Alpha-spectrometric method has been used for the determination of boron in borosilicate glasses. For irradiation thermal neutrons with a flux of about 105 n·cm−2·s−1, produced in a paraffin moderator surrounding a deuteron target of a small neutron generator, were used. Alpha-particles from the reaction10B(n, α) were detected by a Si solid state detector with a resolution of about 50 keV. The sensitivity of the method is 0.05 wt % boron in glass samples.