Identification of oxidation states of metal oxides by MALDI-TOF MS

For the detection of inorganic species, we have developed chemical reaction laser desorption ionization mass spectrometry, and applied it to the analysis of metal oxides in different oxidation states. Metal oxide species insoluble in common organic solvents were finely grounded in a mortar and suspended in a solvent. The turbid suspension was placed on a sample holder on which a suitable chelating reagent had been previously spotted in a similar manner for sample preparation employed in the matrix-assisted laser desorption mass spectrometry (MALDI-MS). By using this method, the mass spectra of manganese (II and IV) oxides (MnO and MnO2), cobalt (II and III) oxides (CoO and Co2O3), and chromium (III and VI) oxides (Cr2O3 and CrO3) were successfully obtained. By adjusting the experimental conditions, such as ionization modes and chelating reagents, the non-identical mass spectra were obtained for the elements in the different oxidation state. Thus, the oxidation states could be identified clearly.