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The adaptation of the widely used spin probe method for the investigation of the molecular organization of swelled GO and GO membranes was the aim of the present work. Using this method it was shown that the phase transformation in the systems “BGO (Brodie synthesized graphite oxide) – polar liquid” proceeds within a temperature range of ~30°. The existence of a mobile liquid (water, acetonitrile, trifluoroethanol) in the inter-plane space of GO was confirmed reliably by EPR and NMR spectroscopy. The spin probe method was found to be a unique technique for quantitative estimation of the layer ordering in the graphite oxide membranes. It was shown that nitroxide radicals as well as paramagnetic complexes [Cu(NH3)4]2+ adequately reflect the alignment of the membranes.