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In situ synchrotron X-ray powder diffraction is a powerful tool for studying phase transformations in engineering alloys, which, when combined with Rietveld-based data analysis methods, allows the phase composition of an alloy to be quantified as a function of variables such as time or temperature.This approach has recently been used to gain new insights into phase transformations within the well known Al-Cu-Mg series of 2xxx alloys.In situ isothermal aging experiments have confirmed that the decomposition sequence in Al-Cu-Mg alloys involves a metastable variant of the S (Al2CuMg) phase, and enabled the kinetics of the transformation between metastable and equilibrium S phases to be investigated.