Experimental Analysis and Reconstruction of the Morphology of Particulate and Monolithic Chromatographic Beds
This dissertation is concerned with the acquisition of three-dimensional image data of chromatography columns in capillary format using confocal laser scanning microscopy as well as with the reconstruction and analysis of the acquired image data in view of the dispersive properties of the separation...
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|Summary:||This dissertation is concerned with the acquisition of three-dimensional image data of chromatography columns in capillary format using confocal laser scanning microscopy as well as with the reconstruction and analysis of the acquired image data in view of the dispersive properties of the separation column. Key aspect in the characterization are radial heterogeneities because in UHPLC these heterogeneities contribute in large part to dispersive band broadening. Therefore, radial heterogeneities carry a particular significance in the development of chromatography columns of improved separation efficiency. Consecutively, the topics that are covered in the individual chapters of this work are being summarized: - Chapter 1 and 2 deal with the development of a sample setup for the aberration free optical imaging of capillary chromatography columns via confocal laser scanning microscopy. Additionally, image processing methods are presented that enable image restoration, particle detection, and segmentation of acquired image data. The image data were analyzed using chord length distributions and radial porosity profiles. Subsequent chapters are concerned with the application of the presented method. Herein, focus lies on a characterization of local structural density on the length scales used in J.C. Giddings’ eddy dispersion theory. - In Chapter 3 the separation efficiencies of eleven MTMS-hybrid monoliths were correlated with pore size distribution and wall attachment which outlines a fundamental problem that accompanies the preparation of capillary monoliths. - A first study on the influence of packing parameters on separation efficiency and bed morphology of packed beds was performed in Chapter 4. Six capillary columns of varying inner diameter from 10 µm to 75 µm were packed with 1.7 µm Acquity BEH particles and evaluated for their chromatographic and morphological properties. It was observed that separation efficiency would drop with increasing capillary i.d.. This could be explained by a lower packing density in the wall region of these capillaries. Furthermore, size segregation of particles was observed. - Chapter 5 discusses morphological differences between capillaries packed with core–shell particles and capillaries packed with fully porous particles. Owed to their differing production process the former do have a particle size distribution that is much narrower than the particle size distribution of fully porous particles, which yields a substantially different ordering of the particles in the wall region of the capillaries. - Chapter 6 compares a silica monolith and a sub-2 µm packing in 20 µm i.d. capillaries. The study discusses the microstructure of these columns with regard to transchannel, short-range interchannel, and transcolumn dispersion using the already established descriptors and discusses the potential of each kind of bed structure. - Chapter 7 picks up the results of Chapter 4 and shows how bed microstructure is affected by the slurry concentration used in the slurry packing process. The study showed that the previously observed size segregation of particles can be suppressed by increasing the slurry concentration yielding improved separation efficiency. The trade-off with higher slurry concentrations was an increased number of packing gaps, both in fully porous and core–shell packed beds. Once again, the chapter highlights the potential of using microscopic reconstruction and an analysis of macroscopic separation efficiency comprehensively and illustrates that the packing of beds of increasing inner diameter requires higher slurry concentrations. The concentrations should be chosen to suppress particle size segregation while keeping the amount of packing gaps as small as possible.|