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Counter-flow Ion Mobility Analysis: Design, Instrumentation, and CharacterizationAgbonkonkon, Nosa 14 November 2007 (has links) (PDF)
The quest to achieve high resolution in ion mobility spectrometry (IMS) has continued to challenge scientist and engineers in the field of separation science. The low resolution presently attainable in IMS has continued to negatively impact its utility and acceptance. Until now, efforts to improve the resolution have mainly focused on better instrumentation and detection methods. However, since the resolution of IMS is diffusion limited, it makes sense to address this limitation in order to attain high resolution. This dissertation presents a new IMS technique, which utilizes a high electric field and opposing high gas flow velocity with the aim to improve resolution. This approach essentially reduces the residence time of ions in the analyzer. This new technique is called "counter-flow ion mobility analysis" (CIMA). Theoretical modeling of this new technique predicted that a resolution of over 1000 is possible, which is over one order of magnitude better than that of conventional IMS techniques currently used. A wind tunnel was designed and constructed to produce a plug gas flow profile that is needed for CIMA. The test region of the wind tunnel was used as the CIMA analyzer region and was constructed from power circuit boards, PCBs, (top and bottom walls) and conductive plastic side walls. An inclined electric field was created by applying suitable voltages to multiple electrode traces on the PCBs. This inclined field, when resolved into its x- and y-components, was used to oppose the counter-gas flow and transport the ions to the detector, respectively. The results obtained did not show an improvement over conventional IMS techniques because of a limitation in the voltage that could be applied to the analyzer region. However, the results predict that high resolution is possible if (1) the ratio of the electric fields in the horizontal (x direction) to the vertical (y direction) is within the range of 2--0.5, (2) very high electric field and high gas flow velocities are applied, and (3) wall effects in the counter-flow gas profile are eliminated. While the resolution obtained using the present instrumentation is far from what was predicted, the foundation for ultimately achieving high resolution has been laid. The use of a wind tunnel has made the instrumentation possible. As far as the author knows, this is the first time a wind tunnel has been used in chemical measurement instrumentation. Chapter 5 of this dissertation, reports a method developed for predicting the reduced mobility constants, of chemical compounds. This method uses a purely statistical regression analysis for a wide range of compounds which is different from similar methods that use a neural network. The calculated value for this method was 87.4% when calculated values were plotted against experimental K0 values, which was close to the value for the neural network method (i.e., 88.7%).
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