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Single crystal Bi0. 19MoO3 has been grown by fused salt electrolytic technique. X-ray powder diffraction shows thatthe unit cell parameters are: a=1.9985nm, b=0.4085nm and c=1.4437nm. The temperature dependence of resistivitydemonstrates a semiconductor characteristic. X-ray photoemission spectroscopy studies provide that the valence bandof Bi0.19MoO3 are made up of oxygen pπ and the r*, r and σ bonding bands formed by orbital combination. Theshoulder at 0.4 eV near the top of valence band may be formed from the non-bonding dxy orbitals of some Mo atoms.The O1s core-electron spectrum reveals the presence of two inequivalent bonds of oxygen ions in Bi0.19MoO3. Bi4fcore-level spectrum shows two bonding characters of Bi atoms in bismuth molybdenum oxide single crystals. Mo3dcore-level spectrum could be decomposed into two kinds of valence states of molybdenum(Mo+5 and Mo+6).