Immobilized polysaccharide chiral stationary phases (CSPs) are a new development in chiral chromatography with increasing importance for the resolution of racemic compounds. These CSPs can be used with solvents traditionally applied for the classical coated polysaccharide CSPs as well as solvents that were "forbidden" for the coated phases such as tetrahydrofuran, chloroform, dichloromethane, acetone, 1,4-dioxane, ethylacetate, and certain ethers. However, these forbidden solvents may be required for the determination of the chiral recognition mechanism. Therefore, the immobilized CSPs are effective for the evaluation of chiral recognition mechanisms. Furthermore, immobilized chiral columns are also useful for monitoring the progress of stereospecific synthetic reactions which are normally performed in such solvents. The present chapter describes the detailed experimental protocol of a chiral resolution on immobilized polysaccharides CSPs by HPLC.