Metal-organic frameworks (MOFs) containing Fe, Cr, Ni, and Cu were calcined under nitrogen flow. The formation of carbonized MOFs (CMOFs) was monitored by electrical conductivity, powder X-ray diffraction, and Raman spectroscopic techniques. To remove metallic residues in CMOFs, HF treatment was performed. Powder X-ray diffraction analysis showed that only Ni, but not Fe, Cr and Cu, could be completely removed from CMOFs after HF treatment. Raman spectroscopic data indicated that well-stacked graphene layers structures were present only in Fe and Ni-containing CMOFs. The electrical conductivity, powder X-ray diffraction, and Raman data were correlated. The effect of acid treatment on the structure of CMOFs and the performance of CMOFs as electrode materials were evaluated.