Selective accumulation of B-10 compound in tumour tissue is a fundamental condition for the achievement of BNCT (Boron Neutron Capture Therapy), since the effectiveness of therapy irradiation derives just from neutron capture reaction of B-10. Hence, the determination of the B-10 concentration ratio, between tumour and healthy tissue, and a control of this ratio, during the therapy, are essential to optimise the effectiveness of the BNCT, which it is known to be based on the selective uptake of B-10 compound. In this work, experimental methods are proposed and evaluated for the determination in vivo of B-10 compound in biological samples, in particular based on neutron radiography and gammaray spectroscopy by telescopic system. Measures and Monte Carlo calculations have been performed to investigate the possibility of executing imaging of the 10B distribution, both by radiography with thermal neutrons, using 6LiF/ZnS:Ag scintillator screen and a CCD camera, and by spectroscopy, based on the revelation of gamma-ray reaction products from B-10 and the H. A rebuilding algorithm has been implemented. The present study has been done for the standard case of B-10 uptake, as well as for proposed case in which, to the same carrier, is also synthesized Gd-157, in the amount of is used like a contrast agent in NMRI.