EPA-OW: 533: Select per- and polyfluoroalkyl substances (PFAS) in drinking water by SPE LC-MS/MS
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Official Method Name
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METHOD 533: DETERMINATION OF PER- AND POLYFLUOROALKYL SUBSTANCES IN DRINKING WATER BY ISOTOPE DILUTION ANION EXCHANGE SOLID PHASE EXTRACTION AND LIQUID CHROMATOGRAPHY/TANDEM MASS SPECTROMETRY |
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Current Revision
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Media
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WATER |
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Instrumentation
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Liquid Chromatography with Tandem Mass Spectrometry |
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Method Subcategory
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Organic |
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Method Source
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Citation
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Brief Method Summary
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This is a solid phase extraction (SPE) liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of select per- and polyfluoroalkyl substances (PFAS) in drinking water. Method 533 requires the use of MS/MS in Multiple Reaction Monitoring (MRM) mode to enhance selectivity. Accuracy and precision data have been generated in reagent water and drinking water for the compounds included in the Analyte List.
This method is intended for use by analysts skilled in the performance of solid phase extractions, the operation of LC-MS/MS instrumentation, and the interpretation of the associated data. |
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Scope and Application
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This is a method for the determination of select per- and polyfluoroalkyl substances (PFAS) in drinking water. |
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Applicable Concentration Range
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Prepare a series of calibration standards of at least five levels. The lowest calibration standard must be at or below the MRL for each analyte. The analyte calibration ranged from approximately 0.50 ng/mL to 25 ng/mL extract concentration. |
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Interferences
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Sources of interferents include labware, reagents, equipment, and supplies including the SPE cartridges. Matrix interferences may include contaminants that are co-extracted from the sample, inorganic salt concentrations up to 250 mg/L chloride, 250 mg/L sulfate, and 340 mg/L hardness measured as CaCO3, contaminants in the ammonium acetate preservative. Bias can be caused by isotopic impurity of standards. |
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Quality Control Requirements
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Calibration Standard, Continuing Calibration Check (CCC), Field Duplicates (FD), Field Reagent Blank (FRB), Isotope Dilution Analogues, Isotope Performance Standards, Laboratory Fortified Blank (LFB), Laboratory Fortified Sample Matrix (LFSM), Laboratory Fortified Sample Matrix Duplicate (LFSMD), Laboratory Reagent Blank (LRB), Primary Dilution Standards (PDSs), Isotope Performance Standard PDS, Isotope Dilution Analogue PDS. |
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Sample Handling
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Samples are collected in polypropylene bottles fitted with polypropylene screw caps, or polyethylene bottles with polypropylene screw caps. The bottle volume should approximate the volume of the sample. Based on sample volume, add ammonium acetate to each sample bottle as a solid (prior to shipment to the field or immediately prior to sample collection) to achieve a 1g/L concentration of ammonium acetate. After collecting the sample, cap the bottle and agitate by hand until the preservative is dissolved. Keep the sample sealed from time of collection until extraction. Each sample set must include an FRB consisting of reagent water poured into a sample bottle containing preservative. Samples must be shipped on ice and are good if any ice remains in the cooler when it is received at the laboratory or the bottles are received within 2 days of collection and below 10 °C. Samples must be stored in the laboratory at or below 6 °C until extraction. Samples must not be frozen and should be analyzed as soon as possible. Samples must be extracted within 28 days of collection. Extracts are generally stored at room temperature and must be analyzed within 28 days after extraction. |
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Maximum Holding Time
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Samples must be extracted within 28 days of collection. Extracts must be analyzed within 28 days after extraction. |
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Relative Cost
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Sample Preparation Methods
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