The catalytic properties of plasma-chemically and thermally treated triple zirconium orthophosphates Na3ZrM(PO4)3 (M = Zn, Co, Cu) in the transformation of butanol-2 are studied. X-ray photoelectron spectroscopy data indicate that the surface composition of the samples differs from the stoichiometry, especially in the case of M = Cu. The partial reduction of copper ions occurs during plasma-chemical treatment (PCT), while the amount of Cu on the surface of Na3ZrCu(PO4)3 diminishes. Treatment in an oxygen glow discharge results in a 3-8 times greater yield of the alcohol dehydrogenation product, methyl ethyl ketone. The energy of the alcohol's bonds with the surface is reduced and the dehydration active sites become fully inactivated. In contrast, thermal treatment (TT) results in an increase in the activity of Na3ZrM(PO4)3 in the dehydration of butanol-2. © 2013 Pleiades Publishing, Ltd.