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The chiral separation principle ligand-exchange is applicable for HPLC, capillary electrophoresis as well as for capillary electrochromatography. Among other chiral separation principles, ligand-exchange permits simple method optimization and can be used particularly for chiral amino acids, amino alcohols or α-hydroxy acids. Up to now, three different approaches how to prepare capillaries for ligand-exchange electrochromatography have been published: The use of packed columns, monolithic columns, and particle-loaded columns. This chapter describes examples for the preparation of such columns for all three approaches and illustrates their use for chiral separations.