Cementation is an effective process that meets the requirements of process cleanliness. The performance of the cementation reaction is dictated by a number of variables. In this study, the effects of various parameters on the yields of copper-iron cementation (wire and powder) were investigated. Statistical full factorial designs were used to produce appropriate mixture models for the yields. The experimental designs were done at three different levels of three operating variables, namely initial concentration, temperature, and pH. The optimization studies were carried out with MATLAB 7.0 software. The optimum yields obtained from the predicted models were found to be 0.9916 and 0.9088 for iron wire and powder, respectively, under optimized conditions, and these were in accordance with the experimental observations.