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Currently, standard samples with high hydrogen concentrations that meet the requirements of hydrogen extraction in an inert atmosphere are not currently available on the market. This article describes the preparation of Ti-H standard samples and the calibration of RHEN602, a hydrogen analyzer, using LECO (LECO, Saint Joseph, MI, USA). Samples of technically pure titanium alloy were chosen as the material for sample production. The creation procedure includes five main steps: sample preparation (polishing to an average roughness of 0.04 ?m using sandpaper), annealing, hydrogenation, maintenance in an inert gas atmosphere, and characterization of the samples. The absolute hydrogen concentration in the samples was determined by two methods: volumetric and mass change after the introduction of hydrogen. Furthermore, in-situ X-ray diffraction, temperature programmed desorption (TPD) analysis, and thermogravimetric analysis were used during measurements to investigate the phase transitions in the samples. As a result of this work, a series of calibration samples were prepared in a concentration range up to 4 wt % hydrogen, optimal parameters for measuring high concentrations of hydrogen. The calibration line was obtained and the calibration error was 10%.