Comparative Thermal and Thermodynamic Study of Homologous series by Chromatography using Liquid Crystalline Stationary Phase

Bouchareb Hadj, B. Mokhtar, Djedid Mebrouk, Tafer Asma, Mounir Habati, Al-Dujaili A. H.
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Abstract

This work consisted in the preparation and the study of a new stationary phase based on liquid crystals for gas chromatography applications. Most of the synthesized compounds that have the character of liquid crystals in their constitution include aromatic molecules. In addition, there is little work that replaces this type of molecules with heterogeneous molecules that have a liquid crystalline character. This study constitutes an approach for the synthesis of a new molecule azoesters involves a 1,3,4-oxadiazole unit instead of aromatic rings, and which exhibits liquid crystalline characters. A liquid crystal has been prepared and characterized. The thermodynamic characteristics of the n-alkanes for the filled column were studied by reverse gas chromatography. The intermediate products, as well as the mesogens obtained, were characterized by various experimental analysis techniques such as infrared spectrometry (IR) and nuclear magnetic resonance (NMR). The thermal properties of synthesized liquid crystal require the use of DSC technique. Thermodynamic parameters such as enthalpies, partial solution molar entropy and infinite dilution, were determined for the liquid crystal-solvent system. The thermodynamic quantities show that these values depend on the number of carbon atoms of the CL phase terminal substituent. The transition temperatures obtained by gas chromatography are in good agreement with those found by DSC.
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液晶固定相色谱法对同源系的热、热力学比较研究
这项工作包括制备和研究一种新的基于液晶的气相色谱固定相。大多数具有液晶结构特征的合成化合物都含有芳香分子。此外,用具有液晶特征的异质分子代替这种类型的分子的工作很少。本研究提出了用1,3,4-恶二唑代替芳环合成具有液晶特征的新型分子偶氮酯的方法。制备了一种液晶并对其进行了表征。用反相色谱法研究了填充柱中正构烷烃的热力学特性。通过红外光谱(IR)和核磁共振(NMR)等实验分析技术对中间体产物以及所得到的中间产物进行了表征。合成液晶的热性能要求采用DSC技术。测定了液晶-溶剂体系的焓、部分溶液摩尔熵和无限稀释度等热力学参数。热力学量表明,这些值取决于CL相末端取代基的碳原子数。气相色谱法测定的转变温度与DSC法测定的结果吻合较好。
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