The temperature influence of the structure of polyvinyl alcohol (PVA) and polyethylene glycol (PEG) adsorption layers on the controlled porosity glass (CPG) surface was studied. Adsorption, surface charge, zeta potential and viscosity measurements were carried out in the 5–40 °C temperature range. Applied methods allowed determination of the amount of polymer adsorbed, the surface and diffuse layer charge of CPG particles in the absence and presence of the polymer as well as the thickness of polymer adsorption layers. The adsorption measurements indicated the increase of PVA and PEG adsorption with the rise of temperature. Such behavior is caused by conformation changes of polymer macromolecules. Moreover, the increase of temperature causes the increase of the thickness of polymer adsorption layers on solid surface. It is due to the fact that the increase of temperature favors more stretched conformation of polymer chains on CPG surface. From the adsorption and viscosity data were calculated parameters, which characterize changes of the polymer chains conformation on their way from liquid phase to the solid surface.