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The anodic oxidn. of H2SO4 to H2S2O8 was investigated on B-doped synthetic diamond electrodes obtained by hot filament chem. vapor deposition. High current efficiency for H2S2O8 formation can be achieved in concd. H2SO4 (7.5 mol dm-3) and using high current densities (200 mA cm-2). The main side reaction is oxygen evolution. [on SciFinder (R)]