The article presents the results of studying the elemental composition of films of CuNi alloys by X-ray microanalysis (an X-ray microanalyzer based on an energy-dispersive spectrometer, which is part of the REM-103-01 scanning electron microscope). Alloy films 30-150 nm thick were obtained by simultaneous separate evaporation of the components (copper and nickel) in a vacuum of 10 -4 Pa. Copper was evaporated from a tungsten foil ribbon 0.05 mm thick. Nickel was evaporated by the electron beam method using an electron diode gun. The condensation rate was 0.5-1.5 nm/s. The purity of the evaporated metals was no less than 99.98 %. The calculated composition of the concentrations of the sample components varied over a wide range. The characteristic X-ray spectrum of the film substance was excited by scanning a section of the film with dimensions of 300 300 μm with an electron beam; for thicker films, the size of the scanning area was 1 1 μm. Thin Ni films of the same thickness were used as standards for quantitative measurements of the elemental composition of alloy films of a certain thickness. The results of X-ray microanalysis indicate a high purity of the films. Comparison of the calculated concentrations of alloys and the results of measurements by X-ray microanalysis showed that in the region of film thicknesses d 100 nm, the discrepancy is about 10 %, decreasing to 1 -3 % for sample thicknesses d 100 nm.