This article presents an experimental study of the chemical and mechanical properties of the cement paste / aggregate interphase. Interfacial Transition Zone (ITZ) represent the contact zone of the cement paste with the aggregate with a thickness of about 20 -50 μm. This zone has different mechanical and chemical properties compared to the bulk paste. Cement paste / limestone aggregate composite samples were performed to allow the study of the chemical and mechanical properties of ITZ. The cement paste is made with Portland cement with a water/cement mass ratio of 0.4. Calcium concentration profiles in the ITZ show a high concentration of calcium due to the presence of portlandite and ettringite. The nanoindentation tests indicate weakness of ITZ compared to bulk cement paste.