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Dissertation Jiayi Liu.pdf (29.48 MB)

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Development and Applications of Functionalized Octatetrayne as Novel Carbon Media in Chromatography

Liu, Jiayi
http://rave.ohiolink.edu/etdc/view?acc_num=osu1519322396476316

Abstract Details

2018, Doctor of Philosophy, Ohio State University, Chemistry.
Open tubular capillary columns, in which stationary phases are coated onto inner wall, have been continuously developed for chromatographic use. Functionalized octatetrayne was synthesized and covalently attached to the capillary column inner wall. Thermal processing at elevated temperatures ensured the formation of a uniform ultrathin layer carbon stationary phase. This robust coating method extended the novel carbon stationary phase into open tubular liquid chromatography and comprehensive two-dimensional gas chromatography for the first time. Open tubular liquid chromatography (OTLC) has potentially high efficiency, fast analysis time and low solvent consumption. The chromatographic performance of the carbon capillary column strongly depended on the final curing temperature, sample size and mobile phase composition. The optimal curing temperature of the carbon phase was determined to be 400 °C. Good separations using the carbon column were obtained on the basis of reversed-phase interactions. The high surface area and unique selectivity of the carbon phase led to improved retention and efficiency for the separations of polycyclic aromatic hydrocarbons (PAHs) and nucleosides at isocratic conditions. The separation impedance of the carbon OTLC was more than 100-fold of commerical packed or monolithic columns. Comprehensive two-dimensional gas chromatography (GCxGC) is recognized as a powerful tool for complex mixtures due to its high peak capacity. Due to the unique selectivity of the carbon phase, the carbon column was utilized as the second dimension coupled to a nonpolar first dimension commercial column using a reverse-inject differential flow modulator. The carbon GCxGC was optimized using an experimental design method and the chromatographic performance of the carbon GCxGC was evaluated by separating a mixture of hydrocarbons. The carbon column offered improved separation space and comparable separation power to a commercial HP-INNOWax column. The superior stability of the carbon phase also expanded the separation temperature range up to 350 °C with no column bleeding and maintained selectivity. The carbon GCxGC also provided feasibility and potential for complex separations such as fuel oil samples. Month-to-month and column-to-column reproducibility tests were performed on both the carbon OTLC and GCxGC systems. The low relative standard deviations (<8%) for the retention times of tested species confirmed high durability of the carbon stationary phase for both LC and GCxGC, and excellent reproducibility of the coating method.
Susan Olesik (Advisor)
251 p.
Analytical Chemistry
Open tubular columns; liquid chromatography; two-dimensional gas chromatography; carbon materials

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Citations

  • Liu, J. (2018). Development and Applications of Functionalized Octatetrayne as Novel Carbon Media in Chromatography [Doctoral dissertation, Ohio State University]. OhioLINK Electronic Theses and Dissertations Center. http://rave.ohiolink.edu/etdc/view?acc_num=osu1519322396476316

    APA Style (7th edition)

  • Liu, Jiayi. Development and Applications of Functionalized Octatetrayne as Novel Carbon Media in Chromatography. 2018. Ohio State University, Doctoral dissertation. OhioLINK Electronic Theses and Dissertations Center, http://rave.ohiolink.edu/etdc/view?acc_num=osu1519322396476316.

    MLA Style (8th edition)

  • Liu, Jiayi. "Development and Applications of Functionalized Octatetrayne as Novel Carbon Media in Chromatography." Doctoral dissertation, Ohio State University, 2018. http://rave.ohiolink.edu/etdc/view?acc_num=osu1519322396476316

    Chicago Manual of Style (17th edition)

osu1519322396476316
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This open access ETD is published by The Ohio State University and OhioLINK.