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71.
72.
Summary The coupling of carbon dioxide supercritical fluid chromatography with Fourier transform infrared spectrometry (SFC-FTIR)
is a powerful tool for the separation and on-line identification of non-volatile compounds. The IR transparency of carbon
dioxide in the Fermi resonance bands region versus its density has been studied. Functional groups with stretching vibrations
outside the transparent window of carbon dioxide are examined. SFC-FTIR separations allow Gram-Schmidt reconstruction chromatograms
or IR window chemigrams with high quality spectra to be obtained. This SFC-FTIR lightpipe (flow cell, beam condensing optics,
narrow band detector) has allowed detection limits of 250ng for benzonitrile and 70ng for methyl benzoate to be reached. The
feasibility of very rapid SFC-FTIR separations is shown along with the subsequent peak spectra. 相似文献
73.
基于Lagrange原理和假设模态法建立了旋转输液管的动力学模型.通过降阶升维的方法求解系统的特征值问题,并分析了旋转输液管自由振动特性.得到了不同端部集中质量和转速下,系统特征值随流速升高的演变轨迹.揭示了临界流速随系统参数的变化规律.研究发现,内部流体的流动对旋转输液管动力学特性存在显著影响.在某些参数组合下,系统低阶模态能够形成不同形式的内共振关系.预示了旋转输液管模型蕴含丰富的动力学现象. 相似文献
74.
We consider a fluid model including viscoelastic and viscoplastic effects. The state is given by the fluid velocity and an internal stress tensor that is transported along the flow with the Zaremba–Jaumann derivative. Moreover, the stress tensor obeys a nonlinear and nonsmooth dissipation law as well as stress diffusion. We prove the existence of global-in-time weak solutions satisfying an energy inequality under general Dirichlet conditions for the velocity field and Neumann conditions for the stress tensor. 相似文献
75.
Summary Polyethylene oxide (PEO)-based polymers with hydroxy, methoxy, and aminopropoxy terminal groups were coated on diol functionalized and hexamethyldisilazane end-capped silica particles. Proton-donor and proton-acceptor test solutes, including carboxylic acids, hydroxy-containing compounds, arylamines, and alkylamines were used to evaluate the chromatographic performances of these polymer coated particles under SFC conditions with neat CO2 as mobile phase. It was found that the particles coated with hydroxy-terminated PEO were suitable for the separation of proton-donor compounds such as hydroxy-containing compounds and carboxylic acids, and the particles coated with aminopropoxy-terminated PEO could be used for the separation of amines. That is, the proton-accepting stationary phase is suitable for the separation of proton accepting solutes, including strong basic alkylamines (pKb4), using neat CO2 as mobile phase, while the protondonating stationary phase is suitable for the separation of proton-donating compounds such as carboxylic acids (pKa4). Hydrogen bond basicity was found to be a critical factor for the chromatography of basic amines. Low volatility acidic and basic drugs were chromatographed using the new stationary phases. The stability of the PEO coated particles was determined by measuring the loss of organic carbon under SFC conditions. It was found that approximately 18 % of the coating (average molecular weight of 15,000) was washed out of the particles by supercritical CO2 after 7 h at 350 atm and 50°C 相似文献
76.
77.
Robert J. Houben Hans-Gerd M. Janssen Piet A. Leclercq Jacques A. Rijks Carel A. Cramers 《Journal of separation science》1990,13(10):669-673
A simple and versatile system is described for the on-line coupling of SFE to capillary GC. The interfacing consists of a programmed temperature vaporizer (PTV) injector. With this injector it is possible to combine solute trapping, elimination of a high flow of extraction fluid, and quantitative transfer of solutes to the seperation column. The problems caused by impurities in the extraction fluid in on-line SFE-GC are discussed. Simple methods are described for the purification of commercially available carbon dioxide. The trapping efficiency of the PTV injector is studied. Applications of the SFE-PTV-GC system are given for the analysis of polymer anti-degradants, polar compounds, and samples with environmental relevance. 相似文献
78.
T. Bücherl M. Eschler A. Gruner N. Palibroda E. Wolff 《Journal of separation science》1994,17(11):765-769
An integral restrictor interface with jet separator for coupling capillary column supercritical fluid extraction – supercritical fluid chromatography with high resolution mass spectrometry (SFE-SFC-MS) has been built and used for the analysis of a fatty acid ester, and of polymer additives with a wide range of masses. The mobile phase used was supercritical carbon dioxide; a flame ionization detector (FID) was used in parallel with the mass spectrometer. Different SFC-MS interface operating conditions, e.g. temperature, restrictor position, flow rate, and sample transfer conditions were optimized to obtain good sensitivity and separation for these applications. In addition, the sensitivity of measurements performed with the direct insertion probe and by SFC-MS interface have been compared. 相似文献
79.
Summary Methods for the determination of specific migration of polymer additives from polypropylene to aqueous acetic acid and isooctane have been studied. The migrants were extracted from aqueous acetic acid and characterized by supercritical fluid chromatography (SFC) with flame ionization detection (FID) and mass spectrometry (MS). The isooctane simulant was concentrated and injected directly into the SFC. Injection of extracts after incubation, using the solvent venting injection technique in the SFC, enabled additive concentrations as low as 10 ppb in 150 ml simulant to be determined, corresponding to a specific migration level of approximately 1 g additive/dm2 polymer. 相似文献
80.
在仅以碘化钾为重原子微扰剂、亚硫酸钠为除氧剂及无任何保护性介质存在的水溶液中 ,吲哚_3_丁酸 (IBA)能发射很强的室温光 (RTP) ;详细研究了分析测定条件及有机溶剂对RTP的影响 ;在最大光波长λex/λem =281/447nm处 ,光强度与IBA浓度在2.0×10 -7~1.0×10 -5mol/L范围内呈良好的线性关系 ,检出限4.3×10-8 mol/L ;方法直接用于强化水样和土壤中IBA的测定 ,回收率96 %~104 % ,相对标准偏差2.37 %~3.97 %。 相似文献