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Title: Instrumental development of novel detection methods for liquid chromatography and capillary electrophoresis

Thesis/Dissertation ·
OSTI ID:5938216

This dissertation presents the development and improvements of instrumental techniques for detection in liquid chromatography (LC) and capillary electrophoresis (CE). The first chapter reviews the current status of the various detection methods for LC and CE. Section 1 presents the first universal detector based on magneto-optical rotation (MOR) for high performance liquid chromatography (HPLC). The experimental results confirm the linear dependence of the MOR signal on the analyte concentration. The feasibility of this method is demonstrated in the detection of polynuclear aromatic hydrocarbons, where the limit of detection is in the sub-microgram range. For the first time, a novel axial-beam on-column absorption detector for open tubular capillary liquid chromatography is described in Section 2. For a typical 10 {mu}m i.d. capillary column, the axial-beam detection provides an increase of up to 1000 times in path length and a 192-fold associated improvement on the limit of detection. The project described in the third section is the optimization of detectability in the laser-based polarimetric detector for HPLC. A mathematical simulation is performed in order to optimize the detectability of the detector. The experimental verification of the optimized parameters provides the performance approaching the shot-noise limit. Finally, Section 4 demonstrated the feasibility of axial-beam absorption detection for capillary electrophoresis using a conventional light source. The cross-beam and axial-beam detection schemes can be easily switched. The high stability of light intensity, variable wavelength and uv ability make this detector attractive. The improved limit of detection in the axial-beam arrangement should make CE with absorption detection feasible to a wider range of applications. 139 refs., 19 figs., 2 tabs.

Research Organization:
Ames Laboratory (AMES), Ames, IA (United States)
Sponsoring Organization:
USDOE; USDOE, Washington, DC (USA)
DOE Contract Number:
W-7405-ENG-82
OSTI ID:
5938216
Report Number(s):
IS-T-1526; ON: DE91010926
Resource Relation:
Other Information: Thesis (Ph.D.). Thesis submitted to Iowa State University
Country of Publication:
United States
Language:
English