Polyoxometalates having various structures and properties can be organized by the Langmuir-Blodgett (LB) technique. The adsorption of such polyanions along a positively charged monolayer of DODA (dimethyldioctadecylammonium) induces large changes in the compression isotherm and enables the transfer of the Langmuir Nm onto solid substrate. X-ray diffraction and infrared dichroism experiments demonstrate that the polyoxometalates are organized in monolayers within the LB films. Furthermore, these magnetic multilayers were characterized by their paramagnetic susceptibility measured by a SQUID magnetometer.