The mechanism of gold dissolution in acidic thiourea (Tu) solutions was investigated using cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and linear sweep voltammetry (LSV). CV over the potential range of -0.3 to 0.75 V vs. SCE shows peaks for the Tu/FDS (formamidine disulfide) and Au/Au(Tu)(2)(4) redox reactions. An oxidation peak associated with gold dissolution occurs at phi >= 0.36 V vs. SCE. This peak is often not observed in the first scan and its presence and magnitude are sensitive to the positive sweep potential limit of the first scan. FDS addition to the solution or adsorbed on the electrode has a strong catalytic effect and makes gold dissolution peak shift to lower potential during the first scan. This catalytic effect is identical to that exerted by scanning to higher potential. Tu/FDS ratio has a significant effect on thiourea stability, and it should be about 10:1 for the minimum thiourea decomposition and maximum gold dissolution rate. EIS results at 0.5-0.7 V vs. SCE with only Tu initially present in solution reveal a high-frequency capacitive loop associated with double layer charging, a medium-frequency inductive loop associated with FDS adsorption, and a low-frequency capacitive loop related to Tu oxidation. It appears that FDS adsorption on the gold surface activates the dissolution of gold and inhibits the oxidation of Tu. (C) 2010 Elsevier Ltd. All rights reserved.