Coulometric determination of microamounts of hydrogen in metal

Hydrogen in metal was extracted into a carrier gas (argon) by heating at about 1100 degrees , and oxidized to water with copper(II) oxide. The water was converted into ammonia with sodium amide at 80 degrees . The ammonia was then titrated with electrolytically generated hypobromite ion. The blank value of single determination could be reduced to less than 1 mug of water. Hydrogen in stainless steels, tantalum metal and pure tin metal could be determined satisfactorily, and some results were compared with those obtained by the ordinary vacuum extraction method.