Zwitterionic, Cationic, and Anionic Fluorinated Chemicals in Aqueous Film Forming Foam Formulations and Groundwater from U.S. Military Bases by Nonaqueous Large-Volume Injection HPLC-MS/MS
Abstract
A new analytical method was developed to quantify 26 newly-identified and 21 legacy (e.g. perfluoroalkyl carboxylates, perfluoroalkyl sulfonates, and fluorotelomer sulfonates) per and polyfluorinated alkyl substances (PFAS) in groundwater and aqueous film forming foam (AFFF) formulations. Prior to analysis, AFFF formulations were diluted into methanol and PFAS in groundwater were micro liquid-liquid extracted. Methanolic dilutions of AFFF formulations and groundwater extracts were analyzed by large-volume injection (900 μL) high-performance liquid chromatography tandem mass spectrometry. Orthogonal chromatography was performed using cation exchange (silica) and anion exchange (propylamine) guard columns connected in series to a reverse-phase (C18) analytical column. Method detection limits for PFAS in groundwater ranged from 0.71 ng/L to 67 ng/L, and whole-method accuracy ranged from 96% to 106% for analytes for which matched authentic analytical standards were available. For analytes without authentic analytical standards, whole-method accuracy ranged from 78 % to 144 %, and whole-method precision was less than 15 % relative standard deviation for all analytes. A demonstration of the method on groundwater samples from five military bases revealed eight of the 26 newly-identified PFAS present at concentrations up to 6900 ng/L. The newly-identified PFAS represent a minor fraction of the fluorinated chemicals in groundwater relative to legacy PFAS. The profiles of PFAS in groundwater differ from those found in fluorotelomer- and electrofluorination-based AFFF formulations, which potentially indicates environmental transformation of PFAS.
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Telomerization-manufactured PFAS do not typically contain PFAAs, but do contain fluorotelomers that are now known to degrade to PFCAs.
“Telomerization-manufactured PFAS do not typically contain PFAAs (Backe et al., 2013), but do contain fluorotelomers that are now known to degrade to PFCAs (Buck et al., 2011; Butt et al., 2013; Harding-Marjanovic et al., 2015).”
From Per- and polyfluoroalkyl substances (PFAS) mass flux and mass balance at an aqueous film-forming foam release site in semiarid eastern New Mexico, USA (2025) · cites this paper as Backe et al., 2013
Telomerization-manufactured PFAS dominating the precursor component of PFAS flux is typical in groundwater at AFFF sites.
“which is typical in groundwater at AFFF sites (Backe et al., 2013).”
From Per- and polyfluoroalkyl substances (PFAS) mass flux and mass balance at an aqueous film-forming foam release site in semiarid eastern New Mexico, USA (2025) · cites this paper as Backe et al., 2013
The similarity in fluorine discharge between AFFF released during fire training and among PFAS in groundwater suggests that PFAS precursors that contribute to measured PFAS in groundwater at the site are well-represented in the target analyses performed by Backe et al. (2013) or that rates of PFAS retention in the subsurface are similar to rates of transformation from unknown precursors to PFAS
“The similarity in fluorine discharge between AFFF released during fire training and among PFAS in groundwater (Table 2) suggests that PFAS precursors that contribute to measured PFAS in groundwater at the site are well-represented in the target analyses performed by Backe et al. (2013) or that rates of PFAS retention in the subsurface are similar to rates of transformation from unknown precursors”
From Per- and polyfluoroalkyl substances (PFAS) mass flux and mass balance at an aqueous film-forming foam release site in semiarid eastern New Mexico, USA (2025) · cites this paper as Backe et al., 2013
PFHxS flux exceeding PFOS flux is a trend typical in groundwater at AFFF sites where 6-fluorocarbon PFAA precursors are abundant.
“a trend typical in groundwater at AFFF sites where 6-fluorocarbon PFAA precursors are abundant (Backe et al., 2013).”
From Per- and polyfluoroalkyl substances (PFAS) mass flux and mass balance at an aqueous film-forming foam release site in semiarid eastern New Mexico, USA (2025) · cites this paper as Backe et al., 2013
These results agree with findings at other AFFF sites where these compounds can be found in groundwater at higher concentrations than is typically found in AFFF, suggesting transformation from precursor compounds.
“These results agree with findings at other AFFF sites where these compounds can be found in groundwater at higher concentrations than is typically found in AFFF, suggesting transformation from precursor compounds (Backe et al., 2013).”
From Per- and polyfluoroalkyl substances (PFAS) mass flux and mass balance at an aqueous film-forming foam release site in semiarid eastern New Mexico, USA (2025) · cites this paper as Backe et al., 2013
Commercial standards are available for <10 out of the hundreds of precursors previously detected in AFFF.
“Commercial standards are available for <10 out of the hundreds of precursors previously detected in AFFF.7−10”
From Centurial Persistence of Forever Chemicals at Military Fire Training Sites (2023) · cites this paper as [9]
An increasing number of studies have identified a variety of precursors and replacement products for compounds such as PFOA in both groundwater and surface water.
“An increasing number of studies have identified a variety of precursors and replacement products for compounds such as PFOA in both groundwater and surface water (Backe et al. 2013; Barzen-Hanson et al. 2017; Strynar et al. 2015; Sun et al. 2016).”
From Evaluation of a national data set for insights into sources, composition, and concentrations of per- and polyfluoroalkyl substances (PFASs) in U.S. drinking water (2018) · cites this paper as Backe et al. 2013
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“Recent studies have identified numerous additional PFASs that co-occur with UCMR3 PFASs in surface water and groundwater (e.g. Backe et al. 2013; Barzen-Hanson et al. 2017; Strynar et al. 2015).”
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- Authors
- Backe, W. J., Day, T. C., & Field, J. A.
- Affiliations
- Oregon State University (US)
- Corresponding author
- Field, Jennifer A.
- Venue
- Environmental Science & Technology
- Publisher
- American Chemical Society (ACS)
- Published
- 2013-05-01
- Volume
- 47
- Issue
- 10
- Pages
- 5226-5234
- ISSN
- 0013-936X (ISSN-L)
- 1520-5851
- OpenAlex
- W2334394530
- Cited by
- 611
- References
- 41
- Citations by year
- 2026: 60 · 2025: 65 · 2024: 71 · 2023: 75 · 2022: 73 · 2021: 68 · 2020: 53 · 2019: 32 · 2018: 34 · 2017: 33 · 2016: 16 · 2015: 16 · 2014: 10 · 2013: 4
- FWCI
- 12.23
- Type
- journal article
- Language
- en
- Open access
- closed
- Locations
- Environmental Science & Technology (publishedVersion)
- PubMed (publishedVersion)
- Funders
- Strategic Environmental Research and Development Program
- Topics
- Physical Sciences › Environmental Science › Environmental Chemistry › Per- and polyfluoroalkyl substances research
- Life Sciences › Pharmacology, Toxicology and Pharmaceutics › Pharmaceutical Science › Fluorine in Organic Chemistry
- Physical Sciences › Environmental Science › Health, Toxicology and Mutagenesis › Chemical Analysis and Environmental Impact
- Keywords
- per- and polyfluoroalkyl substances, PFAS, aqueous film-forming foam, groundwater contamination, military installations, fluorotelomer sulfonates, perfluoroalkyl carboxylates, perfluoroalkyl sulfonates, large volume injection, fluorinated compounds
- MeSH terms
- Anions, Cations, Chromatography, High Pressure Liquid, Fluorine, United States, Water, Water Pollutants, Chemical, Tandem Mass Spectrometry, Groundwater
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