Good analytical techniques for the separation and detection of reactive dyes are necessary not only to monitor residual liquors and effluents but also to aid in optimisation of dye synthesis, purification, formulation and application. HPLC, although generally widely employed, often has difficulty in analysing certain reactive dyes, especially the phthalocyanine-based dyes. CE analysis of several gifunctional reactive dyes has been carried out with subsequent activation and hydrolysis reactions for a bis-sulfatoethyl sulfone dye, under different pH and temperature conditions, being monitored. A variety of buffers were investigated; the use of acetonitrile in a micellar buffer system proving to be particularly successful.