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There has been a recent surge in the development of mass spectrometric methods for detailed characterization of naphthenic acid fraction compounds (all C_cH_hN_nO_oS_s, species, including heteroatomic and aromatic components in the acid‐extractable fraction) in environmental samples. This surge is driven by the increased activity in oil sands environmental monitoring programs in Canada, the exponential increase in research studies on the isolation and toxicity identification of components in oil sands process water (OSPW), and the analytical requirements for development of technologies for treatment of OSPW. There has been additional impetus due to the parallel studies to control corrosion from naphthenic acids during the mining and refining of heavy bitumen and crude oils. As a result, a range of new mass spectrometry tools have been introduced since our last major review of this topic in 2009. Of particular …