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PFAS Analysis by U.S. EPA Method 1633 for Aqueous, Solid, Biosolids, and Tissue

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  • Sample Matrix: aqueous, solid, biosolids, and tissue samples
  • Sample Preparation: WAX solid-phase extraction
  • Detection Technique: LC-MS/MS

Analysis of Per- and Polyfluoroalkyl Substances (PFAS) in Aqueous, Solid, Biosolids, and Tissue Samples by LC-MS/MS

U.S. EPA Method 1633 is used for the analysis of 40 PFAS in aqueous, solid, biosolids, and tissue samples. The analysis of bile acids TCDCA, TDCA, and TUDCA is also required. EPA Method 1633 combines solid-phase extraction sample preparation using weak anion exchange (WAX) cartridges with LC-MS/MS analysis on a C18 column. The method is performance based and allows modifications to be made to improve performance (e.g., to overcome interferences or improve sensitivity, accuracy, or precision), but only if all method performance criteria are met. The full analyte list and recommended products for PFAS analysis in aqueous, solid, biosolids, and tissue samples by Method 1633 are provided below. In addition, you can register and directly compare analyte lists and matrices across PFAS analysis methods here or visit www.restek.com/PFAS to explore our technical resources for PFAS analysis.

 

Analyte List for U.S. EPA Method 1633 for PFAS Analysis

PFAS acronyms, compound names, and CAS numbers vary across methods and guidelines, and they also depend on compound form (e.g., neutral vs. salt). The following list uses standardized terminology to allow easy comparison across the methods and guidelines in our comprehensive guide. Please refer to U.S. EPA Method 1633 for method-specific nomenclature. Note that the analysis of bile acids TCDCA, TDCA, and TUDCA is also required by this method.

Acronym Compound Name CAS#
NEtFOSAA N-ethyl perfluorooctanesulfonamidoacetic acid 2991-50-6
NMeFOSAA N-methyl perfluorooctanesulfonamidoacetic acid 2355-31-9
PFBS Perfluoro-1-butanesulfonic acid 375-73-5
PFDA Perfluorodecanoic acid 335-76-2
PFDoA Perfluorododecanoic acid 307-55-1
PFHpA Perfluoroheptanoic acid 375-85-9
PFHxS Perfluoro-1-hexanesulfonic acid 355-46-4
PFHxA Perfluorohexanoic acid 307-24-4
PFNA Perfluorononanoic acid 375-95-1
PFOS Perfluorooctanesulfonic acid 1763-23-1
PFOA Perfluorooctanoic acid 335-67-1
PFTeDA Perfluorotetradecanoic acid 376-06-7
PFTrDA Perfluorotridecanoic acid 72629-94-8
PFUnA Perfluoroundecanoic acid 2058-94-8
HFPO-DA, GenX Hexafluoropropylene oxide dimer acid 13252-13-6
PFBA Perfluorobutanoic acid 375-22-4
PFPeA Perfluoropentanoic acid 2706-90-3
PFDS Perfluoro-1-decanesulfonic acid 335-77-3
PFHpS Perfluoro-1-heptanesulfonic acid 375-92-8
PFPeS Perfluoro-1-pentanesulfonic acid 2706-91-4
FOSA Perfluoro-1-octanesulfonamide 754-91-6
4:2 FTS 1H,1H,2H,2H-Perfluorohexane sulfonic acid 757124-72-4
6:2 FTS 1H,1H,2H,2H-Perfluorooctane sulfonic acid 27619-97-2
8:2 FTS 1H,1H,2H,2H-Perfluorodecane sulfonic acid 39108-34-4
NMeFOSA N-Methylperfluorooctanesulfonamide 31506-32-8
NEtFOSA N-ethylperfluorooctanesulfonamide 4151-50-2
9Cl-PF3ONS 9-Chlorohexadecafluoro-3-oxanonane-1-sulfonic acid (F-53B Major) 756426-58-1
11Cl-PF3OUdS 11-Chloroeicosafluoro-3-oxaundecane-1-sulfonic acid (F-53B Minor) 763051-92-9
ADONA 4,8-Dioxa-3H-perfluorononanoic acid 919005-14-4
PFNS Perfluoro-1-nonanesulfonic acid 68259-12-1
PFEESA Perfluoro(2-ethoxyethane)sulfonic acid 113507-82-7
NFDHA Nonafluoro-3,6-dioxaheptanoic acid 151772-58-6
PFMPA Perfluoro-3-methoxypropanoic acid 377-73-1
PFMBA Perfluoro-4-methoxybutanoic acid 863090-89-5
NMeFOSE 2-(N-methylperfluoro-1-octanesulfonamido)-ethanol 24448-09-7
NEtFOSE 2-(N-ethylperfluoro-1-octanesulfonamido)-ethanol 1691-99-2
PFDoS Perfluorododecane sulfonate 79780-39-5
3:3 FTCA 3:3 Fluorotelomer carboxylic acid 356-02-5
5:3 FTCA 5:3 Fluorotelomer carboxylic acid 914637-49-3
7:3 FTCA, FHpPA 7:3 Fluorotelomer carboxylic acid or 3-perfluoroheptyl propanoic acid 812-70-4

 

Recommended Products for U.S. EPA Method 1633 for PFAS Analysis

ANALYSIS

Analytical LC Columns:

  • Raptor C18 SPP column: 2.7 μm, 50 x 2.1 mm (cat.# 9304A52)
  • Force C18 FPP column: 1.8 μm, 50 x 2.1 mm (cat.# 9634252)

Delay Columns:

  • PFAS delay column: 5 µm, 50 x 2.1 mm (cat.# 27854)
  • PFAS delay column: 5 µm, 50 x 3.0 mm (cat.# 580959 [custom product])

Guard Columns:

  • UltraShield UHPLC precolumn filter: 0.2 µm frit (cat.# 25809)
  • EXP direct connect holder for EXP guard cartridges (cat.# 25808)
  • Raptor C18 EXP guard column cartridge: 2.7 µm, 5 x 2.1 mm (cat.# 9304A0252)

SAMPLE HANDLING

Sample Prep:

  • 30 mm syringe filter: 0.45 µm, nylon (cat.# 23981)
  • 30 mm syringe filter: 0.22 µm, nylon (cat.# 23980)
  • Deactivated borosilicate glass wool (cat.# 20789)
  • Thomson SINGLE StEP standard filter vials with screw-top caps: 0.2 µm, nylon w/preslit cap (cat.# 27896)
  • Resprep PFAS SPE cartridge: 6 mL, WAX 150 mg/GCB 50 mg (cat.# 28930)
  • Resprep PFAS SPE cartridge with filter aid: 6 mL, filter aid 2000 mg/WAX 150 mg/GCB 50 mg (cat.# 28931)
  • Resprep polymeric SPE cartridge: WAX, 6 mL/500 mg, 30 µm (cat.# 28268)
  • Resprep polymeric SPE cartridge: WAX, 6 mL/200 mg, 30 µm (cat.# 28292)
  • Q-sep multispeed centrifuge for QuEChERS (cat.# 28295)

Sample Reservoirs:

  • Polypropylene sample reservoir: 75 mL (cat.# 26015)
  • Polypropylene connectors (cat.# 26007)

Vacuum Manifolds:

  • Resprep QR-24 vacuum manifold (cat.# 28299-VM)
  • Resprep QR-12 vacuum manifold (cat.# 28298-VM)

Vacuum Pumps:

  • Chemker 300 PTFE vacuum pump: 20 L/min, AC110 V, 60 Hz (cat.# 27426)
  • Chemker 300 PTFE vacuum pump: 18 L/min, AC220 V, 50 Hz (cat.# 27427)

GENERAL LAB SUPPLIES

  • Polypropylene vials: 100-pk. (cat.# 23243)
  • Polypropylene vials: 1000-pk. (cat.# 23246)
  • Polyethylene vial caps: 100-pk. (cat.# 23244)
  • Polyethylene vial caps: 1000-pk. (cat.# 23247)
  • Centrifuge tubes: 50 mL, 50-pk. (cat.# 25846)
  • Centrifuge tubes: 50 mL, 500-pk. (cat.# 28290)
  • Norm-Ject plastic syringe: 10 mL Luer Lock tip (cat.# 22775)
  • Norm-Ject plastic syringe: 5 mL Luer Lock tip (cat.# 22774)

 

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