This research applied the techniques of CP MAS Si-29 and C-13, MAS high power decoupling C-13, and MAS H-1 solid-state NMR, variable-temperature dependent H-1 NMR, Xe-129 NMR, low temperature H-1 diffusion, and two-dimensional exchange Xe-129 NMR to study the structure, dynamics, and interaction of the stationary phase and the xenon atoms in the Zorbax SB-C18 HPLC column material. The solid-state NMR experimental results showed the single binding type of alkylsilane groups, -Si(CH2-CH-(CH3)(2))(2)(CH2)(17)CH3, and the mobile alkyl chains on the silica surface at room temperature. The VT H-1 NMR and H-1 spin diffusion experiments suggested that at low temperatures a large portion of the alkyl chain molecules became immobile in the area where the density of the alkyl chains could be higher, while the rest of the alkyl chains remained somehow mobile in the areas with possibly lower density. The results of the VT Xe-129 NMR experiments showed the solvation of the xenon atoms in the stationary phase, the spatial occupation of the xenon atoms in the void spaces of the column material, and the diffusion of the xenon atoms in the column material. The two-dimensional exchange Xe-129 NMR results at low temperatures displayed the slow xenon diffusion between the pores and the voids between the particles. The two-dimensional exchange Xe-129 NMR spectra also indicate that the amorphous areas of the alkyl chains in the stationary phase experienced slow motions even at a temperature of -140 degreesC. This research illustrated that solid-state NMR of the stationary phase and Xe-129 NMR of the mobile phase give complementary information concerning the structure, dynamics, and interaction of column materials.