Nanocrystals of a new CN phase of presumably orthorhombic type embedded in an amorphous CN, (x < 0.2) matrix produced by magnetron sputtering have been identified, The evidence for the co-existence of different phases in the sample is first given by spatially resolved electron energy loss spectroscopy (EELS). A mathematical treatment of collections of EELS spectra applied to the core-edge fine structures (energy loss near edge fine structures (ELNES)) was used to isolate the characteristic signature of the different phases. Electron diffraction patterns and high-resolution transmission electron microscopy images (HRTEM) were then carried out from areas displaying the characteristic identified ELNES to confirm the identification of the structure and chemistry of these nanocrystals.