Oxo molybdenum (V) complexes of substituted 8-quinolinols were synthesized and characterized by means of the investigation of elemental analysis, infrared spectra, electron spectra, electric conductivity and mass spectrometry compared with oxo molybdenum (VI) complexes. Oxo molybdenum(V) complexes were nonelectrolyte and one strong band of stretching mode of molybdenum and terminal oxygen appeared approximately $940cm^{-1}$. Oxo molybdenum(VI) complexes gave two peaks corresponding molybdenum containing ions, a molecular ion (I) of a 2 : 1 (ligand : metal) chelate and a fragment ion (II) of a 1:1 chelate due to the loss of ligand radical from ion (I). Molybdenum(V) complexes were observed the fragment ion(II) of a 1 : 1 chelate partly. The electronic spectra corresponding to d-d transition and charge transfer transition were observed and interpreted