Precursor phenomena of melting in pure metals and alloys have been investigated by means of Mechanical Spectroscopy (MS) and High Temperature X-ray Diffraction (HT-XRD). The examined materials were the pure metals In, Sn, Pb and Bi, and some alloys of the systems In-Sn and Pb-Bi with different compositions. MS tests have been carried out by means of a novel method developed by us that permits to operate in resonance conditions and employs hollow reeds of stainless steel containing the liquid metal. In all the metals a sharp drop of dynamic modulus and a Q-1 maximum were observed in a temperature range ΔT before melting that depends on the specific metal and its structure. Such anelastic behaviour is consistent with an increase of the inters...