Intercalation compounds HxVOPO4 . yH(2)O (x = 0.3-1.0; y = 2.0-3.6) and KxVOPO4 . yH(2)O (x = 0.2-0.98; y = 1) were prepared by redox intercalation of VOPO4 . 2H(2)O with acetone solutions of hydroquinone and potassium iodide respectively. Time course of reactions, X-ray diffraction and ac conductivity of prepared compounds were studied. The decrease of conductivity with increasing content of guest was observed. The activation energy of conductivity of HxVOPO4 . yH(2)O was calculated from the Arrhenius plot. The content of interlayer water increases during intercalation of hydronium ions as it was determined by DTA.