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Electrochemical oxidation methods for recalcitrant toxic wastes treatment have attracted a great deal of attention because the methods are environmentally friendly and do not produce new toxic wastes.Chemiluminescence (CL) is a powerful analytical technique that has excellent sensitivity, wide linear dynamic range and requires relatively simple and inexpensive instrumentation.Since chemiluminescence always originates from redox reaction, it probably exists during the process of electrochemical oxidation.The mechanism can be researched through instantaneous and sensitive CL.