The metastable b -hardening phase in aged 6xxx-series Al alloys has been investigated by threedimensional atom-probe in order to evaluate the composition (Mg 5 Si 6 ) of the structure, previously determined by high-resolution transmission electron microscopy (HRTEM) and electron diffraction. For b , a significant number of Mg and Si atoms are found to be lost during detection in atom-probe analysis. The reason of this is non-resolved events, in which the correlation between the time-of-flight (TOF) and the detected position of the field-evaporated ion is lost. The problem is attributed to uneven evaporation and can be avoided by the use of an advanced delay-line detector (ADLD), which is capable of discriminating extremely closely spaced detection events. Preliminary analysis of a b -particle using this detector gave a Mg/Si ratio of 0.9 and a composition of 15 at.% Al. The Al level is significantly lower than those previously measured by other atom-probe detectors, because of the higher efficiency of the ADLD in detecting Mg and Si in particles. Atom-probe analysis with the ADLD detector is consistent with the b Mg/Si ratio derived from electron microscopy analysis. The measurements indicate that Al atoms may substitute both Si and Mg positions.