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Graphite has been oxidized to graphite hydrogensulfate with (NH 4 ) 2 S 2 Og in concentrated H 2 SO 4 . The stage 2 compound formed very rapidly, but further oxidation to stage 1 could be followed conveniently. X-ray diffraction of the intermediate phases showed nonintegral (00l)-reflections indicative of partial interstratification disorder. The interlayer spacing of the stage 1 compound increased with continued oxidation. The degree of oxidation as function of oxidation time has been determined from the position of the minima in the reflectance spectra. The density of the compounds and the ratio of acid molecules to anions in the intercalated layers has been estimated using these data and those of buoyancy measurements. There is a minimum in packing density early in the formation of the first stage. The kinetics of intercalation seems to be first order with respect to the free interlayer spaces.

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Beobachtungen von Stapelfehlordnungen bei der Oxydation der zweiten zur ersten Stufe des Graphithydrogensulfats / Observation of stacking disorder during the oxidation of second stage to first stage graphite hydrogensulfate