A CVD procedure has been used for the attempted synthesis of boron-doped multiwalled carbon nanotubes using BF 3 /MeOH as the boron-source, Fe/Ca(BO 3 ) 2 /CaCO 3 as catalyst and acetylene as the carbon-source. The boron-doped multiwalled carbon nanotubes were characterized by TEM, Raman spectroscopy and laser ablation mass spectrometry analysis. Variation of the boron concentration was achieved by diluting the boron-source with MeOH and dilution resulted in: (i) a higher yield of carbon material, (ii) a less disordered material and (iii) a decrease in intensity in the first- and second-order Raman spectra of boron-doped multi walled carbon nanotubes.