This paper presents a combined application of in-situ and ex-situ evaluations of products obtained by thermochemical recycling process of NaBH4 from NaBO2-Mg-H-2 ternary system. In-situ yield evaluation according to on-line pressure measurements of hydrogen gas, although already applied by some authors, is presented here with an innovative analysis which offers a thorough comprehension of the NaBH4 regeneration process making feasible the qualitative and quantitative estimations of product and by-product. On the basis of in-situ observations, NaBH4 formation in presence of NaBO2-Mg-H-2 ternary system initiates slowly from 400 degrees C and accelerates above 550 degrees C to the melting point of Mg at 650 degrees C. MgH2 is significantly produced between 370 degrees C and 450 degrees C in both heating and cooling. The amounts of these products produced at the different temperatures are clearly detectable by hydrogen pressure drops. Additionally, ex-situ evaluations by titration of NaBH4 have also been performed in order to confirm the correct interpretation of the experimental data. Copyright (C) 2013, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.