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Spin probes such as nitroxide radicals TEMPOL and TEMPO could be embedded into the inter-plane space of swelled graphite oxide. Experimental EPR spectrum of the systems graphite oxide – polar liquid – spin probe could be considered as superposition of three individual spectra: the intrinsic spectrum of graphite oxide, the spectra of sorbed radicals, and the fast rotating radicals in the presence of polar liquid. In the system “graphite oxide – acetonitrile” the reversible phase transition like incongruent melting with the release of part of the sorbed liquid was found at T=285-300 K as a sharp decrease of rotational mobility of the sorbed radicals. The liquid-like behavior of the polar liquids sorbed into the inter-plane space of graphite oxide was shown using TEMPO radical.