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Structural and electronic properties of the as‐grown (011) crystal face and the mechanically polished (001) surface of potassium titanyl phosphate (KTiOPO4or KTP) have been investigated by core‐level x‐ray photoelectron spectroscopy and reflection high‐energy electron diffraction (RHEED). With XPS analysis the original element binding energies, Auger parameters for K 2p3/2and P 2p core levels, relative element contents and valence band structure have been determined for both crystal cuts. A great depletion of O, K and P in the (011) face with respect to the (001) surface was discovered on comparison of element peak areas. The Ti 2p3/2peak areas were virtually the same for both cuts investigated. The relative element contents at the (001) surface were very close to the formal composition of KTiOPO4, so it is optimal to use the polished (001) KTP surface cleaned by ion bombardment and the Ti 2p3/2core level as standards for determination of the chemical composition of doped crystal surfaces. Copyright © 2002 John Wiley & Sons, Ltd.