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Analysis of Perfluorinated Chemicals and Their Fluorinated Precursors in Sludge: Method Development and Initial Results
Citation:
Yoo, H., J. J. ELLINGTON, J. W. WASHINGTON, T. JENKINS, AND L. LIBELO. Analysis of Perfluorinated Chemicals and Their Fluorinated Precursors in Sludge: Method Development and Initial Results. Presented at 238th ACS National Meeting & Exposition, Washington, DC, August 16 - 20, 2009.
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Description:
A rigorous method was developed to maximize the extraction efficacy for perfluorocarboxylic acids (PFCAs), perfluorosulfonates (PFSAs), fluorotelomer alcohols (FTOHs), fluorotelomer acrylates (FTAc), perfluorosulfonamides (FOSAs), and perfluorosulfonamidoethanols (FOSEs) from wastewater-treatment sludge. PFCAs and PFSAs in test sludge were analyzed by LC/MS/MS. Of five solvents tested for their PFCAs/PFSAs extraction effectiveness, 50%/50% (v/v) ACN/MeOH extraction yielded the highest concentrations. Pretreatment of sludge with NaOH and HCl, prior to extraction, recovered additional PFCAs/PFSAs (e.g., PFOA and PFOS), but KOH and K2S2O8 digestion were less effective than no pretreatment. Volatile fluorochemicals in sludge were extracted with methyl tert-butyl ether (MTBE) using GC-MS. NaOH-treated sludge resulted in recovery of more FTOHs, especially 8:2 FTOH. Presently we are investigating if this observation comes from the OH--facilitated hydrolysis of FTAc. With these efforts, we have been able to measure at least ten volatile fluorochemicals from test sludge at the concentrations of sub-ng to tens ng/g (ww). The identification of a few suspected volatile fluorochemicals, for which no standards exist, was evaluated with a derivitization technique.