Boczkaj Grzegorz, Przyjazny Andrzej, Kamiński Marian
Department of Chemical and Process Engineering, Chemical Faculty, Gdansk University of Technology, Gdansk, Poland.
J Sep Sci. 2015 Mar;38(5):741-8. doi: 10.1002/jssc.201401230. Epub 2015 Jan 27.
The paper describes a new procedure for the determination of boiling point distribution of high-boiling petroleum fractions using size-exclusion chromatography with refractive index detection. Thus far, the determination of boiling range distribution by chromatography has been accomplished using simulated distillation with gas chromatography with flame ionization detection. This study revealed that in spite of substantial differences in the separation mechanism and the detection mode, the size-exclusion chromatography technique yields similar results for the determination of boiling point distribution compared with simulated distillation and novel empty column gas chromatography. The developed procedure using size-exclusion chromatography has a substantial applicability, especially for the determination of exact final boiling point values for high-boiling mixtures, for which a standard high-temperature simulated distillation would have to be used. In this case, the precision of final boiling point determination is low due to the high final temperatures of the gas chromatograph oven and an insufficient thermal stability of both the gas chromatography stationary phase and the sample. Additionally, the use of high-performance liquid chromatography detectors more sensitive than refractive index detection allows a lower detection limit for high-molar-mass aromatic compounds, and thus increases the sensitivity of final boiling point determination.
本文描述了一种采用示差折光检测的尺寸排阻色谱法测定高沸点石油馏分沸点分布的新方法。迄今为止，色谱法测定沸程分布是通过带有火焰离子化检测的气相色谱模拟蒸馏来完成的。该研究表明，尽管在分离机理和检测模式上存在显著差异，但与模拟蒸馏和新型空柱气相色谱法相比，尺寸排阻色谱技术在测定沸点分布方面能产生相似的结果。所开发的尺寸排阻色谱法具有广泛的适用性，尤其适用于测定高沸点混合物的确切终沸点值，对于此类混合物，必须使用标准的高温模拟蒸馏法。在这种情况下，由于气相色谱柱箱的终温较高以及气相色谱固定相和样品的热稳定性不足，终沸点测定的精密度较低。此外，使用比示差折光检测更灵敏的高效液相色谱检测器可降低高摩尔质量芳香族化合物的检测限，从而提高终沸点测定的灵敏度。
