A rapid and reliable analytical procedure has been developed for the separation and analysis of dioxouranium, thorium, gold, and mercury by micellar electro-kinetic chromatography (MEKC) using bis(acetylacetone)ethylenediamine (H(2)AA(2)en) as complexing reagent. Under the optimized conditions (64 mM borate buffer containing 12.25 mM SDS and 13% acetonitrile, pH 8.0, 25 kV, 311 nm as detection wavelength) the ions were separated within 5.0 min. Linear dynamic ranges were 1-5, 8-42, 10-50, and 2-40 mu g mL(-1), respectively, for gold, mercury, thorium, and uranium and the respective detection limits were 0.66, 3.33, 1.6, and 3.3 mu g mL(-1). The applicability of method has been evaluated by application to uranium and thorium from ore samples.