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This paper deals with the electrochemical properties of three iso-structural compounds of general formula [SiW$_{10}$ O$_{36}$(M$_{2}$O$_{2}$E$_{2}$)]$^{6-}$ (M $=$ Mo or W; E $=$ S or O). A first part is focused on their electrochemical behaviors in aqueous medium. A second part concerns the electrocatalytic properties of these compounds in aqueous medium and the preparation of modified glassy carbon electrodes through a layer-by-layer methodology. This method allowed preparing a multilayer system, which was applied to the electroanalysis of iodate anions in aqueous medium with a limit detection of $6.2~\mu \mbox {M}$.