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A method based on the variation of the lattice parameter with Li content, for the quantitative determination of lithium in the system Lix+Ni1-2x2+Nix3+O2-, is proposed. A precision between 1 and 5% relative, depending upon the concentration range, has been obtained. The results are compared with those obtained by flame emission spectroscopy. For values of x > 0.12 the original rhombohedral lattice transforms into a face centred cubic lattice.