A glassy carbon electrode (GCE) and a single-use pencil graphite electrode (PGE) modified through the incorporation of a mixed-ion, amphiphilic, fluorohectorite heterostructure, wherein the galleries are regularly interstratified by hydrophilic inorganic ions (Na+) and lipophilic onium ions, are shown to be efficient electrochemical sensors for the specific determination of the pollutant 2,4-dicholorophenol (2,4-DCP) when incorporated at the 2.5% (v/v) level into a sol-gel (triethoxysilane) matrix on the electrode surface. The voltammetric detection of 2,4-DCP resulted in low detection limits of 26.66 nM and 19.32 nM at the 2.5% (v/v) clay/sol-gel-modified GCE and PGE, respectively, based on a signal-to-noise ratio of 3. The reproducible data obtained from the single-use clay/sol-gel-modified PGE show promise for the microfabrication of a remote sensor specific for 2,4-DCP detection.