The chloropropyl silica gel was modified with octa(3-aminopropyl)octasilsesquioxane and characterized by Fourier transform infrared (FTIR) spectroscopy, nuclear magnetic resonance (NMR), spectroscopies, and surface and area porosity. The specific sorption capacity of metallic ions (Cu2+and Ni2+) increases in the following solvent order: water<ethanol 42%<ethanol<ketone. The high values of the constant (K) in the order of 103 L mol−1suggested the high adsorbent capacity of the modified silica (SGAPC) for Cu2+and Ni2+. SGAPC was applied to a separation column and shows recoveries of around 100% of copper in samples of sugar cane spirit, vodka, ginger brandy, and ethanol fuel.