Wastewater containing pharmaceutical residual components must be treated before being discharged to the environment. This study was conducted to investigate the efficiency of tungsten-carbon nanocomposite in diclofenac removal using design of experiment (DOE). The 27 batch adsorption experiments were done by choosing three effective parameters (pH, adsorbent dose, and initial concentration) at three levels. The nanocomposite was prepared by tungsten oxide and activated carbon powder in a ratio of 1 to 4 mass. The remaining concentration of diclofenac was measured by a spectrometer with adding reagents of 2, 2'-bipyridine, and ferric chloride. Analysis of variance (ANOVA) was applied to determine the main and interaction effects. The equilibrium time for removal process was determined as 30 min. It was observed that the pH had the lowest influence on the removal efficiency of diclofenac. Nanocomposite gave a high removal at low concentration of 5.0 mg/L. The maximum removal for an initial concentration of 5.0 mg/L was 88.0% at contact time of 30 min. The results of ANOVA showed that adsorbent mass was among the most effective variables. Using DOE as an efficient method revealed that tungsten-carbon nanocomposite has high efficiency in the removal of residual diclofenac from the aqueous solution.