Developments in capillary electrophoretic instrumentation and FT-IR spectrometric detection, and semi-automated FT-IR spectrometric sample deposition
Jarman, Jessica Lea
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Capillary electrophoresis (CE) and Fourier transform infrared (FT-IR) spectrometry are powerful analytical techniques currently utilized in a wide variety of problem-solving methodologies. CE is renowned for high resolution, rapid, flexible separation capabilities while FT-IR spectrometry is used for compound identification due to its characteristic functional group fingerprinting ability. Both techniques are commercially available in a wide variety of types and configurations. In this work, one branch of CE, micellar CE with and without the use of cyclodextrin chiral selectors, is used to investigate enantioselective degradation patterns in chiral pesticides. It was determined that one of three compounds investigated in three soils from various geographical regions exhibited enantioselective microbial degradation while the other two compounds showed evidence of hydrolytic degradation. Further, CE has been interfaced to an FT-IR spectrometer in an effort to expand the versatility and applicability of both techniques. The interface was characterized for electrical contact and stability, deposition characteristics, separation efficiency, and robust nature. Interface deposits were characterized for size, shape, splatter patterns, and recoverability. It was determined that separations were performed quickly and efficiently and that analytes were easily deposited, recoverable, and available for multiple analysis methods. High quality spectral identification was the primary method of analyte identification. Finally, many areas of spectral analysis require the manipulation of minute sample quantities. These samples, either in solvated or liquid form, can be easily deposited on transmission analysis windows or on a single-bounce internal reflection element. Deposits from the novel semi-automatic depositor have been characterized for size, shape, precision of placement, and success of solvent elimination. The depositor apparatus has been analyzed for stability and ease of analysis. In addition, a study was completed to determine depth of penetration coverage.