The graphite intercalation compounds CxC8F17SO3·yF and CxN(CF3SO2)2are prepared in 48% hydrofluoric acid, using the oxidant K2MnF6under ambient conditions. Analyses of PXRD peak position and periodic oscillation of the peakwidth indicate that the stable product CxC8F17SO3·4F is comprised of a random solid solution of stage 2 and 3. The addition of conc. HNO3or fuming H2SO4to 48% aqu. HF produces a stage 2 GIC. Structure refinement indicates a helical conformation of the anion. Stage 2 CxN(CF3SO2)2(x = 37) is obtained within 15 minutes under ambient condition in 48% aqu. HF. The anion orientations for these GICs are evaluated by structural refinement. Larger anions containing -CnF2n+1SO2substitutents can also be intercalated.