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Analysis of Per- and Polyfluoroalkyl Substances (PFAS) in Aqueous, Solid, Biosolids, and Tissue Samples by LC-MS/MS
Citation:
Mills, M. Analysis of Per- and Polyfluoroalkyl Substances (PFAS) in Aqueous, Solid, Biosolids, and Tissue Samples by LC-MS/MS. US Environmental Protection Agency, Cincinnati, OH, 2022.
Impact/Purpose:
Method 1633 is for use in the Clean Water Act (CWA) for the determination of the per- and polyfluoroalkyl substances (PFAS) in Table 1 in aqueous, solid (soil, biosolids, sediment) and tissue samples by liquid chromatography/mass spectrometry (LC-MS/MS). The method calibrates and quantifies PFAS analytes using isotopically labeled standards. Where linear and branched isomers are present in the sample and either qualitative or quantitative standards containing branched and linear isomers are commercially available, the PFAS analyte is reported as a single analyte consisting of the sum of the linear and branched isomer concentrations. The instrumental portion of this method is for use only by analysts experienced with LC-MS/MS or under the close supervision of such qualified persons. Each laboratory that uses this method must demonstrate the ability to generate acceptable results using the procedure in Section 9.2. 1.4 By their very nature, many components of PFAS present analytical challenges unique to this class of analytes. For example, PFAS analytes readily adhere to the walls of the sample containers and may also stratify in the container. EPA has included procedures in the method that must be employed to address such challenges (see Section 11.0 and Appendices A and B). This method is “performance-based,” which means that modifications may be made without additional EPA review to improve performance (e.g., overcome interferences, or improve the sensitivity, accuracy, or precision of the results) provided that all performance criteria in this method are met. Requirements for establishing equivalency are in Section 9.1.2 and include 9.1.2.2c. For CWA uses, additional flexibility is described at 40 CFR 136.6. Changes in performance, sensitivity, selectivity, precision, recovery, etc., that result from modifications within the scope of 40 CFR Part 136.6, and Section 9.0 of this method must be documented, as well as how these modifications compare to the specifications in this method. Changes outside the scope of 40 CFR Part 136.6 and Section 9.0 of this method may require prior review or approval.
Description:
Method 1633 is for use in the Clean Water Act (CWA) for the determination of the per- and polyfluoroalkyl substances (PFAS) in Table 1 in aqueous, solid (soil, biosolids, sediment) and tissue samples by liquid chromatography/mass spectrometry (LC-MS/MS). 1.2 The method calibrates and quantifies PFAS analytes using isotopically labeled standards. Where linear and branched isomers are present in the sample and either qualitative or quantitative standards containing branched and linear isomers are commercially available, the PFAS analyte is reported as a single analyte consisting of the sum of the linear and branched isomer concentrations. 1.3 The instrumental portion of this method is for use only by analysts experienced with LC-MS/MS or under the close supervision of such qualified persons. Each laboratory that uses this method must demonstrate the ability to generate acceptable results using the procedure in Section 9.2. 1.4 By their very nature, many components of PFAS present analytical challenges unique to this class of analytes. For example, PFAS analytes readily adhere to the walls of the sample containers and may also stratify in the container. EPA has included procedures in the method that must be employed to address such challenges (see Section 11.0 and Appendices A and B). 1.5 This method is “performance-based,” which means that modifications may be made without additional EPA review to improve performance (e.g., overcome interferences, or improve the sensitivity, accuracy, or precision of the results) provided that all performance criteria in this method are met. Requirements for establishing equivalency are in Section 9.1.2 and include 9.1.2.2c. For CWA uses, additional flexibility is described at 40 CFR 136.6. Changes in performance, sensitivity, selectivity, precision, recovery, etc., that result from modifications within the scope of 40 CFR Part 136.6, and Section 9.0 of this method must be documented, as well as how these modifications compare to the specifications in this method. Changes outside the scope of 40 CFR Part 136.6 and Section 9.0 of this method may require prior review or approval.