The analysis of per/polyfluoroalkyl substances (PFASs) or perfluorinated compounds (PFCs), in particular the perfluorinated alkyl acids (PFAAs), is currently a hot topic in water analysis. The unique chemical properties of these compounds make them components used in a variety of applications such as nonstick cookware, fire resistant clothing, fire-fighting foams, and others. However, these compounds are considered toxic, persistent, and bioaccumulative in wildlife and the environment. Consequently, the United States Environmental Protection Agency (USEPA) has recently issued drinking water health advisories for two PFASs, perfluorooctanoic acid (PFOA) and perfluorosulfonic acid (PFOS) at 70 ng/L (combined). Several states such as New Jersey, New York, and North Carolina already have public health guideline values varying from 20–400 ng/L for several PFAS including PFOA, PFOS, perfluorohexanoic acid (PFHxA), and perfluorononanoic acid (PFNA) in water.