EPA: 8327: Per-and Polyfluoroalkyl Substances (PFAS) in water using LC/MS/MS

Summary
Analytes
Revision
Data and Sites

Official Method Name

US EPA SW-846 Validated Method 8327: Per- and Polyfluoroalkyl Substances (PFAS) Using External Standard Calibration and Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)

Current Revision

Rev. 0, 2021

Media

WATER

Instrumentation

Liquid Chromatography with Tandem Mass Spectrometry

Method Subcategory

Organic

Method Source

EPA

Citation

SW-846 Update VII Announcements

Brief Method Summary

EPA has validated SW-846 Method 8327: Per- and Polyfluoroalkyl Substances (PFAS) Using External Standard Calibration and Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS) in a two-phase study for 24 PFAS analytes and 19 isotopically-labeled PFAS surrogates in four aqueous matrices of reagent water, surface water, groundwater, and wastewater effluent, three of which were intended to represent non-potable water matrices. The PFAS targets included sulfonic acids (e.g., PFOS), carboxylic acids (e.g., PFOA), fluorotelomer sulfonic acids (e.g., 6:2 fluorotelomer sulfonate, or FTS), and sulfonamides and sulfonamidoacetic acids (e.g., N-MeFOSAA).

Scope and Application

This method covers the analysis of selected per- and polyfluoroalkyl substances (PFAS) in prepared extracts of various matrices (e.g., waters and solids) by liquid chromatography/tandem mass spectrometry (LC/MS/MS) analysis.

Applicable Concentration Range

A minimum of five different calibration standard concentrations is required for a linear (first order) calibration model, and a minimum of six concentrations is required for a quadratic (second-order) model.

Interferences

Refer to Methods 3500, 3600 and 8000 for discussions of interferences. Matrix interferences can be caused by contaminants from the sample, sampling devices, or storage containers. The extent of matrix interferences will vary considerably from sample source to sample source, depending upon variations of the sample matrix.

Quality Control Requirements

Reagent blank (RB), Lower limit of quantitation (LLOQ) verification, Initial calibration verification (ICV), Continuing Calibration Verification (CCV), Initial Calibration Acceptance Criteria (ICAL) standards, Matrix blank (MB), Matrix spike (MS, Matrix spike duplicate (MSD), sample duplicates, surrogates, Laboratory control sample (LCS), Laboratory control sample duplicate (LCSD).

Sample Handling

Aqueous field samples and associated QC samples must be collected in separate polypropylene containers, including field blanks, MS/MSDs, and duplicates. All samples are iced or refrigerated at ≤6 °C from the time of collection until sample analysis. In the laboratory, samples and sample extracts should be stored in the refrigerator at ≤6 °C while not being analyzed. A 14-day limit from sample collection to preparation and a 30-day limit from preparation to analysis may be used as a guide until a more formal study is completed.

Maximum Holding Time

14-day limit from sample collection to preparation and a 30-day limit from preparation to analysis.

Relative Cost

Sample Preparation Methods

Method 3512 - Solvent dilution of non-potable waters

This method has 23 analytes associated with it.

Analyte	Detection Level	Bias	Precision	Spiking Level
1H,1H, 2H, 2H-Perfluorodecane sulfonic acid(39108-34-4) 1H,1H, 2H, 2H-Perfluorodecane sulfonic acid 8:2FTS	15.000 ng/L	105% Rec (ML)	9.60 % RSD (ML)	60.00 ng/L
1H,1H, 2H, 2H-Perfluorohexane sulfonic acid(757124-72-4) 1H,1H, 2H, 2H-Perfluorohexane sulfonic acid 4:2FTS	10.000 ng/L	99% Rec (ML)	6.50 % RSD (ML)	60.00 ng/L
N-ethyl perfluorooctanesulfonamidoacetic acid(2991-50-6) Glycine, N-ethyl-N-[(1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluorooctyl)sulfonyl]- N-ethyl perfluorooctanesulfonamidoacetic acid N-ethyl perfluorooctanesulfonamidoacetic acid NEtFOSAA NEtFOSAA	15.000 ng/L	97% Rec (ML)	17.20 % RSD (ML)	60.00 ng/L
N-methyl perfluorooctanesulfonamidoacetic acid(2355-31-9) Glycine, N-[(1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluorooctyl)sulfonyl]-N-methyl- N-methyl perfluorooctanesulfonamidoacetic acid N-methyl perfluorooctanesulfonamidoacetic acid NMeFOSAA NMeFOSAA	15.000 ng/L	99% Rec (ML)	10.50 % RSD (ML)	60.00 ng/L
Perfluoro-1-decanesulfonic acid(335-77-3) 1-Decanesulfonic acid, 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heneicosafluoro- PFDS Perfluoro-1-decanesulfonic acid	10.000 ng/L	98% Rec (ML)	14.60 % RSD (ML)	60.00 ng/L
Perfluoro-1-nonanesulfonic acid(68259-12-1) 1-Nonanesulfonic acid, 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,9-nonadecafluoro- PFNS Perfluoro-1-nonanesulfonic acid	10.000 ng/L	102% Rec (ML)	14.90 % RSD (ML)	60.00 ng/L
Perfluoro-1-octanesulfonamide(754-91-6) 1-Octanesulfonamide, 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluoro- PFOSA Perfluoro-1-octanesulfonamide	10.000 ng/L	88% Rec (ML)	8.40 % RSD (ML)	60.00 ng/L
Perfluorobutanesulfonic acid(375-73-5) 1,1,2,2,3,3,4,4,4-Nonafluoro-1-butanesulfonic acid PFBS Perfluorobutanesulfonic acid	10.000 ng/L	93% Rec (ML)	4.90 % RSD (ML)	60.00 ng/L
Perfluorobutanoic acid(375-22-4) PFBA Perfluorobutanoic acid	10.000 ng/L	93% Rec (ML)	19.60 % RSD (ML)	60.00 ng/L
Perfluorodecanoic acid(335-76-2) PFDA Perfluorodecanoic acid	10.000 ng/L	102% Rec (ML)	14.40 % RSD (ML)	60.00 ng/L
Perfluorododecanoic acid(307-55-1) PFDoA Perfluorododecanoic acid Perfluorolauric acid	10.000 ng/L	96% Rec (ML)	17.90 % RSD (ML)	60.00 ng/L
Perfluoroheptanesulfonic acid(375-92-8) PFHpS Perfluoroheptanesulfonic acid	10.000 ng/L	101% Rec (ML)	9.50 % RSD (ML)	60.00 ng/L
Perfluoroheptanoic acid(375-85-9) PFHpA Perfluoroheptanoic acid	10.000 ng/L	99% Rec (ML)	10.70 % RSD (ML)	60.00 ng/L
Perfluorohexanesulfonic acid(355-46-4) 1,1,2,2,3,3,4,4,5,5,6,6,6-Tridecafluorohexane-1-sulfonic acid PFHxS Perfluorohexanesulfonic acid	10.000 ng/L	95% Rec (ML)	12.90 % RSD (ML)	60.00 ng/L
Perfluorohexanoic acid(307-24-4) PFHxA Perfluorohexanoic acid Undecafluoro-1-hexanoic acid	10.000 ng/L	97% Rec (ML)	8.20 % RSD (ML)	60.00 ng/L
Perfluorononanoic acid(375-95-1) PFNA Perfluorononanoic acid	10.000 ng/L	97% Rec (ML)	8.90 % RSD (ML)	60.00 ng/L
Perfluorooctanesulfonic acid(1763-23-1) 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-Heptadecafluoro-1-octanesulfonic acid PFOS Perfluorooctane sulfonate Perfluorooctanesulfonic acid	10.000 ng/L	100% Rec (ML)	14.00 % RSD (ML)	60.00 ng/L
Perfluorooctanoic acid(335-67-1) Hexanoyl fluoride, 3,3,4,4,5,5,6,6,6-nonafluoro-2-oxo- PFOA Perfluoroheptanecarboxylic acid Perfluorooctanoic acid	10.000 ng/L	100% Rec (ML)	9.70 % RSD (ML)	60.00 ng/L
Perfluoropentanesulfonic acid(2706-91-4) PFPeS Perfluoropentanesulfonic acid	10.000 ng/L	97% Rec (ML)	6.20 % RSD (ML)	60.00 ng/L
Perfluoropentanoic acid(2706-90-3) PFPeA Perfluoropentanoic acid	10.000 ng/L	104% Rec (ML)	13.70 % RSD (ML)	60.00 ng/L
Perfluorotetradecanoic acid(376-06-7) PFTA Perfluoromyristic acid Perfluorotetradecanoic acid	10.000 ng/L	96% Rec (ML)	22.60 % RSD (ML)	60.00 ng/L
Perfluorotridecanoic acid(72629-94-8) PFTrDA Perfluorotridecanoic acid	15.000 ng/L	98% Rec (ML)	19.30 % RSD (ML)	60.00 ng/L
Perfluoroundecanoic acid(2058-94-8) PFUnA Perfluoroundecanoic acid	10.000 ng/L	99% Rec (ML)	14.70 % RSD (ML)	60.00 ng/L

Precision Descriptor Notes:	Recovery and precision were determined at two concentrations (60 and 200 ng/L) in four matrices (reagent water, groundwater, surface water, and waste water) in a multi-laboratory setting. Pooled mean percent recovery was determined on 40 samples, including 5 replicates of each matrix and spike level tested by each of 8 laboratories except for 60 ng/L wastewater where 39 samples were analyzed. Within-laboratory standard deviation of percent recovery and between-laboratory standard deviation of percent recovery were determined from results from 8 laboratories. All calculations can be found in the following publication: “Protocol for Review and Validation of New Methods for Regulated Organic and Inorganic Analytes in Wastewater Under EPA’s Alternate Test Procedure Program, February 2018”, available at: https://www.epa.gov/sites/production/files/2018-03/documents/chemical-new-method-protocol_feb-2018.pdf .
Detection Level Note:	General guidance for verifying LLOQs is provided in this section and in Method 8000. The LLOQ must be ≥ the lowest point in the calibration curve. The laboratory shall establish LLOQs at concentrations where both quantitative and qualitative requirements can consistently be met. Verification of LLOQs using spiked clean control material represents a best-case scenario because it does not evaluate the potential matrix effects of real-world samples. For application of LLOQs on a project-specific basis, with established DQOs, a representative matrix-specific LLOQ verification may provide a more reliable estimate of the lower quantitation limit capabilities. LLOQ verifications are prepared by spiking a clean control material with the analyte(s) of interest at 0.5 - 2 times the LLOQ concentration level(s). Alternatively, a representative sample matrix free of targets may be spiked with the analytes of interest at 0.5 - 2 times the established or anticipated LLOQ. LLOQ verifications are carried through the same preparation and analytical procedures as environmental samples and other QC samples. Recovery of target analytes in the LLOQ verification should be within established in-house limits or within other such project-specific acceptance limits to demonstrate acceptable method performance at the LLOQ. Preliminary acceptance criteria for the LLOQ verification are 50-150%. This practice acknowledges the potential for greater uncertainty at the low end of the calibration curve. Statistically based LLOQ verification acceptance criteria should be determined once sufficient data points have been acquired.

Precision Descriptor Notes:

Recovery and precision were determined at two concentrations (60 and 200 ng/L) in four matrices (reagent water, groundwater, surface water, and waste water) in a multi-laboratory setting. Pooled mean percent recovery was determined on 40 samples, including 5 replicates of each matrix and spike level tested by each of 8 laboratories except for 60 ng/L wastewater where 39 samples were analyzed. Within-laboratory standard deviation of percent recovery and between-laboratory standard deviation of percent recovery were determined from results from 8 laboratories. All calculations can be found in the following publication: “Protocol for Review and Validation of New Methods for Regulated Organic and Inorganic Analytes in Wastewater Under EPA’s Alternate Test Procedure Program, February 2018”, available at: https://www.epa.gov/sites/production/files/2018-03/documents/chemical-new-method-protocol_feb-2018.pdf .

Detection Level Note:

General guidance for verifying LLOQs is provided in this section and in Method 8000. The LLOQ must be ≥ the lowest point in the calibration curve. The laboratory shall establish LLOQs at concentrations where both quantitative and qualitative requirements can consistently be met. Verification of LLOQs using spiked clean control material represents a best-case scenario because it does not evaluate the potential matrix effects of real-world samples. For application of LLOQs on a project-specific basis, with established DQOs, a representative matrix-specific LLOQ verification may provide a more reliable estimate of the lower quantitation limit capabilities. LLOQ verifications are prepared by spiking a clean control material with the analyte(s) of interest at 0.5 - 2 times the LLOQ concentration level(s). Alternatively, a representative sample matrix free of targets may be spiked with the analytes of interest at 0.5 - 2 times the established or anticipated LLOQ. LLOQ verifications are carried through the same preparation and analytical procedures as environmental samples and other QC samples. Recovery of target analytes in the LLOQ verification should be within established in-house limits or within other such project-specific acceptance limits to demonstrate acceptable method performance at the LLOQ. Preliminary acceptance criteria for the LLOQ verification are 50-150%. This practice acknowledges the potential for greater uncertainty at the low end of the calibration curve. Statistically based LLOQ verification acceptance criteria should be determined once sufficient data points have been acquired.

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Rev. 0, 2021

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EPA: 8327: Per-and Polyfluoroalkyl Substances (PFAS) in water using LC/MS/MS

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