A sensor of a WO3 nanopores electrode combined with a thin layer reactor was proposed to develop a Chemical Oxygen Demand (COD) determination method and solve the problem that the COD values are inaccurately determined by the standard method. The visible spectrum, e.g., 420 nm, could be used as light source in the sensor we developed, which represents a breakthrough by limiting of UV light source in the photoelectrocatalysis process. The operation conditions were optimized in this work, and the results showed that taking NaNO3 solution at the concentration of 2.5 mol·L−1 as electrolyte under the light intensity of 214 μW·cm−2 and applied bias of 2.5 V, the proposed method is accurate and well reproducible, even in a wide range of pH values. Furthermore, the COD values obtained by the WO3 sensor were fitted well with the theoretical COD value in the range of 3–60 mg·L−1 with a limit value of 1 mg·L−1, which reveals that the proposed sensor may be a practical device for monitoring and controlling surface water quality as well as slightly polluted water.
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