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  • 1
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 10 (1997), S. 825-834 
    ISSN: 0894-3230
    Schlagwort(e): N-tert-butoxycarbonyl-L-phenlylalanine-pyridine complex ; isotope effect ; x-ray structure ; vibrational spectroscopy ; Chemistry ; Theoretical, Physical and Computational Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: The x-ray structure of the complex between N-tert-butoxycarbonyl-L-phenylalanine and pyridine shows that the crystals are held together by short hydrogen bonds between the OH group and the N atom of the pyridine ring [RO(H)· · ·N=2·574(3) Å]. Deuteration of the OH and NH groups results in a small expansion of the unit cell associated with an elongation of the O· · ·N distance [RO(D)· · ·N=2·610(3) Å]. The infrared spectra show very broad stretching protonic bands in the range 2750-600 cm-1. The isotopic ratio ν(OH· · ·H)/ν(OD· · ·N) of nearly unity suggests a double minimum potential with a low barrier for the hydrogen bridge. The Raman and near-infrared spectra are discussed. The perturbation of the fundamental modes and of the overtones of pyridine suggests that the complex is not of the proton transfer type. The broad absorptions of the hydrogen bridge disappear in the near-infrared region. The perturbation of the pyridine overtones is discussed. © 1997 John Wiley & Sons, Ltd.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 2
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Journal of Physical Organic Chemistry 10 (1997), S. 680-686 
    ISSN: 0894-3230
    Schlagwort(e): 8-aminoquinoline ; x-ray structure ; vibrational spectra ; three-center hydrogen bond ; Chemistry ; Theoretical, Physical and Computational Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: -The x-ray structure of 8-aminoquinoline indicates that one of the NH bonds of the NH2 group forms a three-center hydrogen bond, the major component being the intramolecular hydrogen bond and the minor component the intermolecular hydrogen bond. The IR and Raman spectra of 8-aminoquinoline and of its N-deuterated counterpart reflect the non-equivalence of the two NH(D) bonds and the weakness of the hydrogen bridge. © 1997 John Wiley & Sons, Ltd.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 3
    Digitale Medien
    Digitale Medien
    Hoboken, NJ : Wiley-Blackwell
    AIChE Journal 43 (1997), S. 577-587 
    ISSN: 0001-1541
    Schlagwort(e): Chemistry ; Chemical Engineering
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Werkstoffwissenschaften, Fertigungsverfahren, Fertigung
    Notizen: Complex mixing flows and mixing parameters are calculated to evaluate mixing quality on the basis of kinematic parameters together with a statistical analysis. The results allow for a comparative evaluation in terms of geometry and flow parameters. The evaluation is limited to two-dimensional flows with moving boundaries in periodic motion such as the flow in the cross section of a twin-cam mixer. The finite-element calculation requires a remeshing procedure for every time step with special techniques to upgrade mixing variables from one time step to the next. The relative mixing quality of single cam and co: or counterrotating cam devices are compared by evaluating segregation scale, length stretch, and efficiency. The numerical results exhibit a good correspondence with their experimental counterpart.
    Zusätzliches Material: 15 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 4
    Digitale Medien
    Digitale Medien
    Hoboken, NJ : Wiley-Blackwell
    AIChE Journal 43 (1997), S. 588-597 
    ISSN: 0001-1541
    Schlagwort(e): Chemistry ; Chemical Engineering
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Werkstoffwissenschaften, Fertigungsverfahren, Fertigung
    Notizen: Numerical tools for the analysis of complex 3-D mixing devices were developed. Calculations are based on the finite-element method. The flow calculation is combined with that of pathlines for a fairly large number of material points; along these pathlines, relevant kinematic variables, which are then subjected to a statistical treatment, are evaluated. These numerical techniques are applied to the analysis of a Kenics mixer. It is assumed that the geometry is periodic in the axial direction, that is, that the mixer contains an infinite number of blades; the finite-element analysis may then be completed on a single wavelength of the geometry. To test the accuracy of the three-dimensional calculation, a Kenics device was mounted in order to mix clays of different colors, and photographs of experimental cross-sections were compared with numerical results showing concentration maps. A statistical treatment was performed on some 8,000 material points crossing the entry section to evaluate mixing quality.
    Zusätzliches Material: 16 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 5
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 20 (1997), S. 222-226 
    ISSN: 0935-6304
    Schlagwort(e): LC-GC ; Partially concurrent solvent evaporation ; Organochlorines ; PCBs ; Fatty matrices ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Off-line normal-phase LC has been used for the clean-up of compounds in our laboratory for several years. On-line coupling of this LC system, which typically yields 12 ml fractions, is not possible due to its large fraction volume. The maximum transfer volume in on-line LC-GC/ECD is approx. 300 μl. Therefore down-scaling of the LC system was attempted in order to reach these low fraction volumes. Miniaturization resulted in a 240 μ1 LC fraction containing the analytes of interest, which is transferred to GC/ECD via an on-column interface. Sensitivity requires that a minimum amount equivalent to 1-2 mg of sample should reach the GC detector; the selectivity is determined by the separation between the matrix and the last eluting target analyte.For the analysis of fatty samples, limitations were observed in the separation of dieldrin from triglycerides. Other organochlorine compounds, e.g. polychlorobiphenyls (PCBs), the DDT group, HCB and the HCHs can be analyzed with RSDs of 2-4 % (n = 10) at concentration levels of sub-μ/kg in milk fat using a 3 μm Hypersil silica 50 × 1.0 mm i.d. LC column.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 6
    ISSN: 0935-6304
    Schlagwort(e): Capillary GC ; Continuous liquid-liquid extraction ; Environmental applications ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The applicability of a liquid-liquid extraction system which is coupled on-line with a capillary gas chromatograph was studied for environmental and ecotoxicological analyses. The optimized and automated system was used for the determination of apolar and rather non-volatile organic compounds in aqueous samples. Relevant aspects of sample introduction, phase separation and selection of extraction solvent are discussed. Three routine-tipe applications are described, viz. an improved method for the determination of hexachlorocyclohexanes in ground water and the determination of the so-called NCC-ether and ACC-ether in ecotoxicological studies. Depending on the application studied, the concentration levels varied from 0.1 to 6000 μg/I, using ECD and/or FID detection. Typical coefficients of variation obtained with the total extraction-GC procedure were 2-25%.The system was found to be rugged, it saves time compared with set-ups involving off-line liquid-liquid extraction and considerably reduces the manual work load.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 7
    Digitale Medien
    Digitale Medien
    Weinheim [u.a.] : Wiley-Blackwell
    Materials and Corrosion/Werkstoffe und Korrosion 48 (1997), S. 243-251 
    ISSN: 0947-5117
    Schlagwort(e): Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Maschinenbau
    Beschreibung / Inhaltsverzeichnis: Corrosion of parts used for microelectronics applicationsManifestations of corrosion on parts used in microelectronics occur for different reasons and are frequently described in literature. They are not only caused by operational circumstances but are also favoured by the production process. Investigations have been carried out to ascertain the cause of the failure of several circuit boards used in the operation electronics of the preparation unit for kitchen waste water. During microscopic and electronmicroscopic observations of failed circuit boards, different corrosion types have been found, mainly on the surface of a commonly used Sn-Pb-alloy. Hence, potentiostatic and free-corrosion experiments under laboratory conditions have been performed using the employed Sn-Pb-alloy. In order to simulate the increased concentration of harmful substances at the surface of the boards, the medium used contained a high percentage of the substances found in the surroundings of the unit. From the measured values of current density for different potentials and the observed corrosion on the sample's surface, conclusions as to the reported failure of the electrical operation system have been made. During the experiments under laboratory conditions, manifestations of corrosion similar to those found on the surface of the failed circuit boards have been observed. Based on these results, it seems likely that pitting and selective corrosion of the Sn-Pb-alloy led to the failure of the investigated circuit boards and, therefore, of the operation electronics.
    Notizen: Korrosionserscheinungen an Bauteilen der Mikroelektronik treten aus unterschiedlichen Gründen auf und sind in der Literatur beschrieben. Sie werden nicht nur durch die Betriebsumstände hervorgerufen, sondern werden nicht selten auch durch die Fertigung begünstigt. Untersuchungen zum Ausfall mehrerer Platten, die in der Steuerungselektronik einer Fettaufbereitungsanlage für Großküchenabwässer zum Einsatz gekommen sind, wurden durchgeführt. Bei der licht- und elektronenmikroskopischen Betrachtung der ausgefallenen Platine wurden verschiedene Korrosionserscheinungen gefunden, die hauptsächlich an dem eingesetzten Lötwerkstoff auftraten. Aus diesem Grund sind an der als Lötstoff eingesetzten Zinn-Blei-Legierung unter Laborbedingungen potentiostatische Halteversuche und Versuche hei freier Korrosion mit Medien durchgeführt warden, welche die Schadstoffe der Umgebungsluft der Anlage in erhöhten Mengen beinhalten, um damit ein Aufkonzentrieren an den Oberflächen der Platine zu simulieren. Anhand der ermittelten Stromdichte-Werte für verschiedene Potentiale und der Korrosionserscheinungen an den Proben werden Rückschlüsse auf den vorliegenden Schadensfall gezogen. Bei den unter Laborbedingungen durchgeführten Versuchen werden ähnliche Korrosionserscheinungen beobachtet, wie sie an den Bauelementen der ausgefallenen Platinen gefunden wurden. Es wird aufgrund der vorliegenden Ergebnisse Vermutet daß Lochfraß und selektive Korrosion der Sn-Pb-Legierung ursächlich für den Ausfall der untersuchten Platinen der Steuerungselektronik ist.
    Zusätzliches Material: 16 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 8
    Digitale Medien
    Digitale Medien
    Weinheim [u.a.] : Wiley-Blackwell
    Materials and Corrosion/Werkstoffe und Korrosion 48 (1997), S. 207-215 
    ISSN: 0947-5117
    Schlagwort(e): Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Maschinenbau
    Beschreibung / Inhaltsverzeichnis: Investigation on stress corrosion cracking of austenitic steels in cold chloride solutionsAt ambient temperatures of about 25°C austenitic chromium nickel steels can suffer stress corrosion in media with a concentration of both hydrogen ions and chloride ions exceeding 1 mol/L or in strongly concentrated chloride solutions. With the aid of constant strain rate testing and with U-bend specimens the parameters of this types of corrosion were investigated. Contrary to the situation with the acid solutions, the reproducibility of test results with the concentrated chloride solution was found to be low. The formation of martensite by cold working was found to be essential. The corrosion susceptibility decreases with increasing nickel content.Stress corrosion takes place within small critical potential ranges without a limit to more positive potentials as this is the case of stress corrosion with hot media. These potential ranges are widened with increasing cold working especially in the case of strongly grinding or cyclic loading in the plastic range.Corrosion cracking was observed with solutions of MgCl2, LiCl, with a less amount with NaCl, but not with ZnCl2. The concentration of chloride ions have an effect for solutions with a given kind of salt, but not for different salt solutions.
    Notizen: Bei austenitischen Chrom-Nickel-Stählen kann transkristalline Spannungsrißkorrosion bei 25°C auftreten, wenn sowohl die Wasserstoffionen- als auch die Chloridionen-Konzentration etwa 1 mol/L überschreiten oder wenn stark konzentrierte Chloridlösungen vorliegen. Die Parameter dieser Korrosion wurden mit CERT-Versuchen und mit Bügelproben untersucht. Im Gegensatz zu den sauren Lösungen ist die Reproduzierbarkeit bei den konzentrierten Lösungen gering, wobei im wesentlichen die Bildung von Verformungsmartensit die Korrosionsanfälligkeit bestimmt, die mit ansteigendem Nickelgehalt abnimmt.Die Spannungsrißkorrosion findet in begrenzten Potentialbereichen statt und ist im Gegensatz zu der Spannungsrißkorrosion in warmer Medien zu positiveren Potentialen hin begrenzt. Die Potentialbereiche können mit zunehmender Kaltverformung ausgeweitet werden, wobei eine grobe Schleifbehandlung und zyklische Belastungen im plastischen Bereich die Rißbildung begünstigen.Rißbildung wurde in Lösungen mit MgCl2, LiCl und im geringen Ausmaß auch mit NaCl, nicht aber mit ZnCl2 beobachtet, wobei die Konzentration der Chlorid-Ionen nur innerhalb einer Salzart, nicht aber bei den verschiedenen Lösungen einen erkennbaren Einfluß hat.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 9
    ISSN: 0941-1216
    Schlagwort(e): Chemistry ; Organic Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 10
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 20 (1997), S. 363-368 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Solid-phase extraction ; Automation ; Water samples ; Acetylation ; Chlorophenols ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: An automated system for derivaatization was coupled on-line with solid-phase extraction-gas-chromatography (SPE-GC). The system was optimized for the determination of phenol and chlorinated phenols in aqueous samples. The test analytes were acetylated with acetic anhydride; proper buffering of the sample was a critical factor. Next, the phenol acetates were enriched on a SPE cartridge and transferred to a GC; two appraoaches were studied. In the first approach, the derivatives were enriched on disposable C18 cartridges (ASPEC type) and desorbed with methylacetate. Aan aliquot of the final eluate was injected on-line the GC by means of a loop-type interface. In the second approach, trace enrichment was performed on 10 × 2 mm i.d. LC-type precolumn packed with polystyrenedivinylbenzene copolymer (PLRP-S) this precolumn was dried with a mitrogen purge and the phenol acetates were desorbed with ethyl acetate which was injectedon-line into the retention gap of the GC under partially concurrent solvent evaporation (PCSE) conditions. The Derivatization-SPE-GC system which was based on the loop-type interface has the advantage of simplicity and easy operation, the main drawback is the impossibility to determine phenol acetates which elute prior to trichlorophenol acetates. With the derivatization-SPE-GC approach using PCSE-based desorption, even the most volatile analyte of the test series, phenol acetate, can be determined successfully. The entire procedure, including the derivatization step, was fully automated and integrated in one set-up. The precision data for the integrated on-line derivatization-SP-FID system were fully satisfactory, with RSD values of 1-12 % at the 1 μg/1 level. When a sample volume of 2.2 ml was analyzed, The detection limits for the chlorinated phenol acetates were in the 0.1-0.3 μg/1 range.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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