Metal–organic frameworks (MOFs) are crystalline porous materials composed of metal nodes connected by organic ligands, forming highly ordered structures with exceptionally high surface area and tunable porosity. These properties make MOFs promising candidates for gas storage applications, particularly hydrogen and carbon dioxide. This research investigates the synthesis, characterisation, and gas-adsorption performance of selected MOFs prepared by solvothermal, microwave-assisted, and mechanochemical techniques. Structural analysis using X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, and BET surface area measurements confirmed the formation of highly porous frameworks. Gas adsorption experiments demonstrated hydrogen storage capacities up to 2.45 wt% and carbon dioxide uptake up to 4.85 mmol g⁻¹. Statistical analysis showed a strong correlation between the BET surface area and the adsorption capacity. Linear regression analysis yielded R² values of 0.997 for hydrogen and 0.999 for CO₂ adsorption. These findings highlight the potential of MOFs as efficient materials for clean energy storage and carbon capture technologies.