The use of low dielectric constant materials in the on-chip interconnect process reduces interconnect delay, power dissipation and crosstalk noise. To achieve the requirements of the ITRS for 2007-2009 minimal sidewall damage from etch, ash or cleans is required. In chemical vapor deposited (CVD) organo-silicate glass (OSG) which are used as intermetal dielectric (IMD) materials the substitution of oxygen in SiO2 by methyl groups (-CH3) reduces the permittivity significantly (from 4.0 in SiO2 to 2.6-3.3 in the OSG), since the electronic polarizability is lower for Si-C bonds than for Si-O bonds. However, plasma processing for resist stripping, trench etching and post-etch cleaning removes C and H containing molecular groups from the near-surface layer of OSG. Therefore, compositional analysis and chemical bonding characterization of structured IMD films with nanometer resolution is necessary for process optimization. OSG thin films as-deposited and after plasma treatment are studied using X-ray absorption spectroscopy (XAS) and electron energy loss spectroscopy (EELS). In both techniques, the fine structure near the C1s absorption or energy loss edge, respectively, allows to identify C-H, C-C, and C-O bonds. This gives the opportunity to differentiate between individual low-k materials and their modifications. The O1s signal is less selective to individual bonds. XAS spectra have been recorded for non-patterned films and EELS spectra for patterned structures. The chemical bonding is compared for as-deposited and plasma-treated low-k materials. The Fluorescence Yield (FY) and the Total Electron Yield (TEY) recorded while XAS measurement are compared. Examination of the C 1s near-edge structures reveal a modified bonding of the remaining C atoms in the plasma-treated sample regions.