jats:titleAbstract</jats:title> jats:pThe ability to quantify accurately the formation of topologically close-packed phases in nickel-based superalloys is key to assessing their thermal stability and ensuring that their performances will not deteriorate during long-term exposure at high temperatures. To investigate the effectiveness of synchrotron XRD for the detection of such minority phases in Ni-based superalloys, the commercial polycrystalline alloy RR1000 was analyzed following exposures of varying times at 800 °C. Data were collected from both solid samples and extracted residues, and additional laboratory X-ray diffraction was performed on the residues. The minor phases were successfully detected in solid samples using synchrotron radiation, and a comparison of the results from these quantification methods shows that the extraction method gives results of the right order of magnitude to reflect the phase quantities that are present in the alloy. However, the results indicate that the synchrotron route is not a suitable method for the quantification of phases present in quantities less than approximately 0.3 wt pct.</jats:p>