During homogenisation of AA 6xxx aluminium alloys, the platelike β-AlFeSi intermetallic phase will transform to a less Si-rich and more spheroidised α-Al(FeMn)Si phase which is more favourable for extrusion. In this study, several quantitative methods, which determine the relative volume fraction of α-Al(FeMn)Si and β-AlFeSi, are compared and an assessment of each method is made. The methods used are optical microscopy, scanning electron microscopy (SEM) in combination with electron dispersive X-ray (EDX) using polished samples, and X-ray diffraction (XRD) on intermetallics, extracted through selective dissolution of the Al matrix. The highest accuracy is obtained by using SEM/EDX analysis and applying two criteria.