The suitability of a selection of amorphous alloys as electrocatalysts or as inhibitors for hydrogen evolution (HE) was investigated in 1 M KOH at 25 degrees C. Mild basic conditions were chosen so as to make direct comparison with other data, where available. The alloys studied were the known glassy alloys Fe67Co18B14Si1, Co66Fe4Si16B12Mo2, Fe40Ni40B20 and Fe40Ni40P14B6 and an entirely new glassy alloy Zr73.22Ti19.71Cu1.24Fe5.83. The electrochemical techniques of slow sweep anodic and cathodic polarisation were used, in conjunction with the surface analysis techniques of scanning electron microscopy (SEM) and X-ray analysis, to characterise the alloys and new data has been obtained for all alloys. The glassy alloys were tested in their as-polished state, as well as after surface activation, by ex situ chemical (acid etching) and in situ electrochemical (anodic oxidation in base) pre-treatment. The least corrosion resistant composition, Fe67Co18B14Si1, displayed the highest activity for HE in the as-polished state and only a minor improvement resulted from surface pre-treatment. Corrosion resistance was partly characterised by the degree to which the passive region increased and the passive region current decreased as a function of pre-treatment. The most corrosion resistant alloy, Zr73.22Ti19.71Cu1.24Fe5.83, displayed the poorest activity for HE in the as-polished state, but a significant improvement resulted from surface activation by in situ anodic oxidation in basic media. Surface activation by acid pre-treatment reduced the corrosion resistance of the Zr73.22Ti19.71 Cu1.24Fe5.83 alloy and was, therefore, a non-viable and destructive procedure. However, acid pre-treatment was effective in substantially activating the glassy Co66Fe4Si16B12Mo2 and Fe40Ni40P14B6 alloys towards HE and did not alter the corrosion properties of these compositions. A novel technique for mounting thin alloy specimens has been developed, using an insulating photo-resist coating, resulting in sharply defined electrode edges.