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11.
Five different analytical schemes for examining isothermal and nonisothermal degradation of polymers were reviewed and found inadequate for describing multistage decomposition. The different schemes were experimentally tested using thermogravimetric analysis data for an ethylene-vinyl acetate (EVA) copolymer, which exhibited a well-behaved two-step decomposition process in a nitrogen environment. Based on these experimental and analytical findings, a generalized methodology was developed capable of describing the exhibited complex decomposition behavior of polymers by combining two or more kinetic mechanisms in a series or parallel arrangement. This composite of combinational methodology thus extends established analytical schemes for describing complex decomposition of polymers in a rational manner, incorporating both experimental and theoretical considerations.  相似文献   
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Reactions of pyrrolidine with 2 equiv of aldehydes without any catalyst in a pressurized vessel at 140–200 °C yielded 1,3-disubstituted pyrroles. -Branched aldehydes gave fairly good yields of the corresponding products by this method, which provides a facile non-oxidative procedure for synthesizing 1,3-dialkylpyrroles from inexpensive pyrrolidine and aldehydes.  相似文献   
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The availability of both a tandem deuteron beam and a linac electron beam, the latter converted into Bremsstrahlung, at the new ALTO facility at IPN-Orsay offers a unique opportunity to compare the performance of a laser ion guide under different regimes. The ALTO accelerator has delivered its first electron beam at the end of 2005 and a design for a gas-cell prototype is being studied.  相似文献   
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Oxychelerythrine, benzo[c]phenanthridine alkaloid, was synthesized from easily available starting toluamide 5 and benzonitrile 6 using toluamide-benzonitrile cycloaddition reaction in 6 steps.  相似文献   
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A capillary electrophoretic method with UV detection at 278 nm has been developed for analysis of the immunosuppressant rapamycin (sirolimus) in human blood at low microgram per liter levels. Separation has been achieved in an acidic carrier electrolyte containing sodium dodecylsulfate and 30% (v/v) acetonitrile. For sample clean-up and preconcentration, an off-line solid-phase extraction step using a silica-based reversed-phase material and an on-capillary focussing technique were employed. The latter allows the injection of increased sample volumes without excessive band broadening. Although this new method is less sensitive than existing liquid chromatographic procedures combined with mass spectrometry, it is fully suited to routine analysis of rapamycin in blood from patients treated with this drug. Last but not least the low costs make it an attractive alternative to established methods.  相似文献   
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Five new natural labdane-type diterpenoids (5-9), designated leoheteronins A-E, together with four known diterpenoids (1-4), two phytosterols as a mixture of beta-sitosterol and stigmasterol, and the flavone genkwanin (10) were isolated from the aerial parts of Leonurus heterophyllus SW. (Lamiaceae) collected in northern Vietnam. Compound 1 was isolated for the first time from a Leonurus species, and 10 is considered to be a chemotaxonomic marker of the Leonurus genus. Their structures were determined using spectroscopic analyses.  相似文献   
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De Marco R  Phan C 《Talanta》2003,60(6):1215-1221
The direct flow injection potentiometric (FIP) analysis of phosphate in hydroponic nutrient solution has been carried out using a cobalt-wire ion-selective electrode (ISE). Synthetic hydroponic nutrient solution, commercial hydroponic nutrient solution and working hydroponic farm nutrient solution were analysed for phosphate using the FIP technique. It is shown that FIP results compare favourably to standard methods of analysis such as spectrophotometry and indirect photometric ion-pair chromatography. Reproducible FIP response curves with a slope of −(47.57±0.03) mV per decade and intercept of −(169.7±0.1) mV were obtained for four separate calibrations in the concentration range 5.0×10−4–1.0×10−2 M H2PO4. Anion corrections for interferences by Cl, NO3 and SO42− were applied to all samples using the selectivity coefficients determined independently using a fixed interference method. Nevertheless, it was found that anion corrections were not necessary, as the deviations fell within the bounds of experimental error for the cobalt-wire ISE technique (i.e.±2–5% R.S.D.). The proposed FIP method enables the direct determination of phosphate in hydroponic nutrient solutions.  相似文献   
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