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  • Chemistry  (25)
  • Magnetism
  • 1985-1989  (25)
  • 1970-1974
  • 1988  (25)
  • 1
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ionic Structures of 4- and 5-coordinated Silicon. Novel Ionic Crystal Structures of 4- and 5-coordinated Silicon: [Me3Si(NMI)]+ Cl-, [Me2HSi(NMI)2]+ Cl-, [Me2Si(NMI)3]2+ 2 Cl-. NMIMe3SiCl forms with N-Methylimidazole (NMI) a crystalline 1:1-compound which is stable at room temperature. The X-ray single crystal investigation proves the ionic structure [Me3Si(NMI)]+Cl- 1 which is the result of the cleavage of the Si—Cl bond and the addition of an NMI-ring. The reaction of Me2HSiCl with NMI (in the molar ratio of 1:2), under cleavage of the Si—Cl bond and co-ordination of two NMI rings, yields the compound [Me2HSi(NMI)2]+Cl- 2. The analogous reaction of Me2SiCl2 with NMI (molar ratio 2:1) leads to a compound which consists of Me2SiCl2 and NMI in the molar ratio of 1:2. During the sublimation single crystals of the compound [Me2Si(NMI)3]2+ 2 Cl-. NMI 3 are formed.
    Notes: Me3SiCl bildet mit N-Methylimidazol (NMI) eine bei Raumtemperatur beständige, kristalline 1:1 Verbindung. Nach der Röntgenstrukturanalyse entsteht unter Spaltung der Si—Cl-Bindung und Anlagerung eines NMI-Rings eine Verbindung ionischer Struktur [Me3Si(NMI)]+Cl- 1. Die Reaktion von Me2HSiCl mit NMI (Molverhältnis 1:2) führt unter Spaltung der Si—Cl-Bindung und Koordination von zwei NMI-Ringen zur Verbindung [Me2HSi(NMI)2]+Cl- 2. Bei der analogen Umsetzung von Me2SiCl2 mit NMI (Molverhältnis 2:1) entsteht eine Verbindung, die Me2SiCl2 und NMI im Molverhältnis 1:2 enthält. Bei der Sublimation werden Einkristalle der Verbindung [Me2Si(NMI)3]2+ 2 Cl-· NMI 3 erhalten.
    Additional Material: 3 Ill.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 11 (1988), S. 106-110 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Tandem capillaries ; Charcoal trapping ; Soil fumigants ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Soil fumigants, like 1,3-dichloropropene and metham-sodium (forming methyl isothiocyanate) diffuse into the atmosphere, thus presenting a hazard to people in the surroundings. A method is described in which a large volume (50 μl) of extractant, used to desorb the compounds from charcoal, is injected into a GC, equipped with two capillary columns. By way of Deans switching, the solvent is separated from the compounds of interest. Modification of a GC sampler makes unattended analyses possible.
    Additional Material: 2 Ill.
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  • 3
    ISSN: 0935-6304
    Keywords: Coupling LC/GC ; Retention gap ; Polychlorinated biphenyls ; Sediment ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Narrow-bore column liquid chromatography coupled on-line with capillary gas chromatography (LC/GC) is used for the determination of polychlorinated biphenyls (PCBs) in sediment via a heart-cutting technique. This method is compared with a method in which two off-line column clean-up steps are used with subsequent analysis by capillary gas chromatography. For the LC/GC analysis the recovery of PCBs was 90-100%. For two sediment samples from the river Meuse the LC/GC and the other, more laborious method showed good agreement.
    Additional Material: 5 Ill.
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  • 4
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Detectability ; Thick films ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: For a typical narrow bore (50 μm) and wide bore (320 μm) capillary column the effects of increased stationary phase film thickness (df) on the minimum detectable amount, Qo, as well as on the minimum analyte concentration, Co, are described. In treating the effect of an increased film thickness, two approaches can be followed; either the separation temperature is kept constant, resulting in larger values of the capacity ratio, k, or the column temperature is increased such as to keep k constant. For normalized chromatographic conditions the effects of both approaches on the minimum plate height, optimum carrier gas velocity, and required plate number are described, finally yielding expressions for Qo and Co for both mass flow and concentration sensitive detectors. At constant temperature, Co always increases with the film thickness for mass flow sensitive detectors (e.g. FID). Wide bore thin film columns offer the lowest value of Co attainable. For concentration sensitive detectors (e.g. TCD), Co is affected neither by column diameter nor by film thickness. The Qo-df plot for constant temperature shows a minimum, suggesting an optimum film thickness for mass flow sensitive as well as concentration sensitive detectors. The corresponding capacity ratio has a value between 0.5 and 1.5. At elevated temperatures (k constant) in combination with mass flow sensitive detectors, again an optimum film thickness exists, corresponding to a minimum value of Co. For constant capacity ratio Qo always increases with the film thickness for both types of detectors. As indicated above, in some situations the lowest values of Co and Qo are obtained at an increased film thickness, the effect being marginal. As an initial guideline, for the daily practice of capillary gas chromatography with respect to minimum values of Co and Qo, the use of thin film columns is to be preferred.
    Additional Material: 5 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 11 (1988), S. 462-470 
    ISSN: 0935-6304
    Keywords: Grob and splitless injection ; Injection techniques, capillary GC ; Splitless injection ; PTV splitless injection ; Matrix effexts ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Kurt Grob introduced splitless injection in 1969. He elaborated most of the working guidelines including the techniques required for reconcentrating the broad intial bands, i.e. the solvent effects and cold trapping. He also designed a vaporizing injector suited for splitless injection. Nevertheless, splitless injection is still often carried out using inappropriate conditions, and many of today's vaporizing injectors are not suited for splitless injection. No autosampler is available that introduces the sample at the appropriate position. Conventional splitless injection is compared to PTV splitless injection for the range of samples that cannot be handled by the anyway superior oncolumn injection, i.e. sample with high loads of involatile byproducts. There is a clear preference for PTV splitless injection as matrix effects observed in conventional splitless injection were found to be substantially reduced or even eliminated.
    Additional Material: 5 Ill.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 11 (1988), S. 862-869 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Column-detector systems ; Detectability ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Expressions for the minimum detectable amount Qo and the minimum analyte concentration Co as functions of the chromatographic parameters are derived for both mass and concentration sensitive detectors. The effects of pressure drop, column inner diameter, and film thickness are given.The minimum analyte concentration for mass flow sensitive detectors, Com, can be reduced considerably by selecting the carrier gas velocity well above its optimum value (related to Hmin), however, at the cost of long columns and long analysis times. For Qo the improvements can be neglected, and so the analysis can best be performed at uopt.When the flow rate in the detector, Fd, is equal to the column flow rate Fc, the maximum permissible detector volume of concentration sensitive detectors is proportional to dc2 up to dc3, and so narrow bore columns require detectors of extremely small volume. Make-up gas has to be added when the actual volume is too large, thus worsening the detectability. Another approach, vacuum operation of the detector cell, appears to be very attractive. On the other hand, when wide bore columns are used in combination with small volume concentration sensitive detectors, very small values of Qoc and Coc are obtainable when the abundant carrier gas can be removed before entering the detector cell.Digital noise filtering can further reduce the obtainable Qo and Co values, especially for broad peaks and thus for wide bore columns.
    Additional Material: 8 Ill.
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  • 7
    ISSN: 0935-6304
    Keywords: Capillary GC ; Coupled LC-GC ; Large injection volumes ; Trace analysis ; Aqueous samples ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This paper describes the design of a new, versatile, and low-cost on-line LC-GC interface that allows the fast and reliable introduction of large sample volumes onto a capillary GC column. The sample introduction procedure consists successively of: evaporation of the entire sample (LC fraction), selective removal of the solvent and simultaneously cold-trapping of the solutes, splitless transfer of the solutes to the GC column, on-column focusing, GC separation and detection. Quantitative and qualitative aspects of various experimental parameters are evaluated and optimum conditions are reported. The applicability of the method is demonstrated on a synthetic aqueous sample of chlorinated pesticides.
    Additional Material: 15 Ill.
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  • 8
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Journal für Praktische Chemie/Chemiker-Zeitung 330 (1988), S. 305-308 
    ISSN: 0021-8383
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: HPLC Studies on the Distribution Behaviour of Selected I-Amino-3-aryl-guanidinium Nitrates
    Additional Material: 1 Ill.
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  • 9
    ISSN: 0021-8383
    Keywords: Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Substituted aromatic isothiocyanates with malonyl chloride yield 7-chloro-3-substituted-3,4-dihydro-4,5-dioxo-2-thio-2H,5H-pyrano [3,4-e]-1,3-oxazine (1).Alkyl isothiocyanates with malonyl chloride yield a mixture of 7-chloro-3-alkyl-2-thio pyranooxazine (2) and the 2-oxo-analogue (3).The pyrano oxazine 1 react stepwise with morpholine undergoing replacement of the 7-chloro substituent yielding the 7-morpholino analogue (4), then the pyrone ring was opened producing 5-morpholino carbonyl-4-oxo-3-substituted phenyl-2-thio-1,3-oxazine-6-ylacetomorpholid (5). Finally the oxazine ring was opened yielding 2-substituted phenyl carbomyl-3-morpholino-N,N-glutaconoyldimorpholine (6).Ethanol react with compound 1 at any molar ration causing the opening of the pyrone ring and retain the oxazine ring.Mass spectra. 1H-n.m.r., u.v. and i.r. spectroscopic data provided information about the fine structures of the products.
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  • 10
    Electronic Resource
    Electronic Resource
    Hoboken, NJ : Wiley-Blackwell
    Journal of Biomedical Materials Research 22 (1988), S. 423-439 
    ISSN: 0021-9304
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine , Technology
    Notes: The biocompatibility of two silicone rubbers, Silastic and Dow Corning Elastomer, and of a polyether and a polyester urethane, a polyether polyester copolymer, and polypropylene oxide was assessed in vitro. These elastomers were selected for assessment as a possible alloplastic tympanic membrane. For these studies use was made of rat middle ear mucosa explants and serially cultured epithelium. The quantitative results were based on epithelial growth curves, the morphological picture was based on the findings in epithelium, and the aging of a biomaterial was simulated. Epithelium morphology was investigated by scanning and transmission electron microscopy and x-ray microanalysis. Quantitative results showed that on Dow Corning Elastomer and polypropylene oxide, cell proliferation was significantly lower compared to normal growth curves. The morphological findings were negative for polypropylene oxide, and did not discriminate between the other biomaterials under study. The simulation results indicated better biocompatibility for the polyurethanes and the polyether polyester copolymer compared with that of polypropylene oxide and both silicone rubbers. Under the simulation conditions, cells exposed to Silastic showed siliconcontaining inclusions. These in vitro results suggest that the biocompatibility of the polyurethanes and the polyether polyester copolymer is better than that of both silicone rubbers and polypropylene oxide.
    Additional Material: 9 Ill.
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