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Powder X-ray diffraction and the Rietveld method have been exploited to determine quantitatively the mass fraction and the mean size evolution with aging time of the δ′ precipitates in an Al–Li alloy at 453 K. Although obtaining good refinements is not straightforward, the principal difficulties being the texture of the sample, the small intensities of the δ′ peaks, the coincidence of the most intensive δ′ peaks with α peaks, and the determination of several parameters (crystallographic structure, linear absorption, texture, temperature factors) before Rietveld application in order to avoid too many free parameters, this technique has proved to be a very powerful tool in applications in physical metallurgy.