This research is aimed to manufacturing of lead dioxide electrode having high electrocatalytic activity and durability for the ozone evolution to treat waste water. The characteristics and electrocatalytic activities of β-PbO₂ deposited electrochemically on titanium substrate by added anionic surfactants such as sodium lauryl sulfate, sodium dodecylbenzenesulfate in HClO₄ supporting electrolyte were investigated by using XRD, SEM, cyclic voltammograms, and macro-electrolysis. Results of XRD analysis ascertained that β-PbO₂ films electrodeposited in the presence of anionic surfactant have the same tetragonal structure as pure β-PbO₂ films. The SEM results showed that these anionic surfactants tend to diminish crystal size of the deposited layer. The β-PbO₂ electrodes electrodeposited in the presence of anionic surfactant improved significantly electrocatalytic activity for anodic oxidation of dimethyl sulfoxide, benzaldehyde in 1.0M H₂SO₄ supporting electrolyte. The observed electrocatalytic phenomenon is concluded to be the beneficial consequence of surface activity generated on deposited layer when anionic surfactant was added to electrolyte, and surface activity increased surface sites capable of adsorbing hydroxyl radical which are transferred in the anodic oxygen transfer reaction. Electrode performance and durability for the evolution of ozone in perchloric acid solution with using lead dioxide electrodes electrodeposited on titanium madras have been investigated. It was ascertained that the PbO₂ electrode electrodeposited by adding sodium lauryl sulfate and NaF in HClO₄ supporting electrolyte showed the highest current efficiency and durability.