Phase Equilibria and Critical Curves of Binary Ammonia–Hydrocarbon Mixtures

Liquid or dense supercritical ammonia has been suggested as an extraction fluid. It is indeed good solvent for very different classes of compounds, as can be seen from phase diagrams. Such diagrams for binary systems of ammonia and hydrocarbons are presented and discussed on the basis of their critical curves. Apparatus and methods for the measurement of phase equilibria and equation of state data of fluid mixtures at high pressure are described.     

Synthesis and characterisation of advanced UHMWPE/silver nanocomposites for biomedical applications

A supercritical fluid (SCF) route for facile and homogeneous introduction of silver nanoparticles into polymer hosts is described. Our focus is on ultra-high molecular weight polyethylene (UHMWPE). We demonstrate that the metallic nanoparticles have a substantial effect upon the wear and tribochemical properties of the polymer substrate.     

乙醇对超临界CO2中乙酰乙酸乙酯异构化平衡的影响

超临界流体（SCF）是物质所处的温度和压力同时高于其临界值时的流体．在超临界体系中存在特殊的分子间相互作用，从而使其具有诸如高压缩性、高扩散系数、强溶剂化力等许多独特的性质.在超临界流体研究领域引起人们普遍关注的问题之一是共溶剂效应（cosolventeffect），即在超     

Carbon dioxide supercritical fluid chromatography-Fourier transform infrared spectrometry

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.     

Supercritical carbon dioxide extraction of Mentha pulegium L. essential oil

The dependence of Mentha pulegium L. (pennyroyal) essential oil composition, obtained by supercritical carbon dioxide (SC-CO₂), with the following parameters: pressure, temperature, extraction time (dynamic), and modifier (methanol) was studied. The results were also compared with those obtained by conventional hydrodistillation method in laboratory conditions. Regarding the percentages of menthone (30.3%) and pulegone (52.0%), the optimum SFE results were obtained at the following experimental conditions: pressure=100 atm, T=35 °C, dynamic time=10 min, and V_modifier=0 μl. The results of hydrodistillation showed that the major components of M. pulegium L. were pulegone (37.8%), menthone (20.3%), and piperitenone (6.8%). The evaluation of the composition of each extract was performed by gas chromatography-mass spectrometry.     

End-functionalized polyethylene oxide coated silica particles for packed capillary column supercritical fluid chromatography

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 (pK_b4), using neat CO₂ as mobile phase, while the protondonating stationary phase is suitable for the separation of proton-donating compounds such as carboxylic acids (pK_a4). 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     

Efficiency of composite vs. conically shaped chromatographic columns

The theory of composite chromatographic columns has been re-examined and general equations relating their efficiency to those of individual columns were derived. The derivations were based on elementary principles without reference to the principle of variance additivity. Derived also, were general equations for the efficiency of columns with continuously varying diameters, HETP and other properties from which formulae for special cases of practical interest were deduced. An example comparing the efficiencies of two columns, one conical and the other composite was given. The calculations show clearly that the conical column is superior in efficiency for the same total length and total retention volume.     

离子交换法纯化重组类人胶原蛋白II的研究

用阳离子交换树脂CM-52分离纯化类人胶原蛋白II(HumanCollagen-likeBioproteinII,HCBII)。通过实验,分别确定了静态吸附和柱层析吸附的操作条件,即静态吸附:在pH4.0、NaCl0.15mol/L、进料浓度7g/L,处理量17.26ml/g树脂的条件下进行吸附,吸附时间为60min;柱层析:在pH4.0、NaCl0.15mol/L、进料浓度5g/L、流速5ml/min的条件下进行吸附。然后上柱,在pH4.0、NaCl0.30mol/L下进行脱附。实验表明,采用静态吸附的方式吸附HCBII,然后上柱洗脱,HCBII的吸附量可达到48.6mg/g树脂,回收率83.8%,操作时间短,分辨率高,最终纯化的HCBII达电泳纯,分子量为97kD。     

离线超临界流体萃取和气相色谱/质谱联用对实验室内空气中气相有机污染物的测试

通过团体吸附剂富集，再用超临界ＣＯ２脱附后用气相色谱及质谱技术对实验室内空气中气相有机污染物进行了考察。文中对采样和萃取条件进行了优化，并与热脱附所得结果做了比较。结果表明在２２ＭＰａ，８０℃时，用甲醇改性的超临界ＣＯ２进行萃取的结果优于热脱附法。该法鉴定出气相有机污染物中５２个组分，占色谱峰总面积的９９．６％。     

Supercritical fluid extraction-capillary gas chromatography: On-line coupling with a programmed temperature vaporizer

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.