Levels of vanadium, sulphur and bromine within the vanadopohores of Ascidia mentula vanadocytes have been determined by quantitative X‐ray microanalytical techniques. Values obtained for vanadophore vanadium in thin sections correspond to 2.5‐3.25% or 0.5‐0.65 molal aqueous solutions in vivo. Quantitation of sulphur in thin sections gives levels an order of magnitude lower than for vanadium, but it is likely that major losses of sulphur have occurred, since analysis of unfixed, air dried vanadocytes gives V/S atomic ratios close to unity. This 1: 1 ratio may have implications for the structure of the vanadium complex. Quantitation of bromine is less reliable, but levels of this halogen in vanadocytes are significant. The possibility that bromine, in the form of brominated metabolites, together with vanadium and acid, contribute to a multicomponent chemical defense role in ascidians is discussed.