Cyclic voltammetric measurements were made using well-characterized microcrystalline boron-doped diamond thinfilm electrodes to test the material×s responsiveness for ferrocene as a function of scan rate, solvent, and electrolyte composition. Apparent heterogeneous electron transfer rate constants, k8 app , of 0.042 AE 0.015, 0.048 AE 0.015, and 0.008 AE 0.002 cm/s were observed in 0.1 M NaClO 4 /CH 3 CN, 0.1 M TBAClO 4 /CH 3 CN, and 0.1M TBAClO 4 /CH 2 Cl 2 , respectively. These rate constants, obtained using electrodes without any type of pretreatment, are similar to those observed for freshly polished glassy carbon. The results demonstrate that boron-doped diamond is a viable material for the electrochemical analysis of nonaqueous analytes.