A hierarchical procedure is developed to determine maximum overall yield of a process and optimize process changes to achieve such a yield. First, a targeting procedure is developed to identify an upper bound of the overall yield ahead of detailed design. Several mass integration strategies are proposed to attain maximum yield. These strategies include rerouting of raw materials, optimization of reaction yield, rerouting of product from undesirable outlets to desirable outlets, and recycling of unreacted raw materials. Path equations are tailored to provide the appropriate level of detail for modeling process performance as a function of the optimization variables pertaining to design and operating variables. Interval analysis is used as an inclusion technique that provides rigorous bounds regardless of the process nonlinearities and without enumeration. Then, a new approach for identification of cost-effective implementation of maximum attainable targets for yield is presented. In this approach, a mathematical program was developed to identify the maximum feasible yield using a combination of iterative additions of constraints and problem reformulation. Next, cost objectives were employed to identify a cost-effective solution with the details of design and operating variables. Constraint convexification was used to improve the quality of the solution towards globability. A trade-off procedure between the saving and expenses for yield maximization problem is presented. The proposed procedure is systematic, rigorous, and computationally efficient. A case study was solved to demonstrate the applicability and usefulness of the developed procedure.