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Alkylphenol polyethoxylates (APEOs) are nonionic surfactants whose degradation metabolites have become ubiquitous in the aquatic environment. The environmental significance of APEO metabolites and the threat they pose to wildlife is still a matter of debate. Even though advanced analytical procedures are available, researchers have been unable to obtain a complete mass balance during biodegradation studies. The ultimate fate of APEOs and their metabolites is not adequately understood. Biodegradation is believed to be the dominant attenuation process, but photodegradation may also play an important part. The synthesis of single isomer standards for APEOs and their metabolites is necessary for accurate quantification, estrogenicity experiments, and biological and chemical fate studies.