N,N-dibutyldiglycol amic acid(HLI) and N,N-dioctyldiglycol amic acid(HLII) were synthesized and characterized by conventional spectroscopic methods. These molecules were examined as extractants for extraction-separation of La(III), Eu(III) and Er(III), as representative ions of light, middle and heavy rare earths, from aqueous chloride solutions. The analysis of the extraction equilibria revealed that the extracted species of lanthanum and europium ions by both of the extractants had a 1:3 metal to ligand ratio. It was suggested that erbium ions were extracted into the organic phase via the formation of Er(LI or II)2Cl complexes. The effect of the organic diluents on the extraction-separation efficiency of the studied rare earths by HLI and HLII was investigated by comparing the results obtained in dichloromethane and carbon tetrachloride. Regardless to the diluent used, the order of selectivity presented by the investigated extractants was Er(III)>Eu(III)>La(III). It is noteworthy that, a significant enhancement in separation of the studied rare earths by the extractants was achieved in their competitive extraction experiments with respect to that obtained in single component extraction experiments. Applicability of the extractants for the removal of rare earth ions from spent Ni-MH batteries was tested by removal of La(III), Eu(III) and Er(III) ions from simulated leach solution of such batteries. N, N-dibutyldiglycol amic acid (HLI) and N, N-dioctyldiglycol amic acid (HLII) were synthesized and characterized by conventional spectroscopic methods. These molecules were examined as extractants for extraction- separation of La (III) and analysis of the extraction equilibria revealed that the extracted species of lanthanum and europium ions by both of the extractants had a 1: 3 metal to ligand ratio. It was suggested that erbium ions were extracted into the organic phase via the formation of Er (LI or II) 2Cl complexes. The effect of the organic diluents on the extraction-separation efficiency of the studied rare earths by HLI and HLII was investigated by comparing the results obtained in dichloromethane and carbon tetrachloride. Regardless to the diluent used, the order of results by the investigated extractants was Er (III)> Eu (III)> La (III). It is noteworthy tha t, a significant enhancement in separation of the studied rare earths by the extractants been achieved in respect to the competitive extraction experiments with respect to that obtained in single component extraction experiments. Applicability of the extractants for the removal of rare earth ions from spent Ni-MH batteries was tested by removal of La (III), Eu (III) and Er (III) ions from simulated leach solution of such batteries.