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Current and emerging analytical techniques to monitor PFAS
in the environment
Anna Kärrman
MTM Research Centre, Örebro University, Sweden
OECD Global Forum on the Environment Per- and Polyfluoroalkyl Substances (PFAS) 13 February 2024 1
Analytical questions
• PFAS group approach
How can all PFAS be
assessed?
How can legislations directed to
all PFAS be enforced?
2
EU Chemicals Strategy for Sustainability Towards a
Toxic-Free Environment
Analytical questions
• Less studied substances/groups
Knowledge gaps on occurrence, global and local transport, bioaccumulation, and safe limits
Wang et al. 2017
Knowledge on occurence and effects
Manufacturing volume
Analytical questions
• Lower detection limits
Hazards at lower concentrations
Need for cost-efficient methods
4
https://www.eea.europa.eu/themes/human/chemicals/emerging-chemical-risks-in-europe. US National Toxicology
Program, (2016); C8 Health Project Reports, (2012); WHO IARC, (2017); Barry et al., (2013); Fenton et al.,
(2009); and White et al., (2011).
Current and emerging techniques
5
PFAS fingerprint
Current and emerging techniques
6
Nontarget and suspect screening
 data bases ~15 000 PFAS
• limited possibilities for
quantitative analysis
• challenging data mining and
reduction, quantification
• standards needed for highest
confidence
Target analysis
 sensitive and specific using MS/MS
• large physicochemical range requires
• multiple techniques
• several/series of sample preparation
steps
• lack of commercial standards
• poorly ionizable compounds not
included
Specific PFAS analysis providing direct or
indirect structural information
Chemical conversions
 conversion by oxidation (TOP
Assay) or hydrolysis followed by target
analysis of oxidation/hydrolysis products
• not always quantitative yields
Requirements for low detection limits
7
 Water Frame Directive EQS/QS
PFAS24 4.4 ng/L PFOA equivalents
 Limit values for food (EU) 2022/2388,
PFAS4 down to 1.3 µg/kg
• <30% of the limit value is required
• the more PFAS included, the more challenging
Less studies groups: polymeric PFAS
8
 Less studied groups: dissolved and undissolved
polymeric PFAS
• LC-MS (APPI, ESI)
• pyrolysis-GC-MS
 Chemical conversion of side-chain
fluorinated copolymers
Distinguishing PTFE from PFAS surfactants in clothes with pyr-GC-MS (Muensterman et al., 2022)
15% fluorine yield
69% fluorine yield
Fredriksson et al., Chemosphere 2022
Current and emerging techniques
9
Sum of fluorine or F-
complexes
• measurement of F as
proxy of PFAS
• no sample pretreatment
returns
total fluorine (TF)
• after extraction 
Extractable Fluorine (EF),
or Extractable Organic
Fluorine (EOF)
• Sample pretreatment
defines the output
• Combustion ion chromatography (CIC)
(Miyake et al., 2007; DIN 38409-
59:2020-11)
• Particle Induced Gamma-ray Emission
(PIGE) spectroscopy (Ritter et al., 2017)
• Inductively coupled plasma mass
spectrometry (ICP-MS/MS) (Jamari et
al., 2017)
• Continuum source graphite furnace
molecular absorption spectroscopy (HR-
CS-GF-MAS) (Gehrenkemper et al.,
2021)
Targeting fluorine
10
Natural occuring Industrial chemicals
Natural occuring Industrial chemicals
Eg.
• CaF2
• NaF
• Na2PO3F
Eg.
• Trifluoromethane
• Fluoroacetate
• Fluorinated fatty acids
Eg.
• PF6
-
• BF4
-
Eg.
• PFAS
• Pharmaceuticals
• Agrochemicals
• F-gases
• Other industrial chemicals
Analysis of sum fluorine/fluorine complexes
11
• No pre-treatment = total F
• Pre-treatment excluding compound
classes = false negatives
• False positives by including non-
PFAS, inorganic fluorine, and
possibly non-prioritized PFAS, in the
pre-treatment
Extraction of WWTP sludge –comparison TF
with three diffent EOF methods.
Fredriksson 2023
12
Jiao et al. 2023 Environmental Science and Technology, Vol. 57, no 38, p. 14330-14339
Extractable fluorine mass balance – tap water
from China
Current and emerging techniques
13
Sum of fluorine or F-
complexes
• measurement of F as
proxy of PFAS
• no sample pretreatment
returns
total fluorine (TF)
• after extraction 
Extractable Fluorine (EF),
or Extractable Organic
Fluorine (EOF)
• Sample pretreatment
defines the output
Sum of effects
• capture the sum of mixture
effects of groups of chemicals
that elicit the same mode of
action
• high-trough put bioassays
• Thyroid hormone transport
disruption potential has been
suggested (Behnish et al., 2021)
Sum of perfluoroalkyls
 CF2 or CF3 groups can be targeted
and summed by NMR, XPS, FTIR
 highly selective
• detection limits high
Current analytical possibilities
• Specific PFAS analysis based on
structural information
• PFAS-n, or nΣPFAS (n=
number of PFAS analyzed)
• PFAS Total – or what the
technique is able to assess using
different assumptions
• ”Total Assessed PFAS” by
[methodology]
14
Needs at international level
• Common definition of the analytical requirements for
assessing PFAS as a group
standardization of methods delays progress
 Clear and harmonized QA/QC guidance can act as
intermediate, or pre-standardisation
15
Needs at international level
• Common definition of the analytical requirements for
assessing PFAS as a group
• Acceptance of the group approach
• acceptance of non-specific methods, and
semi-quantitation
• value fast screening vs specific (structural)
confidence, and adapt the requirements
16
PFAS
TOTAL
Technical
Social
acceptance
Economical
Needs at international level
• Common definition of the analytical requirements for
assessing PFAS as a group
• Acceptance of the group approach
• Support the analytical development for regulatory
purposes
• regulatory – scientist dialogues
• availability of reference standards
17
Thank you for your
attention!
18
Selection of references
19
Wang et al. (2017). A Never-Ending Story of Per- and Polyfluoroalkyl Substances (PFASs)?
Environ. Sci. Technol 51, 5, 2508–2518
• Suspect and nontarget screening
Charbonnet, et al. (2022). Communicating Confidence of Per- and Polyfluoroalkyl Substance
Identification via High-Resolution Mass Spectrometry. ​​ Environ Sci Technol Letters. 9(6):473–
481
Zweigle et al. (2023) PFAS-Contaminated Soil Site in Germany: Nontarget Screening before
and after Direct TOP Assay by Kendrick Mass Defect and FindPFΔS. Environ Sci Technol
• Sum of perfluoroalkyl groups
Gauthier, J. R. & S. A. Mabury. (2023). Identifying Unknown Fluorine-Containing Compounds
in Environmental Samples Using 19F NMR and Spectral Database Matching. Environ Sci
Technol , 57(23): 8760-8767.
Tokranov et al. (2019). How Do We Measure Poly- and Perfluoroalkyl Substances (PFASs) at
the Surface of Consumer Products? Environ Sci Technol Letters 6(1): 38−43.
• Pyrolysis-GC-MS
Fisher & Scholz-Böttcher. (2017). Simultaneous Trace Identification and Quantification of
Common Types of Microplastics in Environmental Samples by Pyrolysis-Gas Chromatography-
Mass Spectrometry Environ Sci Technol 51(9):5052-5060.
Muensterman et al. (2022). Disposition of Fluorine on New Firefighter Turnout Gear. Environ
Sci Technol 18;56(2):974-983.
• Sum of F or F-complexes
Miyake et al. (2007). Trace analysis of total fluorine in human blood using combustion ion
chromatography for fluorine: a mass balance approach for the determination of known and
unknown organofluorine compounds J Chromatogr A. 2007 Jun 22;1154(1-2):214-21;
DIN 38409-29:1996-01. German standard methods - Part 29: Determination of dissolved,
absorbable organically bound fluorine (AOF).
Ritter et al. (2017). PIGE as a screening tool for Per- and polyfluorinated substances in papers
and textiles. DOI:10.1016/J.NIMB.2017.05.052
Jamari et al. (2019). Novel non-targeted analysis of perfluorinated compounds using fluorine-
specific detection regardless of their ionisability (HPLC-ICPMS/MS-ESI-MS). Analytica
Chimica Acta, vol. 1053, pp. 22–31.
Gehrenkemper et al. (2021). Determination of organically bound fluorine sum parameters in river water
samples—comparison of combustion ion chromatography (CIC) and high resolution-continuum source-graphite
furnace molecular absorption spectrometry (HR-CS-GFMAS). Anal Bioanal Chem 413, 103–115
• Chemical conversion
Houtz, E.F. and David L. Sedlak. (2012). Oxidative Conversion as a Means of Detecting Precursors to
Perfluoroalkyl Acids in Urban Runoff. Environ Sci Technol . 46(17): 9342-9349
Hutchinson et al. (2020) Pre-digestion with hydrogen peroxide. Environ. Chem. 17, 558–567
Zweigle et al. (2022). PhotoTOP: PFAS Precursor Characterization by UV/TiO2 Photocatalysis. Environ. Sci.
Technol. 56, 22, 15728–15736
Bugsel et al. (2023). Photocatalytical transformation of fluorotelomer- and perfluorosulfonamide-based PFAS
on mineral surfaces and soils in aqueous suspensions. Sci Total Environ. 894:164907.
Kaiser et al.. (2021): Ozone as oxidizing agent for the total oxidizable precursor (TOP) assay and as a preceding
step for activated carbon treatments concerning per- and polyfluoroalkyl substance removal. J of Environ
Management 300: 113692.
Nikiforov, V.A. (2021): Hydrolysis of FTOH precursors, a simple method to account for some of the unknown
PFAS. Chemosphere, 276: 130044.
Liagkouridis et al. (2022). Combined Use of Total Fluorine and Oxidative Fingerprinting for Quantitative
Determination of Side-Chain Fluorinated Polymers in Textiles. Environ. Sci. Technol. Lett., 9 (1), 30– 36,
Fredriksson et al..(2022). Analysis and Characterization of Novel Fluorinated Compounds used in Surface
Treatments Products. Chemosphere, 302, 134720
• Effect-based methods
Behnisch et al. (2021). Developing potency factors for thyroid hormone disruption by PFASs using TTR-TRβ
CALUX® bioassay and assessment of PFASs mixtures in technical products. Environ Int, 157: 106791.
• Extraction methods
Nickerson et al. (2020). Enhanced Extraction of AFFF-Associated PFASs from Source Zone Soils. Environ Sci
Technol 54(8):4952-4962
Fredriksson F. (2023). Analysis of fluoroalkyl sulfonamide (FASA) based copolymers: An indirect source of
non-polymeric PFAS. Doctoral thesis. Örebro Studies in Chemistry, ISSN 1651-4270 ; 30. urn:nbn:se:oru:diva-
105113

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OECD Global Forum on the Environment dedicated to Per- and Polyfluoroalkyl Substances: Current and emerging analytical techniques to monitor PFAS in the environment | Anna Kärrman

  • 1. Current and emerging analytical techniques to monitor PFAS in the environment Anna Kärrman MTM Research Centre, Örebro University, Sweden OECD Global Forum on the Environment Per- and Polyfluoroalkyl Substances (PFAS) 13 February 2024 1
  • 2. Analytical questions • PFAS group approach How can all PFAS be assessed? How can legislations directed to all PFAS be enforced? 2 EU Chemicals Strategy for Sustainability Towards a Toxic-Free Environment
  • 3. Analytical questions • Less studied substances/groups Knowledge gaps on occurrence, global and local transport, bioaccumulation, and safe limits Wang et al. 2017 Knowledge on occurence and effects Manufacturing volume
  • 4. Analytical questions • Lower detection limits Hazards at lower concentrations Need for cost-efficient methods 4 https://www.eea.europa.eu/themes/human/chemicals/emerging-chemical-risks-in-europe. US National Toxicology Program, (2016); C8 Health Project Reports, (2012); WHO IARC, (2017); Barry et al., (2013); Fenton et al., (2009); and White et al., (2011).
  • 5. Current and emerging techniques 5 PFAS fingerprint
  • 6. Current and emerging techniques 6 Nontarget and suspect screening  data bases ~15 000 PFAS • limited possibilities for quantitative analysis • challenging data mining and reduction, quantification • standards needed for highest confidence Target analysis  sensitive and specific using MS/MS • large physicochemical range requires • multiple techniques • several/series of sample preparation steps • lack of commercial standards • poorly ionizable compounds not included Specific PFAS analysis providing direct or indirect structural information Chemical conversions  conversion by oxidation (TOP Assay) or hydrolysis followed by target analysis of oxidation/hydrolysis products • not always quantitative yields
  • 7. Requirements for low detection limits 7  Water Frame Directive EQS/QS PFAS24 4.4 ng/L PFOA equivalents  Limit values for food (EU) 2022/2388, PFAS4 down to 1.3 µg/kg • <30% of the limit value is required • the more PFAS included, the more challenging
  • 8. Less studies groups: polymeric PFAS 8  Less studied groups: dissolved and undissolved polymeric PFAS • LC-MS (APPI, ESI) • pyrolysis-GC-MS  Chemical conversion of side-chain fluorinated copolymers Distinguishing PTFE from PFAS surfactants in clothes with pyr-GC-MS (Muensterman et al., 2022) 15% fluorine yield 69% fluorine yield Fredriksson et al., Chemosphere 2022
  • 9. Current and emerging techniques 9 Sum of fluorine or F- complexes • measurement of F as proxy of PFAS • no sample pretreatment returns total fluorine (TF) • after extraction  Extractable Fluorine (EF), or Extractable Organic Fluorine (EOF) • Sample pretreatment defines the output • Combustion ion chromatography (CIC) (Miyake et al., 2007; DIN 38409- 59:2020-11) • Particle Induced Gamma-ray Emission (PIGE) spectroscopy (Ritter et al., 2017) • Inductively coupled plasma mass spectrometry (ICP-MS/MS) (Jamari et al., 2017) • Continuum source graphite furnace molecular absorption spectroscopy (HR- CS-GF-MAS) (Gehrenkemper et al., 2021)
  • 10. Targeting fluorine 10 Natural occuring Industrial chemicals Natural occuring Industrial chemicals Eg. • CaF2 • NaF • Na2PO3F Eg. • Trifluoromethane • Fluoroacetate • Fluorinated fatty acids Eg. • PF6 - • BF4 - Eg. • PFAS • Pharmaceuticals • Agrochemicals • F-gases • Other industrial chemicals
  • 11. Analysis of sum fluorine/fluorine complexes 11 • No pre-treatment = total F • Pre-treatment excluding compound classes = false negatives • False positives by including non- PFAS, inorganic fluorine, and possibly non-prioritized PFAS, in the pre-treatment Extraction of WWTP sludge –comparison TF with three diffent EOF methods. Fredriksson 2023
  • 12. 12 Jiao et al. 2023 Environmental Science and Technology, Vol. 57, no 38, p. 14330-14339 Extractable fluorine mass balance – tap water from China
  • 13. Current and emerging techniques 13 Sum of fluorine or F- complexes • measurement of F as proxy of PFAS • no sample pretreatment returns total fluorine (TF) • after extraction  Extractable Fluorine (EF), or Extractable Organic Fluorine (EOF) • Sample pretreatment defines the output Sum of effects • capture the sum of mixture effects of groups of chemicals that elicit the same mode of action • high-trough put bioassays • Thyroid hormone transport disruption potential has been suggested (Behnish et al., 2021) Sum of perfluoroalkyls  CF2 or CF3 groups can be targeted and summed by NMR, XPS, FTIR  highly selective • detection limits high
  • 14. Current analytical possibilities • Specific PFAS analysis based on structural information • PFAS-n, or nΣPFAS (n= number of PFAS analyzed) • PFAS Total – or what the technique is able to assess using different assumptions • ”Total Assessed PFAS” by [methodology] 14
  • 15. Needs at international level • Common definition of the analytical requirements for assessing PFAS as a group standardization of methods delays progress  Clear and harmonized QA/QC guidance can act as intermediate, or pre-standardisation 15
  • 16. Needs at international level • Common definition of the analytical requirements for assessing PFAS as a group • Acceptance of the group approach • acceptance of non-specific methods, and semi-quantitation • value fast screening vs specific (structural) confidence, and adapt the requirements 16 PFAS TOTAL Technical Social acceptance Economical
  • 17. Needs at international level • Common definition of the analytical requirements for assessing PFAS as a group • Acceptance of the group approach • Support the analytical development for regulatory purposes • regulatory – scientist dialogues • availability of reference standards 17
  • 18. Thank you for your attention! 18
  • 19. Selection of references 19 Wang et al. (2017). A Never-Ending Story of Per- and Polyfluoroalkyl Substances (PFASs)? Environ. Sci. Technol 51, 5, 2508–2518 • Suspect and nontarget screening Charbonnet, et al. (2022). Communicating Confidence of Per- and Polyfluoroalkyl Substance Identification via High-Resolution Mass Spectrometry. ​​ Environ Sci Technol Letters. 9(6):473– 481 Zweigle et al. (2023) PFAS-Contaminated Soil Site in Germany: Nontarget Screening before and after Direct TOP Assay by Kendrick Mass Defect and FindPFΔS. Environ Sci Technol • Sum of perfluoroalkyl groups Gauthier, J. R. & S. A. Mabury. (2023). Identifying Unknown Fluorine-Containing Compounds in Environmental Samples Using 19F NMR and Spectral Database Matching. Environ Sci Technol , 57(23): 8760-8767. Tokranov et al. (2019). How Do We Measure Poly- and Perfluoroalkyl Substances (PFASs) at the Surface of Consumer Products? Environ Sci Technol Letters 6(1): 38−43. • Pyrolysis-GC-MS Fisher & Scholz-Böttcher. (2017). Simultaneous Trace Identification and Quantification of Common Types of Microplastics in Environmental Samples by Pyrolysis-Gas Chromatography- Mass Spectrometry Environ Sci Technol 51(9):5052-5060. Muensterman et al. (2022). Disposition of Fluorine on New Firefighter Turnout Gear. Environ Sci Technol 18;56(2):974-983. • Sum of F or F-complexes Miyake et al. (2007). Trace analysis of total fluorine in human blood using combustion ion chromatography for fluorine: a mass balance approach for the determination of known and unknown organofluorine compounds J Chromatogr A. 2007 Jun 22;1154(1-2):214-21; DIN 38409-29:1996-01. German standard methods - Part 29: Determination of dissolved, absorbable organically bound fluorine (AOF). Ritter et al. (2017). PIGE as a screening tool for Per- and polyfluorinated substances in papers and textiles. DOI:10.1016/J.NIMB.2017.05.052 Jamari et al. (2019). Novel non-targeted analysis of perfluorinated compounds using fluorine- specific detection regardless of their ionisability (HPLC-ICPMS/MS-ESI-MS). Analytica Chimica Acta, vol. 1053, pp. 22–31. Gehrenkemper et al. (2021). Determination of organically bound fluorine sum parameters in river water samples—comparison of combustion ion chromatography (CIC) and high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS). Anal Bioanal Chem 413, 103–115 • Chemical conversion Houtz, E.F. and David L. Sedlak. (2012). Oxidative Conversion as a Means of Detecting Precursors to Perfluoroalkyl Acids in Urban Runoff. Environ Sci Technol . 46(17): 9342-9349 Hutchinson et al. (2020) Pre-digestion with hydrogen peroxide. Environ. Chem. 17, 558–567 Zweigle et al. (2022). PhotoTOP: PFAS Precursor Characterization by UV/TiO2 Photocatalysis. Environ. Sci. Technol. 56, 22, 15728–15736 Bugsel et al. (2023). Photocatalytical transformation of fluorotelomer- and perfluorosulfonamide-based PFAS on mineral surfaces and soils in aqueous suspensions. Sci Total Environ. 894:164907. Kaiser et al.. (2021): Ozone as oxidizing agent for the total oxidizable precursor (TOP) assay and as a preceding step for activated carbon treatments concerning per- and polyfluoroalkyl substance removal. J of Environ Management 300: 113692. Nikiforov, V.A. (2021): Hydrolysis of FTOH precursors, a simple method to account for some of the unknown PFAS. Chemosphere, 276: 130044. Liagkouridis et al. (2022). Combined Use of Total Fluorine and Oxidative Fingerprinting for Quantitative Determination of Side-Chain Fluorinated Polymers in Textiles. Environ. Sci. Technol. Lett., 9 (1), 30– 36, Fredriksson et al..(2022). Analysis and Characterization of Novel Fluorinated Compounds used in Surface Treatments Products. Chemosphere, 302, 134720 • Effect-based methods Behnisch et al. (2021). Developing potency factors for thyroid hormone disruption by PFASs using TTR-TRβ CALUX® bioassay and assessment of PFASs mixtures in technical products. Environ Int, 157: 106791. • Extraction methods Nickerson et al. (2020). Enhanced Extraction of AFFF-Associated PFASs from Source Zone Soils. Environ Sci Technol 54(8):4952-4962 Fredriksson F. (2023). Analysis of fluoroalkyl sulfonamide (FASA) based copolymers: An indirect source of non-polymeric PFAS. Doctoral thesis. Örebro Studies in Chemistry, ISSN 1651-4270 ; 30. urn:nbn:se:oru:diva- 105113