超临界流体色谱流程设计及其应用

本文设计了多功能超临界流体色谱流程,流程中包括毛细管/微填充柱SFC,GC,计算机控制温度、压力、密度及信号采集、处理,配置有超临界流体萃取池,解决了超临界流体色谱分流口易堵问题。利用该流程,将石腊、DC-200气相色谱固定相、黄油、蜂蜡、救心油、红花油等样品进行超临界流体色谱分离。     

Early Evolution of Gas Chromatography in East Germany. Part I: Beginnings, Instrument and Column Development and Organizations

The early evolution of gas chromatography in the former German Democratic Republic (GDR) is surveyed and instrument development is outlined, describing the most important models manufactured in the GDR. The organization of the Arbeitsgemeinschaft für Gas-Chromatographie (Working Group for GC) is chronicled and its activities are discussed. Subsequent parts of this article will deal with the six symposia organized by the Arbeitsgemeinschaft between 1958 and 1968.     

Nanostructure evolution studies of bulk polymer materials with synchrotron radiation: progress in method development

The prospects of a modern analysis of nanostructure evolution during the processing of polymer materials by means of scattering from synchrotron radiation are demonstrated in examples. The beam sources have gained stability, shortages are located in beamline setups and in method development for the quantitative analysis of voluminous data sets.By using the proposed multidimensional chord distribution function (CDF) analysis method, nanostructure information from small-angle X-ray scattering (SAXS) data are extracted and visualised. The method can be automated if the beamline setup is able to deliver a full data set with simple constraints. In this case even a simultaneous data evaluation is possible (while one pattern is accumulated, the previous one is analysed). The advantages of the method are demonstrated in a study of the straining of a thermoplastic elastomer. The possibilities of an automated analysis are demonstrated in an investigation of the crystallisation behaviour of high-pressure injection-moulded polyethylene (HPIM-PE). The achievable results of nanostructure analysis of polymer materials are discussed. It is shown that the time-resolved SAXS of polymer materials studied during a transformation and analysed by the CDF method is not just a powerful tool to investigate the relationship between structure and properties of materials; the information that can be gained concerning the processes that control nanostructure evolution is equally important. In the future the enlightenment of such relationships may help to tailor polymer materials with respect to their properties and, beyond that, to improve assessments concerning their aging.     

The effect of interface deformation due to gravity on line tension measurement by the capillary rise in a conical tube

Much research has been done on line tension measurement and interpretation, and attempts have also been made to measure line tension with simple, cheap and reliable methods that do not require excessive sophistication. Of particular interest is the method of determining line tensions of solid–liquid–vapor systems from the capillary rise in a conical tube. This simple and relatively inexpensive method gives line tension values comparable to those reported in the literature obtained via highly sophisticated instruments or techniques such as the well known axisymmetric drop shape analysis technique. The absolute value of line tension obtained using the conical tube method and assuming a spherical liquid–vapor interface is larger but of the same order of magnitude (1 μJ m⁻¹) as that reported in the literature. A theoretical analysis presented herein shows that by including the deformation of the liquid–vapor interface due to gravity in the conical capillary analysis, the line tension value inferred from the experimental data is reduced by approximately 50% and compares better with values in the literature obtained using other sophisticated methods. Thus a relatively simple, cheap, accurate and reliable method of line tension measurement has been advanced.     

Estimation of the instrumental band broadening contribution to the column elution profiles in open tubular capillary liquid chromatography

In comparison with conventionally packed HPLC columns, from a theoretical point of view, open capillary liquid chromatography (OTLC) systems offer a number of advantages like high plate numbers and short analysis times. On the other hand, drastic changes have to be made to the instrumentation. In particular, the contribution to band broadening by the chromatographic equipment must be considerably reduced. In the present study an OTLC system was developed and evaluated, which yields satisfactory results for 26 μm i. d. columns. The determination of the contribution of the chromatographic equipment to the total band broadening is discussed.     

Succession of stacking disorder in hard-sphere crystal under gravity by Monte Carlo simulation

We have performed Monte Carlo simulations of hard spheres under gravity. Vertical boundaries are hard walls, which are well separated with each other. On the other hand, the periodic boundary condition is imposed in the horizontal direction. While we previously reported enhancement of crystallinity as well as crystallization due to gravity, we present here the results that demonstrate the succession of a defect. In case that the crystal formed at the bottom of the system includes kinds of stacking disorders for the (0 0 1) growth, twin band structure develops as mediated by a stacking disorder succeeded in the crystal formed in the fluid region which lies on the bottom crystal. In case that the stacking structure along horizontal direction changes from the (1 1 1) stacking to the (0 0 1) stacking, twin band structure in the (0 0 1) stacking region develops as succeeded in the crystal transformed. The twin band structure also becomes large with its upward growth.     

The MPE/UCB far-infrared imaging Fabry-Perot interferometer (FIFI)

FIFI is an imaging spectrometer with two or three Fabry-Perot interferometers (FPI) in series for airborne astronomical observations in the far-infrared range (=40...200m). It employs 5×5 arrays of photoconducting detectors and offers spectral resolutions as small as 2km/s. Resolution and bandwidth can be set over a wide range to match a variety of astronomical sources. Cryogenic optics minimizes thermal background radiation and provides for in-flight step tunable spatial resolution. At 158 m wavelength the background-limited NEP is 3 × 10^-15W/Hz at 40 km/s resolution and with two FPI's; with three FPI's the expected NEP is 10^-15WHz at 5 km/s resolution.The frequency-chopping mode of the high-resolution Fabry-Perot allows for line detection in extended objects. Absolute internal flux calibration ensures adequate flat fielding of the array elements.     

Torsion balances with fibres of zero length

Torsion balances have good immunity to tilt and low rotational stiffness. However precise control of the position of the suspended torsion ‘bob’ is difficult in the presence of ground vibrations and tilt and this is a limiting factor in applications where Casimir forces or putative non-Newtonian short-range forces are being measured. We describe how the desirable characteristics of torsion balances can be reproduced in a rigid body that is suspended using applied forces rather than a torsion fibre. The suspension system can then provide a more precise control of the degrees of freedom of the suspended body. We apply these ideas to a superconducting levitated torsion balance, developed by the authors, and a generic electrostatic suspension. We present results of preliminary experiments that provide support for our analyses.     

碳酸氢钠浸提-连续流动分析法测定园艺植物堆肥中的有效磷

为了解堆肥中有效磷供应状况,采用碳酸氢钠浸提-连续流动分析法测定园艺植物堆肥中有效磷的含量。通过对样品前处理条件、仪器参数进行优化,确定了提取时间45 min,料液比1∶60,吸样时间35 s,清洗时间60 s,去离子水作为基线液。标准曲线的线性关系良好,相关系数大于0.999,精密度好;检出限为0.008 mg/L;与手动法相比,连续流动分析法自动化程度高,而且对环境和人均友好。