关键词: UiO-66 fast separation gas chromatography in situ growth metal–organic frameworks

来  源:   DOI:10.3390/molecules29112505   PDF(Pubmed)

Abstract:
The thermally stable zirconium-based MOF, UiO-66, was employed for the preparation of bonded porous-layer open-tubular (PLOT) GC columns. The synthesis included the in situ growth of the UiO-66 film on the inner wall of the capillary through a one-step solvothermal procedure. SEM-EDX analysis revealed the formation of a thin, continuous, uniform, and compact layer of UiO-66 polycrystals on the functionalized inner wall of the column. The average polarity (ΔIav = 700) and the McReynolds constants reflected the polar nature of the UiO-66 stationary phase. Several mixtures of small organic compounds and real samples were used to evaluate the separation performance of the fabricated columns. Linear alkanes from n-pentane to n-decane were baseline separated within 1.35 min. Also, a series of six n-alkylbenzenes (C3-C8) were separated within 3 min with a minimum resolution of 3.09, whereas monohalobenzene mixtures were separated at 220 °C within 14s. UiO-66 PLOT columns are ideally suited for the isothermal separation of chlorobenzene structural isomers at 210 °C within 45 s with Rs ≥ 1.37. The prepared column featured outstanding thermal stability (up to 450 °C) without any observed bleeding or significant impact on its performance. This feature enabled the analysis of various petroleum-based samples.
摘要:
热稳定的锆基MOF,UiO-66用于制备粘合的多孔层开管式(PLOT)GC柱。合成包括通过一步溶剂热法在毛细管内壁上原位生长UiO-66膜。SEM-EDX分析显示,连续,制服,和UiO-66多晶的致密层在柱的功能化内壁上。平均极性(ΔIav=700)和McReynolds常数反映了UiO-66固定相的极性性质。使用少量有机化合物和实际样品的几种混合物来评估制造的色谱柱的分离性能。从正戊烷到正癸烷的直链烷烃在1.35分钟内基线分离。此外,在3分钟内分离出一系列六个正烷基苯(C3-C8),最小分辨率为3.09,而单卤代苯混合物在220°C下在14s内分离。UiO-66PLOT柱非常适合在210°C下在45s内等温分离氯苯结构异构体,Rs≥1.37。制备的柱具有出色的热稳定性(高达450°C),没有任何观察到的渗出或对其性能的显着影响。此功能可以分析各种基于石油的样品。
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