A biosorbent material based on tilapia scales for the removal of Cu(II) ions was investigated. Modifications in the biosorbent caused by retention of Cu(II) and by the pH effect were evaluated separately in order to comprehend how the removal process occurs. For that, a physico-chemical characterization of the scales was performed before and after the Cu(II) removal. The results obtained from the characterization and biosorption tests led to the conclusion that the Ca–Cu ions exchange was responsible for purifying the solution. Furthermore, the tilapia scales were efficient, removing 95% of Cu(II) with 1 g of adsorbent (surface area ≈ 3 m2).