Sodium borohydride (NaBH4) determination, both qualitative and quantitative, is of great significance in a plethora of areas. These include NaBH4 for energy systems such as direct borohydride fuel cells and in hydrogen production and storage, as well as use as a reducing agent in organic and inorganic synthesis reactions or in electrodeposition processes. Herein the main methods for NaBH4 monitoring have been summarised and described, including hydrogen evolution, hydride hydrolysis and iodate methods, and different electrochemical and spectroscopic techniques overviewed.