EPA-ORD / EPA-OST: 537: Organic contaminants in drinking water by direct aqueous injection-liquid chromatography/tandem mass spectrometry

Summary
Analytes
Revision
Data and Sites

Official Method Name

Determination of Selected Perfluorinated Alkyl Acids in Drinking Water by Solid Phase Extraction and Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)

Current Revision

Version 1.1, September 2009

Media

WATER

Instrumentation

Liquid Chromatography-Mass Spectrometery (also High Performance LC-MS; HPLC-MS)

Method Subcategory

Organic

Method Source

EPA-ORD / EPA-OST

Citation

1997 Edition of the Hach Water Analysis Handbook

Brief Method Summary

A 250-mL water sample is fortified with surrogates and passed through a solid phase extraction (SPE) cartridge containing polystyrenedivinylbenzene (SDVB) to extract the method analytes and surrogates. The compounds are eluted from the solid phase with a small amount of methanol. The extract is concentrated to dryness with nitrogen in a heated water bath, and then adjusted to a 1-mL volume with 96:4% (vol/vol) methanol:water after adding the IS(s). A 10-µL injection is made into an LC equipped with a C18 column that is interfaced to an MS/MS. The analytes are separated and identified by comparing the acquired mass spectra and retention times to reference spectra and retention times for calibration standards acquired under identical LC/MS/MS conditions. The concentration of each analyte is determined by using the internal standard technique. Surrogate analytes are added to all Field and QC Samples to monitor the extraction efficiency of the method analytes.

Scope and Application

This is a liquid chromatography/tandem mass spectrometry (LC/MS/MS) method for the determination of selected perfluorinated alkyl acids (PFAAs) in drinking water. The following analytes that this method may be used to determine are: N-ethyl perfluorooctanesulfonamidoacetic acid (NEtFOSAA), N-methyl perfluorooctanesulfonamidoacetic acid (NMeFOSAA), Perfluorobutanesulfonic acid (PFBS), Perfluorodecanoic acid (PFDA), Perfluorododecanoic acid (PFDoA), Perfluoroheptanoic acid (PFHpA), Perfluorohexanesulfonic acid (PFHxS), Perfluorohexanoic acid (PFHxA), Perfluorononanoic acid (PFNA), Perfluorooctanesulfonic acid (PFOS), Perfluorooctanoic acid (PFOA), Perfluorotetradecanoic acid (PFTA), Perfluorotridecanoic acid (PFTrDA), and Perfluoroundecanoic acid (PFUnA)

Applicable Concentration Range

Interferences

All glassware must be meticulously cleaned. Wash glassware with detergent and tap water, rinse with tap water, followed by a reagent water rinse. Non-volumetric glassware can be heated in a muffle furnace at 400 °C for 2 h or solvent rinsed. Volumetric glassware should be solvent rinsed and not be heated in an oven above 120 °C. Store clean glassware inverted or capped. Do not cover with aluminum foil because PFAAs can be potentially transferred from the aluminum foil to the glassware.

Quality Control Requirements

Detailed quality-control requirements are outlined in the method document, which include initial demonstration of capability, and ongoing QC requirements.

Sample Handling

Samples must be chilled during shipment and must not exceed 10^oC during the first 48 hours after collection. Samples stored in the lab must be held at or below 6^oC until analysis, but should not be frozen. lab must be held at or below 6^oC and protected from light until analysis. Samples should not be frozen.

Maximum Holding Time

Extract within 14 days of collection; extracts must be stored at room temperature and analyzed within 28 days after extraction.

Relative Cost

Unknown

Sample Preparation Methods

Collect with 250-mL polypropylene bottle and screw-cap. Add Trizma 5g/L. Follow guidelines.

This method has 14 analytes associated with it.

Analyte	Detection Level	Bias	Precision	Spiking Level
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	4.200 ng/L	113% Rec	5.50 % RSD	21.00 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	6.500 ng/L	109% Rec	9.30 % RSD	20.00 ng/L
Perfluorobutanesulfonic acid(375-73-5) 1,1,2,2,3,3,4,4,4-Nonafluoro-1-butanesulfonic acid PFBS Perfluorobutanesulfonic acid	3.100 ng/L	93% Rec	12.00 % RSD	9.10 ng/L
Perfluorodecanoic acid(335-76-2) PFDA Perfluorodecanoic acid	0.700 ng/L	114% Rec	4.10 % RSD	7.30 ng/L
Perfluorododecanoic acid(307-55-1) PFDoA Perfluorododecanoic acid Perfluorolauric acid	1.100 ng/L	116% Rec	4.60 % RSD	7.30 ng/L
Perfluoroheptanoic acid(375-85-9) PFHpA Perfluoroheptanoic acid	0.500 ng/L	111% Rec	6.20 % RSD	8.30 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	1.600 ng/L	108% Rec	9.30 % RSD	5.00 ng/L
Perfluorohexanoic acid(307-24-4) PFHxA Perfluorohexanoic acid Undecafluoro-1-hexanoic acid	2.000 ng/L	116% Rec	4.90 % RSD	11.00 ng/L
Perfluorononanoic acid(375-95-1) PFNA Perfluorononanoic acid	0.700 ng/L	121% Rec	7.50 % RSD	9.60 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	1.700 ng/L	110% Rec	6.50 % RSD	9.10 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	1.400 ng/L	116% Rec	4.10 % RSD	9.60 ng/L
Perfluorotetradecanoic acid(376-06-7) PFTA Perfluoromyristic acid Perfluorotetradecanoic acid	1.700 ng/L	117% Rec	2.40 % RSD	8.70 ng/L
Perfluorotridecanoic acid(72629-94-8) PFTrDA Perfluorotridecanoic acid	2.200 ng/L	118% Rec	11.00 % RSD	5.50 ng/L
Perfluoroundecanoic acid(2058-94-8) PFUnA Perfluoroundecanoic acid	2.800 ng/L	120% Rec	5.40 % RSD	11.00 ng/L

Precision Descriptor Notes:	See Section 17 for tables, diagrams, flow charts, and validation data.
Detection Level Note:	Determining the Detection Limit (DL) for analytes in this method is optional (Sect. 9.2.7). Detection limit is defined as the statistically calculated minimum concentration that can be measured with 99% confidence that the reported value is greater than zero. The DL is compound dependent and is dependent on sample preparation, sample matrix, fortification concentration, and instrument performance.

Precision Descriptor Notes:

See Section 17 for tables, diagrams, flow charts, and validation data.

Detection Level Note:

Determining the Detection Limit (DL) for analytes in this method is optional (Sect. 9.2.7). Detection limit is defined as the statistically calculated minimum concentration that can be measured with 99% confidence that the reported value is greater than zero. The DL is compound dependent and is dependent on sample preparation, sample matrix, fortification concentration, and instrument performance.

Revision	PDF/Link
Version 1.1, September 2009

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EPA-ORD / EPA-OST: 537: Organic contaminants in drinking water by direct aqueous injection-liquid chromatography/tandem mass spectrometry

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