The application of organic acids towards the extraction of both Cu and Cr from the Cu-Cr spent catalyst was investigated. A series of organic acid such as acetic acid, citric acid, formic acid, ascorbic acid and tartaric acid were adopted, and after screening, acetic acid showed a profound effect on dissolution of either of the metals over other green reagents. The spent catalyst was characterized by XRD and SEM-EDAX to confirm the existence of the oxide phase due to both Cu and Cr metals. For efficient dissolution of metals, the critical parameters such as agitation speed, acetic acid concentration, temperature, particle size, as well as S/L ratio affecting on it was systematically investigated. It was observed that at approximately 99.99% of Cu along with 62% of Cr was extracted at the optimised conditions (agitation speed: 800rpm, 1.0M CH3COOH, 353K temperature, particle size of (75-105) µm and S/L: 2% (W/V). The leach residue obtained after the first stage of leaching was analysed by SEM-EDAX and XRD, indicating no peaks due to the presence of Cu ensures complete dissolution of Cu at the optimum conditions. Further, to attain the quantitative leaching yield of Cr, the leach residue obtained after the first stage was sequentially investigated using varied acetic acid concentration and temperature. Leaching kinetics was established based on obtained results at the varied operating parameters, and it revealed support for fitting a model of the leaching data to the shrinking core chemical control model (R2 = 0.99) for both metals (Cu and Cr). The activation energy determined to be 34.05kJmol-1 and 43.31kJmol-1 for Cu and Cr, respectively, validates the proposed leaching kinetics mechanism.