4.3 Experiences from enforcement of PFAS restriction stated by the individual Nordic Agencies
In the following the experiences and observed challenges of each Nordic Agency were briefly summarized as stated by the individual agency representatives. However, none of the consulted Agency representatives knew any court cases where the analytical method used for the PFAS analyses has been a central point of interest.
4.3.1 Joint Nordic enforcement project
A joint Nordic enforcement project on PFOS and PFOA in chemical products and articles was launched in 2020 and completed at the end of 2021. The report was published online in 2022. The main responsibility for the project was assigned to the Finnish Safety and Chemicals Agency (Tukes), and participants from the other Nordic countries in the project group were from the Danish Environmental Protection Agency, the Swedish Chemicals Agency, the Finnish Safety and Chemicals Agency, the Norwegian Environment Agency and the Environmental Protection Agency of Iceland. The objectives of the joint enforcement project of the Nordic Enforcement Group were to check the compliance of chemical products and articles placed on the Nordic market with the restrictions in the POPs Regulation (EU No 2019/1021) on PFOA and PFOS, to raise awareness of the restrictions in the POPs Regulation and to learn together how to enforce the new restriction on PFOA. In addition, the presence of PFAS not yet restricted by any chemical legislation and extractable organic fluorine (EOF) were analysed to improve the authorities' knowledge on the use of PFAS in different products and articles. In total, 158 products were tested, 95 chemical products and 63 articles.
However, as the number of PFAS included in the analyses, as well as the analysis methods, differed between countries, it was difficult to conclude whether a particular product contained more PFAS than another. This, and the lack of reference material for most PFAS, posed another enforcement problem for PFAS. With regard to enforcement of the PFOA restriction, the lack of standardised analytical methods that measure PFOA, its salts and PFOA-related substances in different matrices at sufficiently low limits of quantification proved to be another major hurdle. This is compounded by the limited number of PFOA-related compounds that can be measured by currently available (non-standardised) methods.
4.3.2 Swedish Chemicals Agency (KEMI)
KEMI was part of the joint Nordic enforcement project on PFOS and PFOA in chemical products and articles (see chapter 4.3.1). During 2023 KEMI is going to enforce the PFOA-restriction (under the POPs Regulation) and the C9-C14 PFCAs-restriction (under the REACH Regulation) in cosmetics. The project is part of a joint EU-enforcement pilot project (11 countries participate in the project) and includes checking the labels of the cosmetic products for ingredients with INCI-names indicating PFOA-related substances or PFCAs. Some countries may conduct chemical analyses as well.
According to the experience of KEMI analysing for PFAS involves several challenges. KEMI stated that there are about 200 related substances that break down to C9-C14 PFCAs and about 400 related substances that break down to PFOA. Only a few of these substances are known today and have a substance identity in form of a CAS or EC number. Polymeric PFAS can currently not be analysed with targeted analysis, except for side chain perfluorinated compounds for which the side chain – once cleaved from the polymer chain – are accessible for targeted analysis. Non-polymeric PFAS can only be analysed with targeted analysis, once for a given PFAS the analytical reference standard is available (typically a C-13 labelled reference standard). Currently there are no laboratories that can identify more than about 50–60 individual PFAS. This is partly because of a lack of reference standards for many individual PFAS, which makes it difficult to look for specific substances in a sample. Furthermore, experts from KEMI reported back that there are no standardized methods today for the analysis of PFAS, different laboratories use different methods which means that the result can differ e.g., due to different extraction methods. Laboratories usually combine targeted analyses with screening methods, e.g. extractable organic fluorine (EOF), total fluorine (TF), total oxidizable precursors Assay (TOPA), total organic fluorine (TOF) and others. All these methods have their pros and cons, e.g., there is a risk that you cannot extract all the organic fluorine from a sample or that you extract inorganic fluorine as well. This leads to underestimating or overestimating the true content of PFAS in a sample by using only screening methods. There are also other factors that affect the result, e.g., risk of contamination from the measuring equipment (PTFE coating on the inside of the measuring instruments), water used for dilution, contamination from other samples or staff (e.g. hygiene products such as makeup, hair care products, etc.). The experts stressed that when analysing PFAS, it is very important that the laboratory has the right skills and experience with PFAS and has validated its methods.
In addition to addressing the above challenges, KEMI would be interested in guidance on enforcement of PFAS in chemical products and articles, including laboratory analysis, procurement of laboratory services, etc.
4.3.3 Swedish Environmental Agency
The Swedish Environmental Agency currently has no experiences with the enforcement of PFAS. However, one Agency representative pointed out that generally the number of restricted/enforceable substances and articles are already (only few PFAS and PFAS-related substances are restricted) very high which makes it challenging to identify what article/product does/does not comply. This problem will be even more pronounced in the future with more restrictions. Also, analysis are quite costly and affordable effective sampling/analysis tools would be appreciated.
4.3.4 Finnish Safety and Chemicals Agency (Tukes)
Tukes was leading the joint Nordic enforcement project on PFOS and PFOA in chemical products and articles (see chapter 4.3.1). In addition, Tukes conducted a pilot enforcement project on PFAS in clothes and impregnation sprays in 2019. In this project a method comparable with the standard method for PFOS (CEN/TS 15968) was used.
It was highlighted that at the moment analysing for PFAS involves several challenges. Experts from Tukes stressed, that there are currently no laboratories that can identify more than about 50–60 individual PFAS although there are several hundred of these substances (not all have a CAS or EC number). One reason for this is that there are no reference standards for many individual PFAS. This makes it difficult to look for specific substances in a sample. Some laboratories also have difficulties to achieve the low limits of quantification needed in measurements, e.g., 0.025 mg/kg for PFOA. Further, there are no standardized methods today for the analysis of PFAS for different sample types which might be relevant for the market surveillance (the result can differ between the laboratories even for the same sample). PFAS substances have numerous of uses in various product categories and, therefore, there are also wide spectrum of matrixes under the scope (e.g., textiles, polymers, cosmetic products). There are also other factors that affect the result, e.g., risk of contamination, highlighting the need for standardized procedures. Most of the laboratories in the Nordic countries are focused primarily on providing environmental monitoring of PFAS and therefore have experience in using standard test methods to detect PFAS in various environmental samples. For polymeric PFAS, according to the experience of the Agency, targeted PFAS analysis is not possible. Currently the typical laboratory approach is the determination of total organic fluorine, however no standard method is available by now.
4.3.5 Norwegian Environment Agency
In 2021/2022 the Norwegian Environment Agency was involved in four different projects in the context of PFAS analysis. The projects were (A) a joint Nordic enforcement project on PFOS and PFOA in chemical products and articles (see chapter 6.3.1) and Norwegian enforcement projects on the determination of PFOA and its precursors (sometimes in combination with total fluorine detection) in different matrixes which consisted of (B) chemical products for cars and boats, (C) different outdoor or textile articles and (D) food contact materials, meaning paper products and coated metal (frying pan).
In all projects standard methods for analysing PFAS were used in addition to TOPA measurements. One project further employed EOF analysis and this way evidence on further PFAS, either not yet regulated or identifiable by standard methods, could be found in articles. The analysis methods of another project were further supported using XRF analysis. From this project the Norwegian Environment Agency stated that XRF analysis was found to be a possible helpful screening method on fluorine content of the material prior to targeted testing.
The projects did result in the finding of different products containing PFOA or PFOA, from which most were below the enforcement limit, however, some were found to be above the enforcement limit and thus the project resulted in different enforcement actions, mostly the banning of said products. In one instance the exceeding of the limit was probably due to the product being produced before the limit value came into force. The product was nevertheless withdrawn by the producer.
Major drawbacks in the current enforcement of PFAS in products through all projects were reported to be the absence of standardized analysis methods for PFOA or the availability of PFAS reference material, which is needed for validation, calibration, and comparison of the analyses, thus leading to time-consuming and lengthy processes as well as high costs. Another main problem for enforcement was stated to be the low enforcement limit of 0.025 mg/kg, as reaching a limit of quantification below this value is often difficult mainly due to matrix effects.
4.3.6 Danish Environment Protection Agency
The Danish Chemical Inspection Service of the Danish Environment Protection Agency has experience in PFAS enforcement in both administrative and physical/chemical analysing control.
One example of ongoing administrative control is the regular check of safety data sheets on firefighting foam with focus on the content of regulated PFAS (PFOS and PFOA). Further, the Danish Chemical Inspection Service was analysing regulated PFAS (PFOS and PFOA) in (A) firefighting foam in hand portable fire extinguisher and (B) chemical products and their articles (project together with other Nordic Enforcement Agencies) (see chapter 4.3.1) for physical/chemical analysing control.
It is the Danish Chemical Inspection Services experience, that it is not possible to locate commercial laboratories or combination of laboratories, which are able to detect and identify all the PFAS compounds/substances, and their derivatives that are regulated/restricted according to POP and REACH. Most laboratories only offer PFAS analysis developed for the purpose of testing the compliance with the drinking water and feedstuff regulations or modified versions of these.
This does unfortunately severely limit the number PFAS compounds/substances that can be identified. To further aggravate the issues, most laboratories which can analytically identify some of the regulated PFAS compounds/substances, stated that the LOQ for their analysis is above the restriction level in the regulation, or that the experimental uncertainties are extremely high. No laboratory was able to perform any PFAS analysis on any other matrices than drinking water or feedstuff if the analysis need accreditation. To ensure the enforceability of a new restriction it would be highly appreciated if the restriction was always accompanied by an analytical method.
It was highlighted by Agency representatives that total organic fluorine/total fluorine is, in the opinion of The Danish Chemical Inspection Service, not a viable analytical method to determine the presence of PFAS, and neither can it be used to quantify the PFAS in a sample. Total organic fluorine/total fluorine can only be used to determine the presence of covalently bound fluorine/presence fluorine in the sample. However, the presence of fluorine does not equal the presence of PFAS in a sample. The presence of fluorine can be used as an indicator for selecting samples for further testing. For this to be feasible, it does require the total organic fluorine/total fluorine analysis to be significantly cheaper than the PFAS analysis.
4.3.7 Environmental Agency of Iceland
In an annual screening for chemicals in products, nature and indoors, the environmental Agency of Iceland investigated the content of PFAS in products used to enable water repellence for shoes and textiles. One hurdle for the agency was the selection of PFAS included in the screening, as targeted analyses were the preferred method, due to higher accuracy in the concentration measurements. A package deal was bought from a commercial laboratory, which also included a guidance on which PFAS to analyse, resulting in the 22 most common PFAS in Europe being chosen. A problem encountered during the analyses though was the matrix of the products, as the LOQ and LOD in some cases came out to be higher than the proposed enforcement limits. Especially for products like shoe cream or bees wax, which have a higher consistency and viscosity. Water sprays in comparison though had very good LODs and LOQs. The problem arising for enforcement is, that if the LOD and LOQ are higher than the enforcement limits, the applicant or producer must be given the benefit of a doubt.