This paper presents experimental results in study of hydrogen accumulation in technically pure titanium alloy at saturation from gas atmosphere. Automated complex Gas Reaction Controller was used for hydrogen saturation from gas atmosphere. Hydrogen concentration increases significantly in technically pure titanium alloy with increasing the temperature of hydrogen sorption process from 350 °C to 500 °C. At hydrogen saturation from gas atmosphere at temperature 500 °C increasing of saturation time from 10 minutes to 120 minutes leads to hydrogen concentration increasing from 0.1 wt.% to 1 wt.% and increasing of hydrides volume content throughout the samples. The activation energy for hydrogen evolution has been estimated by thermal desorption spectroscopy method by equal 102 kJ/mol.