability of the retention time (RT) and area % of model samples consisting of citronellol, decanol, and geranyl acetate was examined. Also, the volatile compounds present at very low concentrations in ethanol solution were concentrated on the Porapak Q column. These were injected onto the analytical column by the same method as described above, and the repeatability of the RT and area % on the chromatogram was examined. In the two experiments, the standard deviation of the RT and area % for each compound was about 0.02 and less than 2.85, respectively. A commercial geranium oil was successfully analyzed by this technique. The results indicate that this modified MDGC and MDGC-MS system are very useful for detection and determination of compounds in complex mixtures.
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