This paper presents results that show the effect of hydrothermal carbonization and subsequent cold plasma jet treatment with helium and argon on the structure and sorption properties of a material—spent brewery grain. Treatment of activated carbon, with a cold atmospheric plasma jet, was used comparatively. The effect of activation on the pore structure of the materials was carried out by the volumetric method at low pressure (N2, 77 K). The specific surface area as well as the total pore

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... , average pore size, and pore size distribution were determined using different theoretical models. A high improvement in the sorption capacity parameter was obtained for hydrochars after cold atmospheric plasma jet treatment with an increase of 7.5 times (using He) and 11.6 times (using Ar) compared with hydrochars before cold atmospheric plasma jet treatment. The increase in specific surface area was five-fold (He) and fifteen-fold (Ar). For activated carbon, such a large change was not obtained after plasma activation. Regardless of the gas used, the increase in structural parameter values was 1.1–1.3.