The use of ultrasound (US) and microwaves (MW) in the oxidation and purification of multi-walled carbon nanotubes (MWCNTs) was investigated. These techniques, in particular US at a frequency of 300 kHz, strongly accelerate the process and avoid the heavy structural damage, observed at the 20-35 kHz classic range, even at low power. Due to the residual metal catalyst on the head of MWCNTs, MW heating is strongly absorbed, causing the rupture of the tip and the loss of the metal. All our chemico-physical treatment types were performed by suspending the CNTs in a 31 H2SO4/HNO3 mixture. The resulting samples were investigated by TEM microscopy, TGA analyses and Raman spectroscopy, while the degree of oxidation was estimated by colourimetric analyses.