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Transmission Mossbauer spectra of binary coprecipitated nickel(I1)-iron(II1) hydroxides (molar ratios 9 : 1 and 4:l) are analysed and compared with the results of AES analyses of their surface composition. A correlation between the data of the above techniques has been noted, indicating a redistribution of the components (i.e. Ni and Fe) in the surface layers, the latter being enriched with iron(1II) as compared to the bulk. The results obtained are in good agreement with an excellent electrocatalytic activity of composite Ni-Fe hydroxide systems towards anodic oxygen evolution in alkaline electrolytes, taking into account a distinctly exhibited 'surface' electrocatalytic effect of ferric species on the nickel hydroxide electrode in the anodic oxygen evolulion process revealed previously. Transmission Miissbauer spectroscopy has been shown to be a highly effective prob sensitive both to various bulk and surface effects related to the solid phases studied.

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