A series of sample stability tests has been undertaken to support a large UK-based survey of trace substances in wastewater. This program aims to quantify the input of priority chemicals to the aquatic environment via sewage effluent. The stability tests have demonstrated that, in most cases, the proposed approach of chilling samples meets the target that sample concentrations should not change by more than 25%, provided samples are analyzed or otherwise stabilized within 3–5 d. Substances tested fall into three main classes: Instability in effluents greater than the project-based threshold of 25% over 3–5 d can be ruled out provided samples are chilled for: DEHP (DEHA), glyphosate, AMPA, bentazone, mecoprop, ofloxacin, erythromycin, and ibuprofen; Some indication of possible instability up to 25% provided chilled storage periods do not extend beyond 3–5 d for: mercury (note requires acid dichromate preservation on site or as soon as possible), tributyltin, bisphenol A, reactive aluminum (in effluents, note requires filtration on sampling), oxytetracycline, and propranolol; and Clear stability problems are demonstrated for salicylic acid (effluents and influents), with indications of important instability (>25%) for bisphenol (effluents) AMPA and glyphosate (influents).