The potential of various graphite materials including Chinese flake graphite, Madagascan flake graphite, natural vein graphite, recycled vein graphite, and synthetic graphite for the preparation of -bisulfate was investigated through electrochemical intercalation method. All the graphite materials were characterized using laser particle size analyzer, SEM analysis, XRD analysis, and X-ray EDS elemental analysis. Chinese flake and Madagascan flake graphite materials were found to be capable of synthesizing GIC-bisulfate through electrochemical intercalation. Natural vein, recycled vein, and synthetic graphite materials did not show any evidence of forming GIC-bisulfate. The formation of GIC-bisulfate was verified through XRD results. Thermal exfoliation volume was observed as an indicator of GIC-bisulfate when the electrochemically treated material was exposed to a sudden thermal shock at a temperature of 850 °C.