Zn x Cd 1-x S nanorods were successfully synthesized by microwave method. Characterized by transmission electron microscopy, Zn x Cd 1-x S samples were composed of a large quantity of homogeneous rods with diameter about 10 nm. The photocatalytic degradation of methyl orange (MO) in the aqueous phase under visible light irradiation (420 nm < λ < 800 nm) was taken as a model reaction. The conversion of MO degradation using Zn 0.28 Cd 0.72 S as the photocatalyst was up to 96% after 6 h of irradiation. The separation and identification of degradation products were measured by liquid chromatography mass spectroscopy (LC-MS). After 6 h of irradiation, the intensity of the main absorption peak of MO (m/z ) 304) descended in mass spectrum view, while some new peaks of degradation products showed up. From these results of LC-MS analysis, it can be concluded that it was really a photocatalytic degradation process.