Apparatus and separations in supercritical fluid chromatography
Apparatus and separations in supercritical fluid chromatography
复制标题
超临界流体色谱中的装置和分离
DOI：
10.1016/0014-3057(78)90070-8
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发表时间：
1978
期刊：
影响因子：
--
通讯作者：
W. Hartmann
中科院分区：
文献类型：
--
作者：
E. Klesper;W. Hartmann
设计了一种以压力级联为特征的超临界致密气体（超临界流体）色谱装置。由反馈回路分别控制供气部分、色谱柱和检测器的三个降压级。独立控制和编程的压力，温度和进给量，从而成为可能。以正戊烷/甲醇为流动相，多孔二氧化硅为固定相，在分析和制备尺度上进行了低聚苯乙烯的分离。该方法的分辨率似乎优于液相色谱法。峰的质谱分析表明，单体质量为1的低聚物种被清晰地分离。研究了各参数，特别是压力和温度对分离效率的影响。缓慢上升的压力和温度编程有利于分离。
An apparatus for the chromatography with supercritical dense gases (supercritical fluids) has been designed, the characteristic feature being a pressure cascade. Three decreasing pressure levels containing the supply part, the chromatographic column, and the detector, respectively are controlled by feed back loops. Independent control and programming of pressure, temperature, and feed rate thereby become possible. Separations of oligostyrenes withn-pentane/methanol as the mobile phase and porous silica as the stationary phase were carried out on analytical and preparative scales. The resolution appears to be superior to that obtainable with liquid chromatography. Mass spectra of the peaks showed that oligomeric species of 1 monomer weight are cleanly separated. The influence of the parameters, particularly pressure and temperature, on the efficiency of the separation was studied. Slow upward pressure and temperature programming were found beneficial for the separation.