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  • 1
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ephedrine and methamphetamine standards were separately derivatized with heptafluorobutyric anhydride (HFBA) and carbethoxyhexafluorobutyryl chloride (CB) and analyzed by full-scan gas chromatography/ion trap mass spectrometry with electron ionization (EI) and chemical ionization (CI). Using EI, a high-concentration ephedrine standard produced a total ion gas chromatogram containing several minor HFB derivatives in addition to ephedrine. One of these had the same retention time as the derivative of methamphetamine, while another eluted 3 s later. Both contained the same major mass fragmentation ions that could be erroneously used in targeted selected ion monitoring gas chromatographic/mass spectrometric analysis for methamphetamine. The full-scan EI and CI spectra showed that these derivatives were not methamphetamine. CI mass spectrometric studies of ephedrine scanning up to m/z 700 demonstrated that reaction with HFBA caused acylation of both the hydroxyl and secondary amino groups. The HFBA used in this study was contaminated with pentafluoropropionic anhydride and tri-fluoroacetic anhydride and produced mixtures of derivatives, some with retention times near or identical to that of methamphetamine. In contrast, CB derivatization of ephedrine produces a single methamphetamine-like compound that has the same retention time and mass spectra as methamphetamine, and is produced only when high gas chromatograph injector temperatures are used ( 〉 260°C). Collision-induced decomposition tandem mass spectrometric studies for the CB derivative verified that methamphetamine is produced from ephedrine at elevated GC injection port temperatures. In view of these findings, substance abuse testing for methamphetamine in urine must proceed with caution when ephedrine and other sympathomimetic amines are present. Definitive analyses can be accomplished by full-scan CI gas chromatographic/mass spectrometric analysis with HFB derivatives, or by lowering gas chromatograph injector temperatures with CB derivatives.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Oral (44Ca: 0.13-0.20 mmol) and intravenous (42Ca: 0.02-0.037 mmol) isotopically enriched stable calcium (Ca) tracers were given together with an oral dose of 2.5 mmol of natural Ca to normal subjects. Blood and urine samples were collected up to 24 h after the tracer doses and atom fractions (AFs) of these tracers (relative to natural Ca) were measured by high-precision thermal ionization mass spectrometry (TIMS). The time(dependent fractional rate of oral dose absorbed and true fractional intestinal Ca absorption (α) were derived from the AFs by mathematical deconvolution. After 6 h, the ratio AF oral tracer/AF intravenous tracer in blood equalled that in urine and did not change thereafter. Reproducibility of the combination of chemical precipitation of Ca (from a urine standard) and subsequent TIMS measurements, in nine runs over 13 months, was 1.2% (coefficient of variation). This was in accord with the within-run reproducibility. An estimate of α derived from a single blood or urine measurement was 6-10% higher than the reference value obtained by deconvolution. This discrepancy could be explained by a correction factor depending, in part, on the elapsed time for peak Ca intestinal absorption rate. Instrumentally induced mass fractionation, as well as contributions from radiogenic Ca, had a significant effect on the accuracy and reproducibility of the ratio of AFs of tracers in blood and urine.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Stamford, Conn. [u.a.] : Wiley-Blackwell
    Polymer Engineering and Science 27 (1987), S. 653-662 
    ISSN: 0032-3888
    Keywords: Chemistry ; Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: The morphology of blends of polycarbonate and nylon 6,6 with a copolyester of 60 mole percent p-hydroxybenzoic acid/40 mole percent poly(ethylene terephthalate) was characterized under different processing conditions. In particular, single-screw extrusion, steady simple shear flow, and flow through a capillary were studied to determine what conditions were necessary for the development of a fibrillar morphology of the liquid crystalline polymer (LCP). Results indicate that some extensional flow is required for the coalescence and extension of the particulate LCP phase. The viscosity of the blends was determined both in a cone-and-plate geometry of a Rheometrics Mechanical Spectrometer at low shear rates and in the Instron Capillary Rheometer at higher rates. In general, only a small (10 or 30 percent) weight fraction of LCP was required to reduce the viscosity of the thermoplastics to that of the polymeric liquid crystal. An attempt was made to correlate the structure of the blends seen under the scanning electron microscope with the observed rheology. Not all aspects of the morphology were possible to explain in terms of the viscous properties of the blends.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Applied Polymer Science 28 (1983), S. 3301-3307 
    ISSN: 0021-8995
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Applied Polymer Science 33 (1987), S. 2669-2687 
    ISSN: 0021-8995
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Transport of liquid cyclohexane through well characterized, initially glassy, crosslinked polystyrene slabs was investigated. The samples were produced by bulk polymerization of styrene and divinyl benzene using benzoyl peroxide as an initiator at 90°C for 48 h; they had initial crosslinking ratios, X, between 0.005 and 0.025 mol DVB/mol styrene, initial thickness of 0.25 mm to 1.80 mm, and the aspect ratio was maintained above 10 to achieve one-dimensional transport. The results of cyclohexane uptake as a function of time were used to elucidate the effects of degree of crosslinking and sample geometry on the mechanisms of penetrant transport. These results were interpreted in terms of relaxational and diffusional mechanisms.
    Additional Material: 12 Ill.
    Type of Medium: Electronic Resource
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  • 6
    Electronic Resource
    Electronic Resource
    Stamford, Conn. [u.a.] : Wiley-Blackwell
    Polymer Engineering and Science 28 (1988), S. 96-103 
    ISSN: 0032-3888
    Keywords: Chemistry ; Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Transport of liquid cyclohexane through well characterised, initially glassy, crosslinked polystyrene slabs was Investigated at 20, 30, 40, and 50°C. The samples used were produced by bulk polymerization of styrene and divinyl benzene (DVB) at 90°C for 43 hr using benzoyl peroxide as an initiator. The samples tested had initial cross-linking ratios, X, between 5 and 25 × 10-3 mol DVB/mol styrene. The initial thickness of the samples tested varied from 0.25 mm to 1.80 mm, and the aspect ratio (length to thickness ratio) was maintained above 10;1 in order to analyze the results by one-dimensional transport equations. Cyclohexane uptake was followed as a function of time along with dimensional changes in the thickness and area of the samples. The results of penetrant uptake as a function of time were analyzed using a simplified exponential expression and employing all the data points from the beginning of the experiment until the time of observation of the maximum in uptake. Good correlations were established between the penetrant uptake and the transport temperature. These results were interpreted in terms of competitive relaxational and diffusional mechanisms.
    Additional Material: 14 Ill.
    Type of Medium: Electronic Resource
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  • 7
    Electronic Resource
    Electronic Resource
    Stamford, Conn. [u.a.] : Wiley-Blackwell
    Polymer Engineering and Science 30 (1990), S. 1442-1453 
    ISSN: 0032-3888
    Keywords: Chemistry ; Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Three different polymer blends consisting of an isotropic matrix and a ther-motropic liquid crystalline polymer (LCP) as the reinforcement were extruded. Polycarbonate (PC) and polyetherimide (PEI) were the two matrices, and the LCPs used were Vectraw A950 of Hoechst-Celanese, a copolyester of hydroxybenzoic and 2,6 hydroxynaphthoic acids and an LCP of Granmont Inc., a condensation polymer of terephthalic acid, (l-phenylethyl)hydroquinone, and phenylhydroqui-none. These extrudates were characterized by a quantitative morphological technique to determine the percentage of LCP present as fibrils and the average domain diameter. These experimental observations were then coupled with the component Theological behavior and a simple heat transfer analysis to explain the morphology and property differences between the blends. Blends with the Granmont LCP showed no appreciable increase In the quantity of fibrils with draw ratio, for example, whereas the amount of fibrils in Vectra® blends tended to increase to a plateau with draw. The tensile modulus of the blends agreed well with composite theory, with average fibril moduli of 24.6 GPa and 23,3 GPa for Vectra® and the Granmont LCP, respectively. These differences can be explained in terms of the cooling behavior of the LCPs.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
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