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Eingeladener Vortrag
- nein (39)
The performance of a miniaturized channel for the separation of polymer and metal nanoparticles (NP) using Asymmetrical Flow Field-Flow Fractionation (AF4) was investigated and compared with a conventional AF4 system. To develop standard separation methods, experimental parameters like cross flow, gradient profile and injection time were varied and optimized.
Corresponding chromatographic parameters were calculated and compared. Our results indicate that the chromatographic resolution in the miniaturized channel is lower, whereas significantly shorter analyses time and less solvent consumption were obtained. Moreover, the limit of detection (LOD) and limit of quantification (LOQ) obtained from hyphenation with a UV-detector are obviously lower than in a conventional channel, which makes the miniaturized channel interesting for trace analysis.
Poly(l-lactide)s are synthesized and annealed at 120 °C and changes of the molecular weight distribution (MWD) are monitored by matrix-assited laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry. For example, benzyl alcohol+SnOct2 causes equilibration of odd- and even-numbered chains and the final goal of the transesterification is the most probable distribution. The underlying intermolecular transesterification is even observed at 100 and 80 °C in the solid state. However, cyclic tin mercaptide catalysts transform the initial most probable distribution into a MWD with maxima, which display a conspicuous fine structure due to a preferential crystallization of certain ring sizes. The optimum ring sizes for the crystallization are provided by ring-ring equilibration. The gradual formation of a special morphology shifts the melting temperature to values up to 187 °C. Annealing of commercial poly(l-lactide) with a cyclic tin catalyst also yields a distribution of mass peaks with a maximum showing the characteristic fine structure.