Here, two strategies are simultaneously applied to ZnO for easy separation of the photocatalyst particles by forming micron-sized spheres and for extension of the spectral response into the visible region by nitrogen doping. The prepared nitrogen-doped ZnO microspheres show highly improved photocatalytic activity for the degradation of humic acid (HA), a complex refractory organic compound, under visible light. Substitutional and interstitial doping of nitrogen are behind the improved visible light absorption and photocatalytic activity. Using 1 g/L of N-doped ZnO with urea/Zn molar ratio of 3, 95.4% of HA with an initial concentration of 5 mg/L can be degraded within 80 min of visible light irradiation of 122 mW/cm(2). Under identical experimental conditions, almost complete mineralization of HA is achieved within 12 h. Holes and hydroxyl radicals are mainly responsible for the degradation of HA. Significant reduction of toxicity of the photocatalytically treated HA solution is realized within 9 h.