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This paper describes the methodology for conducting experiments to study hydrogen diffusion through metal membranes using a specially designed diffusion chamber of an automated gas reaction controller complex. This complex allows experiments to study hydrogen diffusion with the following parameters: the inlet hydrogen pressure is up to 50 atmospheres, and the temperature in the chamber is from 30 °C to 1000 °C. The size of the samples is limited to a diameter of 10 mm and a thickness of 100 µm. The method for calculating the diffusion coefficient based on the Fick equation is also described. When studying hydrogen diffusion through a sample of Zr–1Nb alloy with nickel film deposited at the temperature of 550 °C, it was noted that phase transformations can be observed on the diffusion curve.