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The surface area of electrodeposited thin films of Ni, Co, and NiCo was evaluated using electrochemical double-layer capacitance, electrochemical area measurements using the [Ru(NH3)6]3+/[Ru(NH3)6]2+ redox couple, and topographic atomic force microscopy (AFM) imaging. These three methods were compared to each other for each composition separately and for the entire set of samples regardless of composition. Double-layer capacitance measurements were found to be positively correlated to the roughness factors determined by AFM topography. Electrochemical area measurements were found to be less correlated with measured roughness factors as well as applicable only to two of the three compositions studied. The results indicate that in situ double-layer capacitance measurements are a practical, versatile technique for estimating the accessible surface area of a metal sample.