This work involve a systematic treatability study of the treatment of acid tars (AT), a waste generated during the processing of petroleum and petrochemical, by stabilization/solidification with Portland cement (CEM I), with the addition of high carbon fly ash (HCFA), an industrial by-product, as a novel sorbent for organic contaminants. A factorial design experiment was adopted to investigate the effects of organic content, HCFA:AT ratio, percentage CEM I addition, and curing time on response variables including unconfined compressive strength (UCS), hydraulic conductivity, porosity, and leachability-related properties of the stabilized/solidified (s/s) products, and to assess management options for the s/s products based on performance criteria adapted from regulatory and other guidance. Results show that all studied factors had significant effects on the tested properties of the s/s products. Acid tar reduced UCS, but strength increase was observed with increased curing time. Increased HCFA addition led to an improvement in hydraulic conductivity. Assessment of management options indicates that the treated acid tars could find application as controlled low-strength materials, landfill liner, and landfill daily cover. The work demonstrates how a systematic treatability study can be used to develop a S/S operating window for management of a particular waste type.