The process parameters (viz. temperature of synthesis, type of catalyst, concentration of catalyst and type of catalyst-support material) for controlling purity of carbon nanotubes synthesized by catalytic chemical vapour deposition of acetylene have been optimized by analyzing the experimental results using Taguchi method. It has been observed that the catalyst-support material has the maximum (59.4%) and the temperature of synthesis has the minimum effect (2.1%) on purity of the nanotubes. At optimum condition (15% ferrocene supported on carbon black at the synthesis temperature of 700 degrees C) the purity of nanotubes was found out to be 96.2% with yield of 1900%. Thermogravimetry has been used to assess purity of nanotubes. These nantubes have been further characterized by scanning electron microscopy, transmission electron microscopy and Raman Spectroscopy. Small angle neutron scattering has been used to find out their average inner and outer diameter using an appropriate model. The nanotubes are well crystallized but with wide range of diameter varying between 20-150 nm.