A new monolithic stationary phase containing multiwalled carbon nanotube (MWCNT) was prepared by in situ polymerization of methacrylate monomers in a silanized capillary. The novel stationary phases were studied by scanning electron microscopy, Raman spectroscopy, thermogravimetric analysis, Fourier Transform Infrared spectroscopy, and mechanical stability test. Application of the columns in ion chromatography (IC) separation of five inorganic anions provided satisfactory under the isocratic elution condition. It was observed that MWCNT in the monoliths played an important role in the IC separation. Both the column efficiencies and exchange capacities were improved by adding MWCNT in the monoliths. (C) 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 128: 741-749, 2013