Nickel and magnesium hydrotalcite-like compounds (NiAlHT, MgAlHT) were investigated to remove fluoride ions from aqueous solutions in batch system. F- ions were determined in the remaining solutions using a fluoride ion selective electrode. Kinetic of the fluoride sorption from aqueous solutions by nickel hydrotalcite-like compound with different grain size were determined as well as the effects of Cl-. SO42- and As(V) on the sorption kinetic. It was found that the adsorption rate is the highest using grains samples of 25-50 mesh and in about 600 min the equilibrium was reached in all systems; the results were best fitted to the Elovich rate model equation which indicates that the sorption mechanism is trough a chemisorption process. Other anions interfere on the F- adsorption from bicomponenr aqueous solution by NiAlHT and MgAlHT. NiAIHT is more efficient than MgAlHT to remove fluoride from the aqueous solutions. (C) 2011 Elsevier B.V. All rights reserved.