Neutron emission measurements are carried out by means of a He3 detector on Carrara marble specimens under compression. While iron-rich minerals generate neutrons—due to phono-fission reactions involving the transformation of one iron atom into two atoms of aluminum or into other lighter elements—this phenomenon does not appear in marble crushing tests. On the other hand, significant alpha particle emissions are detected by a 6150AD-k probe during the same compression tests on marble. The external and fracture surfaces belonging to Carrara marble specimens crushed during the compression tests are analyzed by X-ray Photoelectron Spectroscopy (XPS). Such quantitative compositional analyses are carried out in order to detect any variation in Carrara marble chemical composition due to brittle failure. A total decrement in Ca, Mg, and O by 13% is exactly equivalent to the increment in C, which is observed on the fracture surface, with respect to the external surface. The assumed transmutations involve elements with an equal number of protons and neutrons. Due to this peculiar reason, the microchemical analyses suggest phono-fission reactions with alpha particle emission, and not excess neutron emission.