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5 Conclusion on what is needed and what is proposed

A universal PFAS restriction, covering a wide range of PFAS uses
, has been proposed by the national authorities of Germany, Denmark, the Netherlands, Norway, and Sweden. This proposal, submitted to ECHA in January 2023, is currently undergoing evaluation by ECHA's scientific committees. It follows several other regulations related to specific PFAS substances, which are already in force (see also chapter 4.1). As the need of controllability is equally important in all these legislative measures, learning from experiences and working together to improve the approaches for authorities and industry seems extremely important. This is in particular true as several additional legislative measures are currently under discussion like the inclusion of long-chain perfluorinated carboxylic acids (C9-21 PFCAs) in the Stockholm Convention or the suggested restrictions for undecafluorohexanoic acid (PFHxA), its salts, and related substances. Furthermore, in January 2022, ECHA introduced a restriction proposal specifically targeting PFAS used in firefighting foams. The scientific committees at ECHA endorsed this proposal in their opinions finalized in June 2023. The European Commission, in collaboration with EU countries, will decide on this restriction separately, as it is not part of the universal PFAS restriction proposed by the five national authorities.
In the following, legislations that are already in place are summarised focusing on the aspect of controllability.
Selected PFAS are regulated under the Stockholm Convention globally. In 2009, perfluorooctane sulfonic acid (PFOS) and its derivatives has been incorporated into the international Stockholm Convention for restriction of their use. As a consequence, the EU has imposed restrictions on PFOS for over a decade, operating within the framework of the EU Persistent Organic Pollutants (POPs) Regulation.
Regulation (EU) 2022/2400 of the European Parliament and of the Council of 23 November 2022 amending Annexes IV and V to Regulation (EU) 2019/1021 on persistent organic pollutants (Text with EEA relevance)
 The Stockholm Convention also oversees the worldwide elimination of perfluorooctanoic acid (PFOA), its salts, and PFOA-related compounds. PFOA has been prohibited under the EU POPs Regulation since July 4, 2020. Recently, PFHxS and its salts and related compounds have been included. The European Commission subsequently integrated this substance group into the EU's POPs Regulation in May 2023, and the regulation came into effect on August 28, 2023.
The lowest threshold for PFOS is 10 mg/kg where it is present in substances or in mixtures, for PFOA or any of its salts a limit is set at 0.025 mg/kg and for PFHxS or any of its salts at 0.025 mg/kg where they are present in substances, mixtures or articles. In Article 8 of the EU POP regulation it says that the Forum for Exchange of Information on Enforcement shall be used to coordinate a network of the Member States' authorities responsible for enforcement of this Regulation.
Starting from February 2023, the European Union/European Economic Area (EU/EEA) imposed restrictions on perfluorinated carboxylic acids (C9-14 PFCAs), along with their salts and precursors. In the corresponding Annex XV report
 it is stated that enforcement authorities can set up efficient enforcement mechanisms to monitor industry`s compliance with the proposed restriction. Although there are no standard analytical methods to measure the content of C9-C14 PFCAs, their salts and related substances in articles and mixtures yet available, those methods are being developed already for the restriction of PFOA and related substances. The same methods can be applied for testing C9-C14 PFCAs and related substances. Given that methods exist, the absence of an EU standard analytical method is not considered as a hindrance to the enforceability of the proposed restriction. Nevertheless, the establishment of an EU standard method could make the routine implementation of these tests easier, but it would also imply expenditure of time and money. At the same time, the efforts for the development of such a standardized method are minimized due to the fact that there is already a standardized method (under development) for the very similar restriction of PFOS.
Also in the Commission Regulation 2017/1000 (Annex XVII entry 68) regarding PFOA
 it is stated that while a standard analytical method is available for the determination of extractable PFOS in coated and impregnated solid articles, liquids and firefighting foams (CEN/TS 15968:2010), which most likely can be adjusted to also include PFOA and PFOA-related substances with a relevant detection limit, at present no such standard method is available for extraction and chemical analysis of those substances. The deferral period for the restriction should allow the further development of suitable analytical methods that can be applied to all matrices.
The current universal PFAS restriction proposal is to restrict the manufacturing, the placing on the market and the use of PFAS as substances on their own and the placing on the market of PFAS in another substance (as constituent), in a mixture and in an article, in a concentration of or above:
    • 25 ppb for any PFAS as measured with targeted PFAS analysis (polymeric PFAS excluded from quantification)
    • 250 ppb for the sum of PFAS measured as sum of targeted PFAS analysis, optionally with prior degradation of precursors (polymeric PFAS excluded from quantification)
    • 50 ppm for PFAS (polymeric PFAS included). If total fluorine exceeds 50 mg F/kg the manufacturer, importer or downstream user shall upon request provide to the enforcement authorities a proof for the fluorine measured as content of either PFAS or non-PFAS.
    In general, PFAS enforcement can be done by administrative controls and/or chemical analysis of chemical products and articles. Effective PFAS enforcement based on chemical analysis relies on accurate and reproducible analytical methods and a commitment to ongoing research and improvement in the field of PFAS analysis. Collaboration between regulators, laboratories and research institutions is essential to achieve these goals. Ideally, simple and inexpensive but robust analytical methods should be developed that provide reliable and accurate results. However, it will not be possible to develop a single method that covers the full range of PFAS compounds with the required detection limits and which is suitable for all relevant matrices. It is a common understanding among stakeholders and experts that a combination of methods will be needed.
    Unreliable test methods for the enforcement of restricted PFAS can have significant consequences:
    • Inaccurate Regulatory Compliance: Unreliable tests may produce false results, leading to incorrect assessments of PFAS levels in chemicals and products. This can result in industries mistakenly being deemed compliant with regulations when they are not, or vice versa. However, due to the large group of PFAS, it is assumed that an underestimation of the PFAS content is more likely than an overestimation.
    • Environmental and Health Risks: If PFAS contamination goes undetected due to unreliable tests, it can lead to potential health risks of consumers and communities and/or increased environmental contamination.
    • Legal Challenges: Regulatory agencies, industries and affected parties may engage in legal disputes if the test methods are unreliable, further complicating enforcement efforts.
    • Resource Misallocation: Inefficient use of resources may occur as agencies allocate time and funds to test methods that do not yield accurate results, diverting resources from more effective enforcement measures.
    • Public Trust Erosion: Public trust in regulatory agencies can erode if unreliable testing methods are perceived as ineffective in safeguarding public health and the environment.
    To mitigate these consequences, it is crucial to continually improve and validate test methods for PFAS detection, ensuring their accuracy and reliability in enforcement efforts. In the following table key aspects needed for efficient and effective PFAS enforcement regarding analytical methods are presented, along with proposed strategies:
    Table 9: Needs and proposal for an efficient PFAS enforcement regarding analytical methods.
    Aspect
    Need
    Proposal
    Standardized Analytical Methods
    Develop and establish standardized analytical methods for PFAS analysis to ensure consistency and comparability of results across laboratories and regulatory agencies.
    Collaborate with international standards organizations to create and update standardized methods for PFAS analysis, such as ASTM International and ISO. These methods should cover a wide range of PFAS compounds and matrices.
    Method Validation and Certification
    Rigorously validate analytical methods to demonstrate their accuracy, precision, sensitivity, and selectivity for various PFAS compounds and matrices.
    Regulatory agencies and accredited laboratories should conduct method validation studies, and certified reference materials (CRMs) for PFAS should be developed and made available to laboratories for calibration and quality control.
    Accredited Laboratories
    Ensure that laboratories conducting PFAS analysis are accredited and follow strict quality assurance/quality control (QA/QC) procedures.
    Establish accreditation programs specific to PFAS analysis and regularly assess laboratory performance through proficiency testing programs. Encourage laboratories to participate in interlaboratory studies for method validation and improvement.
    Non-Targeted Screening Methods
    Develop and refine non-targeted screening methods to identify known and emerging PFAS compounds in complex matrices.
    Collaborate with researchers and analytical experts to advance non-targeted screening techniques, such as high-resolution mass spectrometry, and establish data libraries for PFAS compounds.
    Method Harmoni­zation
    Harmonize analytical methods and reporting criteria among regulatory agencies and regions to facilitate data sharing and comparison.
    Collaborate with international organizations and adopt standardized reporting formats and units of measurement for PFAS data. Develop mechanisms for sharing (findability, accessibility, interoperability and reusability FAIR) data among regulatory agencies and laboratories.
    Method Detection and Reporting Limits
    Establish method detection limits (MDLs) and reporting limits (RLs) that are appropriate for PFAS analysis in different matrices.
    Regulatory agencies should define MDLs and RLs based on method performance data and the specific requirements of PFAS regulations.
    Data Quality Assurance
    Implement robust data quality assurance practices to ensure the accuracy and reliability of PFAS data.
    Develop and enforce QA/QC protocols, including the use of CRMs, blank samples, and internal standards, to monitor and verify data quality throughout the analytical process.
    Method Updates and Research
    Stay updated on advancements in PFAS analysis and continuously improve analytical methods to address emerging PFAS compounds.
    Establish research programs and collaborations to explore new analytical techniques and improve existing methods. Encourage the publication of method updates and improvements.
    The following generic approach is proposed to analyse PFAS levels at a reasonable cost:
    1. Administrative assessment without chemical analysis. In a first step, enforcement agencies can examine routines, datasheets and chemical management systems of industries, as well as conducting interviews about chemical content and technologies used in chemical products and articles with typical PFAS functions. This step, which is not expected to be very costly, relies on the cooperation and full transparency of industry. This will allow for a first risk assessment and might help in drawing up a potential analytical project plan.
    2. Fast screening methods to determine the total amount of fluorine (TF) in the sample. Ideally, these methods are inexpensive, require little sample preparation and can be used for the screening of both chemical products and articles. Total amount of fluorine can be determined directly in the field without any sample preparation (surface techniques). However, these methods have higher detection limits, are often not specific enough, and are not always available in commercial laboratories. No initiatives for standardisation of the surface techniques are taken yet which makes it less of interest for regulation. 19F-NMR is the only technique that can be used for the direct determination of the total organic fluorine (TOF), i.e. no extraction/adsorption (EOF or AOF) is required prior to analysis. The advantage is that no PFAS can be missed by sample preparation. TOF can also be determined by CIC (direct analysis TF) with correction for the inorganic fluorine. However, a lot of interferences can occur and extraction methods are often needed to overcome these interferences (especially for difficult matrices like construction products), the acquisition and operating cost of the instrument are high and specialised operators and analysts are necessary, which makes it of less practical interest. Other methods, such as XPS or WDXRF, may also be relevant, but need to be further developed and standard methods are currently lacking. With limited sample preparation, CIC can be used to determine total fluorine content (inorganic and organic) and can be a powerful technique for monitoring and regulation (standard CEN/EN 14582 is available). Other methods (CIC, HR-CS-GMAS) can be used for determination of the total organic fluorine content (including non-PFAS) as extractable/adsorbable (EOF and AOF) fluorine. The latter may be more suitable because projects are ongoing for standardisation (ISO/CD 18127). TF, EOF or AOF analysis can play an important role for fast assessment and commercial laboratories should be able to easily implement these techniques. The limit of detection might unfortunately not be sufficiently low enough (2 µg/L for AOF in drinking water). Further, total fluorine values cannot be translated to actual total PFAS content as the nature of the individual PFAS molecules and thus molar masses is unknown. TF, EOF or AOF however can be used as an indicator for further testing and not to demonstrate compliance, as the presence of (organic) fluorine does not equate to the presence of PFAS in a sample.
    3. Targeted analysis of selected samples identified by the screening methods. Targeted analysis of the sample can be performed by LC-MS (ionizable PFAS) and/or GC-MS (neutral and volatile ionizable PFAS) methods. Many commercial laboratories are equipped with the necessary instrumentation to perform LC-MS methods. Note that not all PFAS are measurable by targeted methods (e.g. fluoropolymers). The TOP assay is used to identify precursor compounds by converting PFAA precursors (e.g. fluorotelomers) into PFAAs via a hydroxyl radical based oxidation reaction. To obtain concentrations on PFAA precursors, the concentration of common target PFAS is measured before and after the oxidation using conventional targeted analysis methods like LC-MS. To capture different classes of PFAS, a combination of these techniques is recommended. For some matrices (mainly environmental matrices and some consumer products), standard protocols are already available for a limited number of PFAS compounds (#50–60). However, the number of target analytes should be extended and revised regularly (according to the industrial processes, uses and analytical data of monitoring campaigns). To bring the quality of the PFAS measurement protocols to the same quality level as for other compounds, certified (matrix) reference materials are a necessity and should be developed. And finally, analytical methods need to be accredited according to ISO 17025 for all relevant matrices. But even with all these measures in place, data of total fluorine and target methods will not fully overlap, and blind spots will remain. To shed light on these blind spots, non-target or suspect screening can be a valuable approach.
    4. Non-targeted or suspect screening (NTS/SS using HRMS) can deliver additional information where there is a large discrepancy between the total fluorine content and the PFAS identified by the targeted analysis. HRMS is used for the identification of unknown PFAS compounds. Non-target screening (both GC or/and LC) is usually an expensive analytical method that cannot be used for routine enforcement activities but can provide valuable information on what other types of PFAS are present in chemical products or articles that are not covered by the common targeted approaches. Standard protocols for non-targeted screening should be developed and libraries for PFAS compounds should be further established. First initiatives are already taken by the NORMAN network (NTS guidance) and the availability of the EPA PFAS master list (>5000 PFAS compounds). Fluoropolymers cannot be measured with the non-targeted or suspect screening methods. A pyrolysis-GC-MS method should be used to capture this class of PFAS.
    Nordic Council of Ministers I www.norden.org/publications I pub@norden.org