The electrochemical dissolution of super alloys containing different amounts of rhenium was investigated. The initial part of the investigation focused on the anodic dissolution of rhenium from second-generation (3% Re) and third-generation (6% Re) nickel based alloys. Exploratory electrochemical tests were conducted to evaluate solution chemistries and to establish fundamental dissolution behavior of the alloys. These included rotating disc electrode (RDE) cyclic voltammetry, linear sweep voltammetry, and chronoamperometry tests. Electrolytes comprising sulfuric acid, hydrochloric acid, and ammonium sulfate were examined. Of these, a 0.1 M HCl solution proved to be extremely effective for electrochemical dissolution of samples of CMSX-4, CMSX-10, and SC-180 alloys. This paper discusses in detail the electrochemical behavior of these alloys.