Calcined layered double hydroxides (LDHs) can be used to remove Sb(V), in the Sb(OH)(6)(-) form, from aqueous solutions. Sorption batch experiments showed that the mixed MgAlFe oxides, obtained from calcined hydrotalcite-like compound (3HT-cal), removed Sb(OH)(6)(-) through the formation of a non-LDH brandholzite-like compound, whereas the mixed ZnAl oxides, resulting from calcined zaccagnaite-like compound (2ZC-cal), trapped Sb(OH)(6)(-) in the interlayer during the formation of a Sb(V)-bearing LDH (the zincalstibite-like compound). The competition effect of coexistent anions on Sb(OH)(6)(-) removal was HAsO42- >> HCO3- >= SO42- for 2ZC-cal and HAsO42- >> HCO3- >> SO42- for 3HT-cal. Considering the importance of assessing the practical use of calcined LDHs, batch experiments were also carried out with a slag drainage affected by serious Sb(V) pollution (Sb = 9900 mu g/L) sampled at the abandoned Su Suergiu mine (Sardinia, Italy). Results showed that, due to the complex chemical composition of the slag drainage, dissolved Sb(OH)(6)(-) was removed by intercalation in the interlayer of carbonate LDHs rather than through the formation of brandholzite-like or zincalstibite-like compounds. Both 2ZC-cal and 3HT-cal efficiently removed very high percentages (up to 90-99%) of Sb(V) from the Su Suergiu mine drainage, and thus can have a potential application for real polluted waters.