X-ray reflectometry and spectroscopic ellipsometry methods were applied for determination of physical properties of gold nonolayers. The nanolayers were prepared by sputtering of gold on different substrates: borosilicate glass, polished crystalline quartz and crystalline silicon. With X-ray reflectometry technique roughness of the substrates and density, thickness and roughness of gold layers were determined. The results showed decrease in density of the gold layers due to their nanometer thickness and that roughness of the underlayer affects roughness of the gold layer. In addition, thicknesses of the gold layers measured with spectroscopic ellipsometry turned out to be in agreement, within the experimental uncertainty, with results of the X-ray reflectometry method.