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Developing methods to probe the nature and structure of nanoscale environments continues to be a challenge in nanoscience. We report a cyclic voltammetry investigation of internal, hydrogen-bond driven phase separation of amide-containing thiols and alkane thiols. Amide-containing thiols with a terminal ferrocene carboxylate functional group were investigated in two binary monolayers, one homogeneously mixed and the other phase separated. The electrochemical response of the ferrocene probe was used to monitor adsorbate coverage, environment and phase separation within each of these monolayers. The results demonstrate that the behavior of ferrocene containing monolayers can be used to probe nanoscale organization.

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