Multi-walled carbon nanotubes (CNTs) and nitrogen-doped carbon (CN x) nanotubes have been synthesized by the aerosol-assisted chemical vapour deposition (CVD) method. The samples were prepared from toluene and acetonitrile taken in different proportion. The structure of CNTs and CN x nanotubes was compared using first- and second-order Raman spectra. The disorder-induced D band was found to up-shift with increase of the acetonitrile fraction. The ID/IG and IG'/I G ratios showed the opposite dependence on the doping level of CNTs. Both kinds of the substitute nitrogen: graphitic-like and pyridinic-like contribute to the disorder in CNx nanotube layers. (Graph Presented) © 2008 Wiley-VCH Verlag GmbH & Co. KGaA.