A performance optimization study has been conducted using a laboratory Jameson Flotation Cell, which resulted in the development of empirical models for four key response parameters, such as product ash content, product total sulfur content, combustible recovery and separation efficiency. The empirical models were utilized to identify an appropriate experimental region to achieve a target set of metallurgical performances from the treatment of a potation feed sample. The separation performance obtained from the treatment of three additional coal samples used in this investigation indicate that a high positive bias factor of about 0.6, which translates to a wash water ratio of 2.5, is required to produce superior quality coal especially from the treatment of high ash coals. The separation performance obtained using the same orifice-downcomer combination with various size separation chambers indicate that the diameter of the separation chamber of the Jameson Cell can be potentially reduced without affecting the separation performance. In other words, more number of downcomers can be used with the same size cell, which will significantly improve the throughput capacity of the Jameson flotation technology without sacrificing the separation performance.