Degradation of 4-chloro-3,5-dimethylphenol (PCMX) by a heterogeneous Fenton-like process using nanoparticulate zero-valent iron (nZVI) and hydrogen peroxide (H 2 O 2 ) at pH 6.3 was investigated. Interactive effects of three factors-initial PCMX concentration, nZVI dosage, and H 2 O 2 concentration-were investigated using the response surface method based on the Box-Behnken design. Experimental results showed that complete decomposition of PCMX and 65% of total organic carbon removal were observed after 30 min of reaction at neutral pH under recommended reaction conditions: nZVI, 1.0 g/L; H 2 O 2 , 18 mM; and initial PCMX concentration, 0.15 g/L. Based on the effects of scavengers n-butanol and KI, removal of PCMX was mainly attributed to the attack of OH, especially the surface-bonded OH. A possible degradation pathway of PCMX was proposed.