There are potentially many thousands of municipally derived contaminants of emerging concern (CECs) present in discharged wastewaters that may cause adverse effects in receiving aquatic environments. Wastewater authorities, therefore, may face the momentous task of investigating these compounds with little or no prior CEC data for their sewage treatment plants (STPs). Such is the case for the Cleveland Bay Sewage Treatment Plant (CBSTP). To evaluate the potential environmental risk posed by municipal CECs, it is first necessary to understand which CECs are present in discharging wastewater, how they will be sampled and quantified, and which CECs are the most concerning regarding ecological risk. A Sampling Analysis and Quality Plan (SAQP) is a valuable tool that can be used to critically review and detail the strategy that will be adopted to achieve these outcomes. As such, this paper describes the development of a SAQP for screening wastewaters released from the CBSTP into Cleveland Bay as part of a preliminary CEC assessment. This paper describes the qualitative decision-making process employed to shortlist CECs into those perceived to pose the greatest ecological risk. In addition, the rationale and methods adopted to determine sampling locations and frequency are described.