In this work, thermogravimetry-differential scanning calorimetry-mass spectrometry (TG-DSC-MS) coupling techniques were used to make a simultaneous characterizing study for the metallic iron-organic coordination compounds formed by iron ions and organic solvent glycol during the sol-gel process of preparing the iron oxide nanometer films. The positive ion mass spectra [Fe(OCH2CH3)(3)](+)(mass to charge (m/z) = 191) and [Fe(OCH2CH2OH)(3)](+) (m/z = 239) of the organic iron coordination compounds were obtained by experimental methods for the first time. Through the comparison analysis with the results of the TG-DSC-MS for the glycol, it can be found that the thermal decomposition temperature for the metallic iron-organic coordination compounds formed with glycol is higher than that of pure glycol. The results in this research work show that the simultaneous TG-DSC-MS coupling techniques can be applied to characterize some of the metallic-organic coordination compounds appeared in the gas state at lower temperature. (C) 2003 Elsevier Science B.V. All rights reserved.