A series of CoB, FeB and NiB catalysts were prepared by the chemical reduction method using base stabilized sodium borohydride solution as reducing reagent. The synthesized catalysts were characterized by using XRD, BET and FTIR spectroscopy. The UV-vis spectroscopy was used for in-situ synthesis of metal boride catalysts. With (BS)/without (WS) base stabilized NaBH4 solution was used during synthesis of metal boride catalysts as well as generation of hydrogen from the solution. The surface area gradually increased with increasing calcinations temperature upto 573 K and furthers increasing calcinations temperature the surface area decreased for the catalysts CoB-BS. The generation of hydrogen using base stabilized NaBH4 solution (BS) with the catalyst was followed as CoB-BS > NiB-BS > FeB-BS and the generation of hydrogen using without base stabilized NaBH4 solution (WS) with the catalyst was followed as CoB-BS > FeB-BS > NiB-BS. However, the generation of hydrogen was highest for CoB-BS catalyst using both of with/without base stabilized NaBH4 solution. (C) 2017 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.