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Chemically functional magnetic nanoparticles, comprised of an Fe core encased in a thin Au shell, have been prepared by sequential high temperature decomposition of organometallic compounds in a coordinating solvent. A novel approach to encapsulate the Fe core in Au has been developed. TEM analysis confirms that the nanoparticles are monodisperse (∼20%) with average diameters of 8nm. The nanoparticles were subsequently functionalized with alkanethiolate ligands, which prevent aggregation, enable solubility in a range of solvents (both hydrophobic and hydrophilic), and permit subsequent derivatization (e.g., via ligand exchange reactions). The functionalized particles are characterized using high-resolution transmission electron microscopy (HRTEM), X-ray powder diffraction (XRD) and ultraviolet-visible (UV-Vis) absorption spectroscopy.We have utilized place-exchange to impart chemical functionality to the nanoparticles by attaching either (1) thiol-derivatized redox moieties (e.g., ferrocene) or (2) alkanethiols with terminal reactive groups such as alcohols, amines and carboxylic acids. This paper presents our preliminary investigations of the voltammetry of the former class of these magnetic core/shell nanoparticles.