A solution of Orange II, one of the typical azo dyestuffs was electrolyzed by Solid Polymer Electrolyte (SPE) electrolysis with two high oxygen overvoltage anodes, PbO
2 and SnO
2 without adding any electrolytes. The solution was decolorized completely by the 120 minutes electrolysis, using PbO
2 anode at current density of 0.2 A·:cm
-2. However, even after 180 minutes of electrolysis with PbO
2 anode at 0.3 A·cm
-2, 60% of total organic carbon (TOC) and 35% of chemical oxygen demand (COD) remained. Biodegradability of the electrolyzedobserved at high current density condition (about 0.5 A·cm
-2) and longterm electrolysis (about 200 hours). TOC reduction was higher for SnO
2 electrode doped with 1% Sb than for PbO
2. Although Sb doping reduced cell resistance, the electrolytical cell voltage for SnO
2 (8.5V) was much higher than that of PbO
2 (3.5V).
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