Nitrogen-containing wastewater is an important issue in optoelectronic and semiconductor industries. Wastewater containing nitrogen compounds such as ammonium, monoethanolamine (MEA), and tetramethylammonium hydroxide (TMAH) must be properly treated due to concerns about health and environmental effects. MnCe-GAC (granular activated carbon) processes were developed in this study for the treatment of TMAH-contaminated wastewater in high-tech industries. The MnCe-GAC processes could effectively remove ammonium, MEA, and TMAH from aqueous solutions. The removal efficiencies of ammonium and MEA by these processes were better than observed for TMAH. Parameters affecting TMAH removal such as type of process, type of wastewater (synthetic or real), pH, salts, and t-butanol were investigated. In general, removal efficiencies of TMAH by various processes were in the following order: MnCe-GAC/O3/H2O2 > MnCe-GAC/O3 > MnCe-GAC/H2O2 > MnCe-GAC > GAC. The negative effect of sulfate and nitrate on pollutant removal might be due to the salting-out effect. Based on t-butanol experiments, the main degradation mechanisms of TMAH by the MnCe-GAC/O3/H2O2 process likely involved hydroxyl radicals. The process proposed in this study could be an effective alternative method for the treatment of high-tech industrial wastewater to meet the new TMAH discharge limit.