Environmental screening of selected new brominated flame retardants and selected polyfluorinated compounds 2009

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1 Statlig program for forurensningsovervåking Rapportnr. 1067/2010 Environmental screening of selected new brominated flame retardants and selected polyfluorinated compounds 2009 TA Utført av DNV i samarbeid med NGI, Universitetet i Umeå, Universitetet i Örebro og Molab AS

2 Foreword Det Norske Veritas AS (DNV), the Norwegian Geotechnical Institute (NGI), University of Umeå, University of Örebro and Molab AS have on behalf of the Climate and Pollution Agency carried out the screening survey of "new" brominated flame retardants and selected polyfluorinated compounds in In this screening project several samples in different environmental matrices have been taken in different parts of Norway. This includes sediment from receiving waters and waste water treatment plants, water from waste disposal sites and waste water treatment plants, air samples, biota samples, soil samples and seepage water from fire fighting training grounds. The results from all samples are presented and discussed in this report. Especially a thanks to University of Umeå for a tremendous job with all work related to development of analytical methods and analysis of the new brominated flame retardants and also to the University of Örebro for analysing the polyfluorinated compounds. In general a special thanks to all which have contributed in this project and especially to: Det Norske Veritas AS (DNV) Tormod Glette, Amund Ulfsnes, Anders Bergslien, Christian Volan, Marte Braathen for field work and logistic, Sam Arne Nøland for verification and control and Gjermund Gravir for GIS related work. Also thanks to Jens Laugesen for support and discussions. Norwegian Geotechnical Institute (NGI) Hans Peter Arp for field work and reporting and Arne Pettersen for logistic. University of Umeå Jenny Rattfelt Nyholm, Roman Grabic and Patrik Andersson for analytical work and reporting. University of Örebro Anna Kärrman and Kristin Elgh-Dalgren for analytical work and reporting. Molab AS Marco Skibnes Venzi for performing the air sampling and reporting. Acknowledgements Thank you to Bård Nordbø at the Climate and Pollution Agency for good co operation and clear communication. Also thanks to all representatives at the different plants included in this screening. Without good will and co operation from all of them this kind of project would be difficult to execute. Høvik, 12 April Thomas Møskeland, Project leader (DNV) 1

3 Content 1. Summary Sammendrag Introduction Flame retardants Brominated Flame Retardants Background Production Environmental release, transport and persistence Toxicity and ecotoxicology Regulations Current levels of BFRs in the Norwegian environment and other parts of the world Shift in focus towards emerging new BFRs Polyfluorinated compounds Background Production Environmental Release, Transport and Persistence Toxicology and ecotoxicology Regulations Environmental levels (published data) Current levels in the Norwegian environment Background and purpose of the study Description of substances included in the screening Newly prioritized brominated flame retardants Polyfluorinated compounds Material and methods Description of sampling sites Drammen area Hokksund area Lillehammer area Tromsø area Bergen area Haugesund area Sampling and sample treatment Drammen area Hokksund area Lillehammer area Tromsø area Haugesund area Bergen area Chemical analysis Brominated flame retardants Polyflourinated compounds

4 6. Results and discussion Brominated flame retardants Polyfluorinated compounds Conclusions Brominated flame retardants (BFRs) Perfluorinated compounds (PFCs) References Appendix I Analytical results Appendix II PNEC values for BFRs Appendix III Description of new BFRs included in the screening Appendix IV Description of PFCs included in the screening

5 1. Summary Det Norske Veritas AS (DNV), the Norwegian Geotechnical Institute (NGI), University of Umeå, University of Örebro and Molab AS have on behalf of the Climate and Pollution Agency carried out the screening survey of "new" brominated flame retardants and selected polyfluorinated compounds in In this study, decabde, 14 new priority brominated flame retardants (BFR), selected polyfluorinated compounds (with focus on PFSAs (PFBS, PFHxS, PFOS, PFDS and 6:2 FTS) were chosen for screening in various samples throughout Norway. Results A summary of the results are presented in the two tables below. Overview of results for the investigated BFRs. +: Detected, O: detected in single replicate and/or very close to detection limit -: not detected Compound Sediment receiving water Sediment waste disposal Sludge waste water facility Waste water Seepage water Biological material Air outdoor Air indoor PBT + o - o PBEB HBB + o o + - BTBPE + o DBDPE o - - DPTE TBPA TBP o ATE TBBPAAE BTBPI EHTBB TBBPA-DBPE o + o - - BEHTBP Overview of results for the investigated PFCs. +: detected, O: detected in single replicate and/or very close to detection limit, -: not detected. Compound Soil Sediment Water Blue mussel Crab Fish liver 6:2 FTS NQ NQ NQ PFBS + o PFHxS PFOS PFDS PFPeA PFHxA o PFHpA PFOA o o PFNA o o + - o + PFDA NQ NQ PFUnDA PFDoDA o + PFTrDA PFTeDA o 3

6 Risk assessment of results In order to assess whether the investigated compounds poses an environmental concern or not some general criteria were used: (i) If the compound was not detected or only detected in samples not taken in the receiving environment it is assessed to be of no or little environmental concern. Included in this category are for example water, sediment and sludge from waste water facilities and waste disposal sites. (ii) If the compound was detected in receiving environment it is assessed as being of moderate environmental concern. This is nuanced based on comparison with limits for negative effects such as predicted no effect concentrations (PNEC). (iii) If the compound was identified in biological material it is automatically assessed as being of environmental concern. Detection of substances in needles is not considered to represent biological material. It s assumed that the pollutants are associated to the waxes on the surface of the needles. In this regards needles are considered as passive samplers. One should be aware that the assessment should be interpreted with care partly because it s based on simple criteria and partly because it is based on few samples for most of the investigated compounds. Conclusions Based on this very general risk assessment the investigated compounds are classified as follows: No or little environmental concern BFRs: Bis(2-ethylhexyl)tetrabromophtalate (TBPH), 2-etylhexyl-2,3,4,5tetrabromobenzoate (EHTBB), 2,4,6-tribromophenylether (ATE), Tetrabromophtalicanhydride (TBPA), 2,3- dibromopropyl-2,4,6-tribromophenyl ether (DPTE) PFCs: None identified Moderate environmental concern BFRs: Hexabromobenzene (HBB), Tetrabromobisphenol A bis(2,3-dibromophenylether) (TBBPA-DBPE), ethylene bis(tetrabromophtalimide) (BTBPI), tetrabromobisphenol A dialyllether (TBBPA-AE), pentabromoethylbenzene (PBEB), pentabromotoulene (PBT) PFCs: Perfluorobutane sulfonate (PFBS) Environmental concern BFRs: 2,4,6-tribromophenol (TBP), decabromodiphenylethane (DBDPE) and 1,2 bis(2,4,6- tribromophenoxy)ethane (BTBPE) PFCs: 1H,1H,2H,2H-tetrahydrofluorooctane sulfonate (6:2 FTS), perfluorooctane sulfonate (PFOS), perfluorodecane sulfonate (PFDS), perfluorohexane sulfonate (PFHxS) 4

7 2. Sammendrag Bakgrunn På vegne av Klima og forurensningsdirektoratet har Det Norske Veritas AS (DNV), Norges Geotekniske Institutt (NGI), Universitetet i Umeå, Universitetet i Örebro og Molab AS gjennomført screeningundersøkelsen av nye bromerte flammehemmere og polyfluorerte forbindelser i I denne studien er decabromodiphenyl eter (decabde,) 14 nye prioriterte bromerte flammehemmere og utvalgte polyfluorerte organiske forbindelser (med hovedfokus på PFBS, PFHxS, PFOS, PFDS og 6:2 FTS) undersøkt i ulike prøvematriser i hele Norge. Det viktigste målet med denne studien er å utvide dagens kunnskap om disse potensielt skadelige stoffene med hensyn til deres forekomst i miljøet, om de utgjør en miljørisiko og om utviklingen over forekomsten i miljøet over tid (overvåking). Dagens kunnskap tilsier at decabde er den vanligste bromerte flammehemmeren og PFOS de vanligste perfluorerte forbindelsen i norsk miljø, og to av forbindelser som gjennomgår en "utfasing". Overvåkning av disse to forbindelsene er viktig i forhold til om utfasing vil føre til lavere konsentrasjoner i miljøet av disse to stoffene fremover. Angående de 14 nye prioriterte bromerte flammehemmerene (BFR) og 6:2 FTS, har forekomsten av disse i norsk miljø ikke vært undersøkt tidligere og kun begrensede mengder data eksisterer i litteraturen på tilstedeværelsen av disse forbindelsene i miljøet. Derfor er det viktig å finne ut om de er tilstede, og hvis de er det om de utgjør en risiko for miljøet. De 14 BFR ble valgt ut av på bakgrunn av en tidligere studie i regi av KLIF (2008) og følgende kriterier ble lagt til grunn: Produksjon volum (HPV eller LPV) Bruk av produktet (additiv, reaktive midler eller polymer) Potensial for langtransport (Long Range Transport - LRT) Bioakkumuleringspotensiale (BAP) Persistens (lite nedbrytbar og kan være i miljøet over lang tid) Miljø nivåer Miljø transportprosesser For å gjøre denne undersøkelsen så meningsfylt og så informativ som mulig er et bredt spekter av miljøprøver tatt på forskjellige steder over hele Norge. Prøvene omfatter sedimenter, vann og slam fra avløpsanlegg, deponier og resipienter, i tillegg til biota (fisk, skjell og krabbe) fra resipienter. Jord og sedimenter har blitt prøvetatt fra brannøvingsfelt. I tillegg er det blitt tatt luftprøver, uteluft fra urbane områder og inneluft fra kontor- og butikklokaler. Resultater En oppsummering av resultatene er presentert tabellene under. 5

8 Oversikt over resultatene for 14 nye bromerte flammhemmere. +: detektert, O: detektert i et replikat og/eller veldig nær deteksjonsgrensen, -: ikke detektert. Forbindelse Sediment resipient Sediment avfalsanlegg Slam renseanlegg avløps vann Sigevann Biologisk materiale Uteluft PBT + o - o PBEB HBB + o o + - BTBPE + o DBDPE o - - DPTE TBPA TBP o ATE TBBPAAE BTBPI EHTBB TBBPA-DBPE o + o - - BEHTBP Inneluft Oversikt over resultatene for polyfluorerte forbindelser. +: detektert, O: detektert i et replikat og/eller veldig nær deteksjonsgrensen, -: ikke detektert. Forbindelse Jord Sediment Vann Blåskjell Krabbe Fiskelever 6:2 FTS NQ NQ NQ PFBS + o PFHxS PFOS PFDS PFPeA PFHxA o PFHpA PFOA o o PFNA o o + - o + PFDA NQ NQ PFUnDA PFDoDA o + PFTrDA PFTeDA o Risikovurdering av resultater For å vurdere om de undersøkte forbindelsene utgjør en miljømessig bekymring eller ikke ble noen generelle kriterier lagt til grunn. Det er ingen til få relevante data på effekt konsentrasjoner (PNEC, NOEC verdier og lignende) for veldig mange av de undersøkte forbindelsene som kan benyttes i den generelle risikovurderingen. Derfor er følgende relativt enkle kriterier brukt: 6

9 (i) Hvis forbindelsen ikke ble detektert i noen prøver eller bare ble detekter i prøver som ikke var tatt i resipientene eller biologisk materiale ble den vurdert å utgjøre ingen til liten miljømessig bekymring. Inkludert i denne kategorien er for eksempel detekterte forbindelser i vann, sediment og slam fra rense- og avfallsanlegg. (ii) Hvis forbindelsen ble detektert i resipientene er den vurdert å utgjøre en moderat miljømessig bekymring. Denne vurderingen er nyansert basert på tilgjengelige grenseverdier for negative effekter (eksempelvis PNEC verdier). (iii) Hvis forbindelsen ble identifisert i biologisk materiale, ble den automatisk vurdert å utgjøre en miljømessig bekymring. Barnåler anses ikke å representere biologisk materiale da det er lagt til grunn at forbindelsene er festet til voks på overflaten av nålene, så her er barnåler betraktet som passive prøvetakere. Det må nevnes at vurderingene bør tolkes med forsiktighet blant annet fordi de er basert på enkle kriterier og dels fordi de er basert på få prøver for de fleste av de undersøkte forbindelsene. Ingen eller liten miljømessig bekymring BFR: Bis(2-ethylhexyl)tetrabromophtalate (TBPH), 2-etylhexyl-2,3,4,5tetrabromobenzoate (EHTBB), 2,4,6-tribromophenylether (ATE), Tetrabromophtalicanhydride (TBPA), 2,3- dibromopropyl-2,4,6-tribromophenyl ether (DPTE) PFC: Ingen identifisert Moderat miljømessig bekymring BFRs: Hexabromobenzene (HBB), Tetrabromobisphenol A bis(2,3-dibromophenylether) (TBBPA-DBPE), ethylene bis(tetrabromophtalimide) (BTBPI), tetrabromobisphenol A dialyllether (TBBPA-AE), pentabromoethylbenzene (PBEB), pentabromotoulene (PBT) PFC: Perfluorobutane sulfonate (PFBS) Miljømessig bekymering BFR: 2,4,6-tribromophenol (TBP), decabromodiphenylethane (DBDPE) and 1,2 bis(2,4,6- tribromophenoxy)ethane (BTBPE) PFC: 1H,1H,2H,2H-tetrahydrofluorooctane sulfonate (6:2 FTS), perfluorooctane sulfonate (PFOS), perfluorodecane sulfonate (PFDS), perfluorohexane sulfonate (PFHxS) 7

10 3. Introduction Worldwide many millions of synthetic chemicals have been identified in the environment. Many of them are a concern from a human health and environmental perspective, as above certain threshold levels they can exhibit toxic effects to humans and organisms as well as deleterious effects to ecosystems. The Norwegian government, represented by the Climate and Pollution Agency (former known as Norwegian Pollution Control Authority), are working systematically to identify chemicals which pose a risk to humans and the environment. Part of this work involves yearly screening investigations of the distribution of selected emerging pollutants in the environment. This report deals with the screening investigation carried out in 2009, where the distribution of 14 new brominated flame retardants(bfrs), 1 legacy BFR, and 5 polyfluorinated compounds (PFCs) where investigated in different environmental compartments throughout Norway. Of special note, two of the chemicals considered in this year s screening investigation are in the process of being phased out in Norway, namely decabrominated diphenyl ether (decabde) and perfluorooctansulfonate (PFOS). Thus, it is of interest to see if their phasing out is being reflected by decreasing concentrations in the environment. 3.1 Flame retardants During the course of the twentieth century, manufactures began to move away from traditional material such as wood and metal towards new, engineered materials used plastics building materials and furniture. Additionally, in the textile industry, engineered textiles with unique properties replaced natural textiles, primarily based on wool and cotton. Many of these new materials were more flammable than the materials they replaced. At the same time there was an increasing emphasis on fire-safety by regulators due to the obvious safety concerns of household appliances, building materials and clothing catching fire. This caused the rapid development of flame retardants and the flame retardant industry, which made safe the use of many of the new materials as well pre-existing materials that society has come to rely on. The basic tasks of flame retardants are to minimise both the chances of ignition and the rate of combustion, ideally without compromising the materials they are being applied to or posing any health risks themselves. There are three major categories of flame retardants: inorganic, organohalogenated and organophosphate compounds. Inorganic flame retardants represent the largest fraction of total flame retardants in use in Europe, organohalogenated flame retardants are most used in other parts of the world, such as Asia. Organohalogenated flame retardants are primarily based on bromine and chlorine. Global consumption figures for 2005 (Fink et al., 2005) are presented in Figure 1. 8

11 Figure 1 Use of various flame retardants in different regions (Fink et al., 2005). Based on this survey, brominated flame retardants are the second most used in the world, and the third most used in Europe. Brominated and chlorinated are in the group organohalogenated flame retardants, aluminium hydroxide and antimony trioxide are in the group inorganic flame retardants and organosphosphorous are one major group. 3.2 Brominated Flame Retardants Background Brominated Flame Retardants (BFRs) comprise a diverse variety of organic compounds, which as their name suggests, are linked by the fact that they contain bromine and are considered commercial flame retardants. Currently, several different types of BFRs exist on the market. Three common molecular-structure categories of BFRs generally assigned are: 1) aromatic, 2) cycloaliphatic and 3) aliphatic; however, there is much more variety amongst BFR structures than these three categories imply. BFRs range in polarity from apolar to ionizable, in size from just a few atoms to macro-molecular, and in reactivity from inert to polymerizing (Andersson et al., 2006, KLIF, 2009a). There are two main economic reasons why such a large variety of BFRs exist on the market. The first reason is that often only very specific BFRs are suitable for fireproofing certain materials (i.e. niche usages), in terms of effectively binding to the material and not influencing the material s commercial properties. The other reason is that many of the initially used BFRs were deemed to have direct impacts on human and environment health (see below) and thus have prompted the use of alternatives. BFRs are designed to be either reactive or additive. Reactive BFRs are chemically bonded to materials or even incorporated as an occasional monomer into the polymeric structure of a plastic. Additive BFRs are only physically-sorbed to the material, either by being adsorbed to the surface or absorbed into the matrix of the material. BFRs are effective flame retardants because when they are heated to combustion temperatures they release bromine radicals, which catalytically bind hydrogen and hydroxyl radicals in the combustion gas, forming water that dilutes the combustion gas and preventing 9

12 hydroxyl radicals from participating in further combustive reactions. This is the same principle also of other halogenated flame retardants; however, fluorine and chlorine radicals are generally not as economically effective (in terms of cost and amount of chemical needed) in this reaction as bromine radicals released from BFRs Production BFRs were first used commercially in 1965 (Vonderheide et al., 2008). Their production dramatically increased since then due to the continuous discovery of new, specific uses for individual BFRs, and especially upon the ban of polychlorinated biphenyls (PCBs) in the late 1970s - early 1980s as BFRs were a suitable replacement (Vonderheide et al., 2008). Though many different BFRs were being manufactured, the first generation of BFRs to be produced on a massive scale consisted of polybrominated diphenyl ethers (PBDEs), polybrominated biphenyls (PBBs), tetrabromobisphenol A (TBBPA) and hexabromocyclododecane (HBCD). Of these, only TBBPA was used as a reactive, chemically binding BFR, and the rest were left to absorb and adsorb to the materials. The BFRs PBDE, HBCD, TBBPA and PBB are here referred to as legacy BFRs. It is worth noting that other BFRs were produced in the 1970s and 1980s too, however, not to the same massive scale as the legacy BFRs Environmental release, transport and persistence One of the first reported environmental disasters related to these compounds was when a BFR mixture called Firemaster TM, comprised mainly of hexabrominated-biphenyl (a PBB), was accidentally mixed into animal feed in 1974, causing diverse harmful effects to livestock as well as exposure to humans of contaminated food (WHO, 1994). As the 1990s progressed, when global production of BFRs exceeded metric tons/year (de Wit, 2002) the presence of BFRs in the environment became a rapidly increasing concern. Globally, many BFRs were found to be leaking in trace amounts from the products they were applied to. At hot spots, such as landfills of electric waste, elevated and even toxic concentrations of BFRs are commonly found in leachate and nearby water supplies (e.g. Leung et al., 2007). Not only in hotspots are BFRs a concern. Like many industrially produced organohalogenated compounds (such as PCBs and many pesticides), BFRs can be found in elevated concentrations within biota and environmental samples in remote locations, far from any sources, where they can potentially exhibit toxic effects. This phenomenon of organic chemicals being transported long distances in the environment is referred to as Long Range Transport (LRT). In order for a molecule to exhibit LRT, it has to a) be persistent in the environment (i.e. resistant to transformation reactions when exposed to the environment), and b) be able to be transported spontaneously by environmental mechanisms (e.g. wind transport, water currents, etc.). Whether or not a molecule is transported in the environment depends on if it has the right range of physical-chemical properties that allow it to volatilize, as well as adsorb or absorb to various, mobile environmental media. For instance, small organohalogenated compounds, such as methylene bromide, are quite volatile and thus can spread in the environment as a vapour in the atmosphere. Polar compounds, (e.g. bromophenols) are soluble in water, and thus can readily be transported by water currents. Very large, apolar compounds (e.g. decabde) are very insoluble in water and usually exhibit low volatility, and thus such compounds are not transported in water substantially as a dissolved molecule, nor in the air as a vapour. However, such molecules can nevertheless be transported within air and water by sorbing to aerosols and suspended sediments that are transported in air and water, as well as into organisms. If the molecules have a particular high affinity for lipids and proteins in 10

13 biota compared to the surrounding medium, it is common to find elevated amounts of these molecules in biota, despite lack of detection in the surrounding medium (a phenomena referred to as bioaccumulation). Transport in the environment can also be facilitated through the food chain, such as from algae to fish to bird (a process referred to as biomagnifications). Why BFRs and other organohalogens are environmental persistent is largely due to the strong nature of carbon-halogen bonds. Breaking these bonds requires a relatively substantial amount of energy, compared to what is available under ambient conditions, and thus they occur only very slowly in the environment. Nevertheless they do occur in the environment and at appreciable levels, such as by photolytic and biological degradation pathways (La Guardia et al., 2007). These reactions typically involve the parent BFR being debrominated or oxidized into another brominated compound. As an example decabde can degrade into other, less brominated PBDEs (e.g. La Guardia et al., 2007; Schenker et al., 2008b). This example is particularly important, as the presence of decabde itself in the environment is generally argued to be benign (as current research indicates it exhibits low toxicity), the formation of ecotoxic daughter products has caused concern regarding the presence of this chemical in the environment Toxicity and ecotoxicology There has been a lot of research studying the toxicity of legacy BFRs in humans, wildlife and ecosystems. Here a main summary of some reviews on the subject (e.g. Darnerud, 2003; de Wit, 2002; Hites, 2004) which have collectively set the framework for ongoing research will be given. Initially, most studies were available for PBBs and PBDEs. Key findings for these molecules were that different congeners (both PBBs and PBDEs consist of 209 individual molecules each) seem to be more toxic than others. For instance, pentabromodiphenylethers (pentabdes) seem to be substantially more toxic at the low concentrations than decabde at much higher concentrations. This is poignant, as many initial PBDE commercial mixtures contained an abundance of pentabdes. Well-known toxic effects are related to endocrine disruption, particularly in the thyroid and in immunological hormones, which causes impairments in growth, neuro-development and reproductive development to a broad array of organisms including humans. Toxic effects on kidneys and livers have also been identified and studied, as well as carcinogenesis and harmful mutagenetic and epigenetic influences. Overall, there seems to be a clear cut case for concern of the presence of tetra- to nonabrominated PBDEs in the environment, as at measured environmental concentrations, toxic and ecotoxicological effects are possible (and very likely occur at hot spots). Based on research so far, decabde, HBCD and TBBPA appear to be relatively benign at current environmental concentration levels, compared to PBB and less brominated PBDE. However, this is not totally verified yet, and it does not apply to degradation products of these compounds, especially for decabde, which as stated earlier, can debrominate to form more toxic daughter products. Toxicological and ecotoxicological studies in this areas have flourished in the past years, though still knowledge gaps exist, and identifying safe exposure levels of these compounds is still a focus of active research. Toxicological studies on the new BFRs, such as analysed in this study, is only just emerging Regulations As a consequence of BFRs possibly having potential deleterious effects to ecosystems and to humans, many governments along with industry decided to ban or phase out certain BFRs of high risk. The first BFR to experience industrial phase-out were PBBs (prompted by the Firemaster TM incident mentioned earlier), which co-occurred with bans of PCBs during the 11

14 late 1970s and early 1980s (WHO, 1994). Starting at around 2003, a wave of bans in many countries on pentabde mix and octabde mix (mixtures of BDEs dominated by pentabromodiphenyl ethers and octobromodiphenylethers, respectively) emerged. The European Union banned these chemicals in 2003 (EU, 2003) and in 2009 these were included in the priority list by the United Nation s Environment Program s Stockholm Convention on Persistent Organic Pollutants (UNEP, 2009). Since the beginning of the century and until the present day, the BFRs that are by far the most commonly produced in Europe are decabde, TBBPA and HBCD. Figures from 2003 show that these chemicals are being produced in 56418, and metric tonnes/year (Andersson et al., 2006). Estimated emissions of these BFRs in Norway are presented in Figure 2 (KLIF, 2009b, see for Norwegian regulations) Figure Emission levels of BFRs in Norway Current levels of BFRs in the Norwegian environment and other parts of the world In recent years, KLIF has done several recent screening of the presence of legacy BFRs in diverse environmental samples in Norway (e.g. KLIF, 2004, 2005a, 2007a, 2008c). A review of previous investigations and studies of levels of PBDE in Norway was recently compiled (KLIF, 2008c), and is summarized here. Regarding air levels (vapour and particles), ΣPBDE can range from pg/m 3, with the decabde being the dominant component. In soils and mosses decabde is also the dominant component, with levels ranging up to 4.4 ng/g d.w in soils and 9 ng/g d.w in mosses. Water samples, mainly from the Mjøsa region, were reported to range from 19 to 820 pg/l, again with decabde being the most common (note, these levels are relatively high). In fresh and salt water sediments, decabde too is the most dominating compound, with levels up to the µg/g d.w range. A sediment core in Oslo harbor (sampled 2006) reported concentrations that penta-mix, octa-mix BDEs and HBCD are decreasing, and that concentrations of decabde are increasing (KLIF, 2008b). Correspondingly, decabde is also the most dominating PBDE reported in landfill and sewage sludge samples (though lighter weight PBDEs are typically found in leachate). In biota, such as fish and birds, however, this dominance of decabde is not reflected, as biota in general appears to be 12

15 contaminated with various levels of diverse BDEs. Although decabde is expected to be strongly attached to soil and sediments and therefore was not expected to bio accumulate, investigations have shown that also decabde bio accumulates. There are several reviews of the emission, distribution and environmental occurrence of legacy BFRs throughout the world, though by far the most amounts of data exists for the Arctic, Europe and Japan (de Wit, 2002; Law et al., 2008; Watanabe and Sakai, 2003). More data has appeared in recent years for China, though to our knowledge no review of this data has been performed yet. Compound class specific reviews on environmental levels were done for PBDE (Hites, 2004; Vonderheide et al., 2008), HBCD (Covaci et al., 2006), and TBBPA (Covaci et al., 2009). General observations that can be made from screens carried out in Norway (from the previous KLIF reviews), Europe and Japan is that concentrations of decabde and HBCD are increasing in biota and environmental samples, whereas levels of pentabde and octabde are decreasing (e.g KLIF, 2008c; Law et al., 2008; Minh et al., 2007; Covaci et al., 2006). Overall, trends in regulation and industry production do seem to be reflected with corresponding changes in environmental concentrations, particularly in sediment and biota. Unsurprisingly, levels of all BFRs are higher nearest source zones in all media (air, soil, sediment and biota). There is little doubt that PBDEs and HBCD are capable of rapid LRT and biomagnification (Breivik et al., 2006; Covaci et al., 2006; Hites, 2004). Levels of TBBPA are lower and are not commonly present in environmental samples outside of local source zones (e.g. production facilities, Covaci et al., 2009). The biggest uncertainties and concerns commonly brought up in these investigations are 1) little data is still available for transformation products as well as transformation pathways of decabde, TBBPA and HBCD, thus there is not enough evidence yet to conclude that generally benign concentrations in certain environments are not an issue (particularly for decabde); 2) more knowledge is needed on identifying specific uptake pathway mechanisms in various organisms (e.g. food chain, ingestion, breathing, lipid partitioning, membrane diffusion, etc) in order to make more realistic risk assessments; and 3) more data is needed on emerging BFRs Shift in focus towards emerging new BFRs Based on the information above, of the three contemporary mass-produced BDEs, decabde is generating the most concern. Increasing regulations are being enforced, mainly because decabde is often the most abundant BFR present in the environment and there are concerns of its degradation products. In 2008 Norway banned decabde, while Sweden, Canada and parts of the USA proposed strict regulations on what it can be used for (KLIF, 2008a; Vonderheide et al., 2008). Currently, there is some momentum in Norway and other countries to take a tighter regulatory line on TBBPA and HBCD (KLIF, 2009b, see also Though the possibility of increasingly stringent regulations on decabde, HBCD and TBBPA is being highly contested, especially by the BFR industry who argue these chemicals are relatively benign to the environment ( and ). This trend is invariably putting pressure on industry to find alternatives, such as other BFRs that can be demonstrated to exhibit less potentially harmful environmental consequences. Four methods of approach by the industry for finding alternatives include the development of BFRs that 1) is itself benign and is rapidly degraded in the environment to benign, irrelevant 13

16 fragments (such as Br-salts or other benign Br-fragments), 2) bind additively chemically to materials, like TBBPA or stronger, 3) be so hydrophobic and persistent that they will be even less soluble and volatile than existing BFRs (e.g. stable brominated polymers), 4) some combination of the above. A less sustainable approach, but another one that may be economically favorable in the short term, is to choose a random BFR in which little is known, but currently does not happen to fall onto the radar of scientists and regulators. Because of regulatory and commercial pressures, studies are now focusing on identifying new BFRs in the environment, including degradation products of legacy BFRs. 3.3 Polyfluorinated compounds Background Polyfluorinated compounds (PFCs) are a large group of chemicals that consist of a perfluorinated alkyl tail (i.e. an alkyl-chain in which all hydrogens are replaced with fluorines) with an organic functional group at one end. The general formula for these compounds is F(CF 2 ) x R. Two important subsets of PFCs exist, perfluoroalkyl compounds in which the head group contains no C-H bonds and fluorotelomer (FT) compounds in which the R-group contains an even-numbed alkyl-chain (general formula F(CF 2 ) x (CH 2 -CH 2 ) y R and F(CF 2 ) x (CH=CH) y R). In industry, these molecules are commonly used as building blocks to form fluorinated polymers (i.e. perfluoralkylpolymers), which are PFC monomers linked by a hydrocarbon backbone. Note that fluorinated polymers are different than the more commonly known fluoropolymers, such as polytetrafluoroethylene (i.e. Teflon TM ), though certain PFCs are used to assist in the manufacturing process of fluoropolymers and thus may appear as residues. PFC-generated fluoropolymers are used as additives for a vast array of materials to either lower their surface tension (e.g. in hydraulic fluids, photographic emulsifiers and paints), or as a coating to make materials more stain and water repellent (e.g. in carpets, textiles, adhesives). A unique and important application is specialised aqueous film forming foams (AFFFs) to extinguish oil and jet fuel fires, as PFCs, being powerful surfactants, can facilitate mixture of water and oil, thus facilitating flame extinguishment and eliminating the dispersion of burning oils. As in the case of BFRs, PFCs concentrations in environmental samples have been found to be increasing and are ubiquitous in the environment, and several toxic effects have been identified. This has caused increased regulations, as well as changes in industrial production. Of the various PFCs, there are two types that have been the most utilized by industry, and have attracted the most attention and concern in recent years. These are the perfluorocarboxylic acids (PFCAs) (general formula F(CF 2 ) x COOH) and perfluorosulfonic acids (PFSAs) (F(CF 2 ) x S(O 3 )H). These acids are readily ionized, and also exist in negatively 14

17 charged ions (by the loss of the proton) or a salt, referred to perfluorocarboxylates and perfluorosulfonates, respectively. Of these two types of PFCs, two individual molecules have attracted the most environmental concern: perfluorooctanoic acid (PFOA, F(CF2) 7 COOH) and perfluorooctosulfonic acids (PFOS, F(CF 2 ) 8 S(O 3 )H) Production PFCs were first produced in 1946, though mass production did not begin until the 1960s and 1970s, when they became more commonly used as additives in AFFFs and other products (Stock et al., 2010). The most abundantly produced chemicals were clearly PFCAs and the precursor to PFSAs, PSFs (perfluorosulfonyl fluorides, general formula F(CF 2 ) x S(O 3 )F). The two individual molecules that were the most abundantly produced were PFOA and POSF (perfluorooctane sulfonyl, F(CF 2 ) 8 S(O 3 )F). POSF was used to make PFOS and other products, for conversion to PFOS, simply the fluorine on the -S(O 3 )F group was cleaved (Paul et al., 2009; Prevedouros et al., 2006). Though PFOA and POSF were the most predominately produced PFCAs, PFSs and PFSAs of other chain lengths were generated in substantial quantities. Production of these molecules peaked around the year 2000, when the company 3M announced that it was phasing out POSF-based products. At this peak, global POSF emissions are estimated at 4500 tonnes / year (Paul et al., 2009), and PFOA based products at over 300 tonnes/year (Prevedouros et al., 2006). By , 3M phased out production of POSF products, and global production levels fell. Estimates for POSF in 2005 are circa 1000 tonnes/year, mainly due to ongoing production in Asia (Paul et al., 2009). In western countries, production of butyl PFCA and PFSA (perfluorobutylcarboxylic acid and perfluorobutylsulfonic acid) have increased, as they are currently thought to be less toxic than PFOA, PFOS, and other long-chain PFCAs and PFSAs (Renner, 2006; Stock et al., 2010). 15

18 Figure 3 Production volumes (tonnes/year) of various perfluorinated products, including perfluorooctane sulfonyl (POSF, the main precursor to PFOS), perfluorooctanoic acid, perfluorononanoic acid, and fluorotelomer products (Paul et al., 2009; Prevedouros et al., 2006). POSF experienced a massive drop in production in the year 2000 when it was phased out by 3M, though production continues in Asia. PFCA products were not as produced on the same scale as POSF, though fluorotelomers were, which degrade to PFSAs and PFCAs in the environment. Little data is available for production in recent years, but it is widely speculated smaller chain POSF and PFCA production has increased substantially (Renner, 2006; Stock et al., 2010) Environmental Release, Transport and Persistence PFCs, particularly PFCA and PFSA, have shown to be exhibit both persistence and LRT (long range transport) in the environment, as confirmed by their ubiquitous presence in environmental samples (Stock et al., 2010). However, the mechanisms of how these chemicals are transported in the environment have eluded scientists, as PFCs have completely different chemical properties than many of the previous chemicals to which environmental persistence and LRT models have been developed for. As opposed to being hydrophobic apolar compounds (like BFRs and PCBs), these compounds are ionic, strong acid, surfactants. The pka (or acid-dissociation constant) of these compounds is estimated to be near 0 for PFCAs and around -3 for PFSA (Campbell et al., 2009; Goss, 2008). As far as their surfactant properties are concerned, these compounds are amongst some of the most powerful surfactants known. The perfluoralkyl tail is one of the most hydrophobic molecular fragments possible, similarly the anionic/acid functional groups (CO 2 -, SO 3 - ) are some of the most hydrophilic functional groups known. As a result, PFCAs and PFSA have a strong affinity for water surfaces, with the hydrophilic head group liking to be in water whereas the rest of the molecule prefers being outside of the water. These molecules are therefore likely to be transported substantially in the environment by water surfaces (e.g. by dispersion on lake surfaces, sorption to clouds and rain droplets), as has been debated and discussed in the recent literature (Arp and Goss, 2009; Goss and Arp, 2009). The uniqueness of PFC s chemical properties and what they mean for environmental transport remains an active area of research. Key findings in this direction are that PFCA and PFAS are readily water soluble at low concentrations, form aggregates and micelles at higher concentrations (Arp and Goss, 2009; Cheng et al., 2009), and in the environment associate at interfaces (Psillakis et al., 2009), sorb somewhat but not readily to soils-water and sediment-water interfaces (Higgins 16

19 and Luthy, 2006, 2007), and in biota prefer sorption to proteins than to lipids (Stock et al., 2010), and are transferred into biota by bioaccumulation and biomagnification (Stock et al., 2010). We note here that knowledge of both physical-chemical parameters and environmental transport pathways are only recently starting to be understood. Thus, reference to hypothesis and physical-chemical data for these compounds from a few years ago can look quite different from what is emerging in the literature today; hence, several statements have been made in the previous paragraph that may appear in contrast to earlier KLIF reports (e.g. in KLIF, 2007b). To deal with the unique environmental transport and partitioning processes, researchers need an additional set of physical-chemical parameters and models to account for the ionic and surfactant nature of these compounds, such as the pka (the acid-dissociation constant), surface-water sorption coefficients, and the critical micelle and aggregate-formation concentrations. Though, parameters that are also necessary for apolar, neutral compounds (like the BFRs looked at) are also relevant. Some of these relevant physical-chemical parameters for compounds considered in this screening are provided in Chapter 4, though most parameters remain unknown. Regarding the persistence of PFC, based on the strong nature of the carbon fluorine bond (the strongest bonds possible in organic molecules), these compounds are extremely resilient to environmental transformations. It appears that the most stable of all PFCs in the environment are PFCAs and PFSAs, which may even be regarded as environmental transformational end products. This is said not only because they are extremely stable (to our knowledge, degradation of these compounds in the environment or under ambient conditions has yet to be observed; though, slow, immeasurable degradation is likely occurring), but also because all other PFCs that have been manufactured appear to be transformed to PFCAs and PFSAs in the atmosphere and elsewhere in the environment (Armitage et al., 2009b; Schenker et al., 2008a; Wallington et al., 2006). The two classes of PFCs that are considered the most substantial precursors of PFCAs and PFSAs are fluorotelomer alcohols (FTOHs) and fluorotelomer sulfonaminds (FSAs) and fluorotelomer sulphonic acids (FTS); however, several hundreds of manufactured PFCs are considered to be capable of conversion into PFCAs and PFSAs (Stock et al., 2010). As a result, the presence of PFCAs and PFSAs are not only due to direct emissions of these compounds, but are also due to indirect transformation of many other PFCs. As a result, multimedia models that account for the occurrence of these molecules consider both these direct and indirect sources of PFCAs and PFSAs (e.g. Armitage et al., 2009a; Armitage et al., 2009b; Schenker et al., 2008a; Wania, 2007) Toxicology and ecotoxicology Most of the toxicological studies of PFCs have focussed specifically on PFOA and PFOS, and are only recently being expanded to other PFCs. Selected findings reported in recent reviews (Lau et al., 2007; Lau et al., 2004) will be summarised here. For the majority of organisms tested, PFOA and PFSA seem to be readily absorbed through oral pathways (ingestion, breathing), and poorly eliminated. The general explanation for this is that they are not metabolized substantially (due to their stability), and tend to accumulate in the liver, blood serum and kidney; likely because they bind to certain proteins, such as β-lipoproteins, albumin and liver fatty acid binding proteins (and not because they accumulate in lipids). 17

20 These compounds have also been identified as peroxisome proliferators, which can lead to a variety of toxicological effects to the liver, including carcinomas. PFOS and PFOA have also been found to inhibit cell growth by inhibiting intercellular communication, which can lead to cancer growth. Chronic toxicity studies have linked PFOA exposure to tumours in rats and other organisms (though a carcinogenic link has yet to be proven for humans) (Rosen et al., 2009). Recently, PFOA and PFOS have also been found to be endocrine disruptors in humans, being able to compete with thyroxin to the human thyroid hormone transport protein transthyretin (Weiss et al., 2009). In general, it appears from evidence so far that longer chain PFOA and PFAS are much more toxic than shorter chained ones PFCA and PFAS, which has prompted a recent shift in industry to favouring more shorter-chain molecules such as PFButS (Renner, 2006). It should be noted here that one of the molecules considered in this investigation is a fluorotelomer sulphonic acid (FTS), namely 1H,1H,2H,2Htetrahydroperfluorooctane sulfonate (6:2 FTS, aka THPFOS). Little toxicological information exists for these molecules, however, in the case of telomere-carboxylic acids it has been argued that these are more toxic than PFCAs (Phillips et al., 2007). In the Norwegian regulation of classification, labelling of dangerous chemicals PFOS is classified as posing a danger for development of cancer, may cause damage to foetus, dangerous by inhalation or contact to the skin, poisonous: severe danger to health by long term influence by swallowing, hazardous to children getting breast milk, poisonous to water living organisms and may cause negative long term effects in water. There also exists a suggestion for classification of PFOA in the EU (after initiative from KLIF): posing a danger for development of cancer, poisonous: severe danger to health by long term influence by inhalation and swallowing, dangerous if inhaled or swallowed and eye irritating Regulations The ubiquitous occurrence and toxicity of PFOS and PFOA has led to an increasing number of governmental regulations, ranging from maximum tolerable intake values, to manufacturing restrictions to outright bans. The U.S. EPA provides a webpage that tabulates recent regulatory developments within the U.S. and elsewhere ( and Norwegian Climate and Pollution Control Authority keep an updated webpage of their action plan of these chemicals ( Key regulations regarding PFOS, is that United Nation s Stockholm Convention on persistent organic pollutants classified it on their list of persistent organic pollutants (UNEP, 2009). It was banned outright (manufacture, use, sale) in Canada in 2008 (Canada, 2008). The EU has set maximum allowable human intake values and maximum values allowed in market goods (EFSA, 2008; EU, 2006), and the U.S. has set maximum tolerable concentration in drinking water (0.2 µg/l for PFOS). In 2005, Norway has set a goal to phase out or severely reduce emissions of PFOS by 2010, and has banned them in AFFFs, textiles and preservatives (KLIF, 2005b, 2008e). In Norway a ban of PFOS and PFOS related compounds in textiles, impregnation compounds and fire foam is given by law trough the regulations relating to restrictions on the manufacture, import, export, sale and use of chemicals and other products hazardous to health and the environment (Product Regulations). 18

21 Regarding PFOA, the U.S. EPA launched in 2006 a campaign to achieve a 95% reduction in PFOA in 2010 compared to the 2000 baseline (EPA, 2006) as well as regulated the maximum drinking water concentration to 0.4 µg/l (EPA, 2009). The EU has established guidelines for maximum allowable human intake values (EFSA, 2008). Norway has set a goal to severely reduce or eliminate PFOA emissions by 2010, with completely eliminating them by 2020, and is reviewing a ban in certain consumer products (KLIF, 2005b, 2007b, 2008e) Environmental levels (published data) Studies can be found that have looked at PFCA levels worldwide in diverse environmental matrices, biota (including wildlife) and humans. A review of the various trends can be found by Stock et al. (Stock et al., 2010), with key ranges summarized here. Keep in mind these levels reflect the ubiquitous presence of these compounds in the environment, and are not only confined to hotspots. Individual PFCs are generally found in the air between <0.1 pg/m 3-1 ng/m 3, in precipitation between <0.1 ng/l 100 ng/l, in groundwater near air force bases (where AFFFs are applied) between undectable to 100 mg/l, in surface water between <1 ng/l 1 µg/l, and in surface sediments <0.1 ng 100 ng/l. In wildlife, generally PFOS is the most dominant species, with values ranging from <1 36 µg/g w.w, opposed to PFOA which is generally << 20 µg/g w.w. Currently, one of the most intriguing elements of environmental exposure limits is whether reductions of emissions of PFOS are manifested in reduced amounts in arctic wildlife. Some reports states that there is a correlation between emission reductions and wildlife concentrations (Butt et al., 2007; Hart et al., 2009), and others are reporting the opposite trend (Bossi et al., 2005; Dietz et al., 2008; Holmstrom et al., 2005). One modelling study on this concluded this noticeable response to reduction emission in wildlife concentration will take several years to manifest; however, this was unable to be definitely concluded, due to uncertainties about the exact mechanisms of environmental transport and bioaccumulation pathways (Armitage et al., 2009b). Thus, to best understand what influence the decreasing emissions and increasing regulations are having on PFCA levels, further monitoring of PFCA levels in the environment and more screening studies, such as this one, are needed Current levels in the Norwegian environment In Norway, KLIF has commissioned several screens of perfluorinated compounds, primarily PFCAs and PFOS, in diverse environmental and biota samples in 2004 (KLIF, 2005a), 2006 (KLIF, 2007a), and has done literature reviews studies compiling all data and reports on (KLIF, 2008c). In air samples the most prevalent compounds are PFOS ( pg/m 3 ), PFOA and PFBA (0 4 pg/m 3 ), and the precursor 8:2 FTOH (8:2 fluorotelomer alcohol) gave high readings in Oslo (10 60 pg/m 3 ). In water samples, PFOS and PFOA levels ranged from and 5 8 ng/l, respectively. In fresh water sediments PFOS was found in most samples ( ng/g d.w), PFOA is only found sporadically (up to 1 ng/g d.w), as well as other PFCAs and PFSAs. A study in Oslo harbour found PFOS and PFDS most abundant in surface sediments, with levels between ng/g d.w. In salt water sediment samples, PFOS was also most abundant, with concentrations ranging from ng/g d.w. Other PFCA and PFAS seemed only sporadically present. 19

22 In shell fish most total analysed PFC concentrations were over 1 ng/g dw with PFOS and the PFOS precursor PFOSA (perfluorooctane sulfonamide) being the most dominant. In crustaceans, PFOS ranged from 1 10 ng/g d.w, and various PFCAs were found (with the most abundant being PFUnA, perfluoroundecanoic acid, at levels up to 2.5 ng/g d.w). In both fresh water and salt water fish, PFOS was clearly the most abundant, with levels ranging from up to 57 ng/g w.w and various PFCA and PFOSA could often be spotted (with individual concentrations generally << 10 ng/g d.w). In fish, the concentrations were greater in the liver than in whole fish samples. In birds, PFOS was the most dominant by far, with concentrations in plasma and livers being on the order of 100 ng/g w.w. Regarding human samples in Norway, plasma levels of females were measured and were found to be highest in PFOS and PFOA, with median levels around 3.7 and 15.5 ng/g w.w in two subsequent studies for PFOS, and 6.8 and 2.3 ng/g w.w for PFOA. Regarding potential hotspots in Norway, in landfill effluents PFOS, PFHxsS (perfluorohexanoic sulfonate) and PFOA are the most abundant, ranging ng/l, ng/l and ng/l respectively. In landfill sediments, PFOS and PFHxS were the most commonly measured, with concentrations of ng/g d.w and ng/g d.w respectively. PFOA was found in some samples (< 10 ng/g d.w). In waste water treatment plants, PFOS was quantified in all sewage samples ( ng/l), and PFOA was found in high concentrations in some samples (up to 17 ng/l). Similar findings were for effluent, in that PFOS was generally found in all samples (1 18 ng/l), whereas PFOA and PFHexA was found only sporadically but in comparable concentrations when found (up to 22 ng/l). Sludge samples had lower concentrations than sewage samples, with PFOS and PFOA concentrations around 0.5 ng/l with trace amounts of other PFCAs. In storm water samples, PFOS was the only analyte commonly found. The largest hotspots in Norway are most likely fire training facilities at airports and oil facilities, due to usage of AFFFs (KLIF, 2008d). Soils from Norwegian fire training facilities are contaminated with a variety of PFCs, though usually most with PFOS (with concentrations often > 5 µg/g d.w near the source, the highest was 48 µg/g at a ditch near Rygge airport), about times higher than levels found in sewage sludge. PFCs from these facilities were also found to leach vertically into the groundwater, and to spread horizontally, with soils 70 m away from the training facilities being 7-8 times higher than the background concentration. Groundwater and stream water concentrations at these sights were also elevated, and were amongst the highest groundwater concentrations ever reported for these compounds at the time (concentration PFOS 2-69 ng/l, sum ng/l), again orders of magnitude higher than levels found in sewage effluent water. These elevated concentrations were also evident in sediment and biota near the facilities. Despite it s likely that these sites are amongst the most PFC contaminated sites in Norway, these nearby areas are low to moderately polluted according to existing risk-criteria set by KLIF (KLIF, 2007c, 2009c). Sediment levels fit into the Good criteria, the most concentrated water levels fit into the Moderate category (i.e. chronic in terms of long term exposure), and only some of the soils had concentrations that went above the normal value maximum of 20 µg/g d.w. Similarly for organisms analysed (earth worms, molluscs), the concentrations of the organisms were in the lower range of exposure to toxic risk, based on the approaches used in the report (KLIF, 2008d). As is evident from this brief overview of the presence of perfluorinated compounds in Norway, PFOS is clearly the most abundant, both in terms of frequency of where it is found and concentration, followed by other PFCs, particularly PFHexS and PFOA. 20

23 3.4 Background and purpose of the study In this study, decabde, 14 new priority BFRs, 4 PFSAs (PFBS, PFHxS, PFOS, PFDS) and one FTS (6:2 FTS) were chosen for screening in various samples throughout Norway. The main the goal of this study is to expand current knowledge of these potentially harmful substances with respect to their occurrence in the environment and possible temporal trends. decabde and PFOS are the most abundant BFRs and PFCs in the Norwegian environment, respectively, and two of the compounds that are undergoing a phase-out transition. Carefully monitoring their presence is important with respect to if stricter regulations will cause lower environmental concentrations of these two substances. Regarding the 14 new priority BFRs and 6:2 FTS, these chemicals have never been selectively screened for in Norway, and only limited data on the presence of these compounds is available in the literature. Therefore it s important to identify if they are present and if they they are a concern. The 14 BFRs were prioritised in an earlier study that assessed which new BFRs could be present in Norway at a substantial level, and were selected from a list of known, manufactured BFRs, based on the following criteria: Production volume (HPV or LPV) Product usage (additive, reactive intermediate or polymer) Long range transport potential (LRT potential) Bioaccumulation potential (BAP) Persistence Environmental levels Environmental transport processes In a screening investigation a wide range of environmental compartments in different places throughout Norway is sampled. Many of the sampled locations are considered to be hot spots meaning that the probability of detecting the compounds here is considered to be relatively high. The samples include sediments, water and sludge from waste water facilities, waste disposal sites and receiving waters, as well as biota from receiving waters and land. Additionally, air samples have been taken, including urban air and indoor air. The localities are located in eastern, western and northern parts of Norway (more details can be found in Chapter 5). 21

24 4. Description of substances included in the screening 4.1 Newly prioritized brominated flame retardants A detailed description for the 14 new BFRs are given in Appendix III, by reproducing information given on these compounds in an earlier report (KLIF, 2009). A summary of the structures looked at is presented in the following figure (note that TBB is also referred to as EHTBB): 22

25 4.2 Polyfluorinated compounds The PFCs looked in this screening include PFSAs of various chain-length and 6:2 FTS. Some introductory information of these particular compounds was provided in Chapter 3.3 and references therein. A summary of the structures within the scope of this screening is presented in the figure below. In addition other PFSAs has been included when presenting the results. A more detailed description of the compounds is presented in Appendix IV. 23

26 5. Material and methods 5.1 Description of sampling sites One of the purposes of a screening investigation is to sample several environmental matrices with a wide geographical distribution and at locations where it s expected to find the compounds investigated (hot spots). A general program was worked out by KLIF stating that samples should cover different environmental matrices from eastern, western and northern parts of Norway. Regarding waste water treatment plants they should have different cleaning technologies (mechanical, chemical and biological) in order to see if this had any consequences for the results. Therefore, samples have been collected from waste water treatment plants, waste disposal sites, recycling plants, receiving water, biota and air. The samples have been taken from the eastern, western and northern part of Norway. An overview of the sampling localities and the matrices are presented in the table below. Table 1 Summary of samples; main area, sampling location, sample category and sample matrices. Area Station Category Matrix Analyses Drammen Solumstrand RA water treatment plant water BFR Drammen Solumstrand RA water treatment plant sludge BFR Drammen Drammensfjord receiving water sediment BFR Drammen Drammensfjord receiving water blue mussel BFR Drammen Drammensfjord receiving water fish liver BFR Drammen Drammensfjord receiving water crab BFR Drammen Lindum Ressurs og waste disposal site water BFR Gjenvinning Drammen Lindum Ressurs og waste disposal site sediment BFR Gjenvinning Drammen Drammen city city urban air BFR Drammen Elkjøp shop/store indoor air BFR Drammen/Hurum Hurum Energigjenvinning incineration of waste moss BFR Drammen/Hurum Hurum Energigjenvinning incineration of waste pine needle BFR Hokksund Hellik Teigen AS metal recycling water BFR facility Hokksund Hellik Teigen AS metal recycling sediment BFR facility Lillehammer Lillehammer RA water treatment plant water BFR Lillehammer Lillehammer RA water treatment plant sludge BFR Lillehammer Mjøsa receiving water sediment BFR Lillehammer Mjøsa receiving water fish liver BFR Lillehammer Losna receiving water (stream) sediment BFR Tromsø Langnes RA water treatment plant water BFR Tromsø Langnes RA water treatment plant sludge BFR Tromsø Sandnessundet receiving water sediment BFR Tromsø Sandnessundet receiving water blue mussel BFR Tromsø Sandnessundet receiving water fish liver BFR Tromsø Sandnessundet receiving water crab BFR Bergen Puddefjorden receiving water fish liver BFR Haugesund RES-Q fire fighting facility water PFC Haugesund RES-Q fire fighting facility sediment PFC Haugesund Bleivika receiving water sediment PFC Haugesund Bleivika receiving water fish liver PFC Haugesund Bleivika receiving water blue mussel PFC 24

27 Table 1 continues Haugesund Bleivika receiving water crab PFC Bergen Flesland airport Airport/ fire fighting water PFC facility Bergen Flesland airport Airport/ fire fighting soil PFC facility Bergen Langavatnet receiving water sediment PFC Bergen Langavatnet receiving water fish liver PFC Bergen Flesland brygge receiving water blue mussel PFC Bergen Flesland brygge receiving water crab PFC Drammen area A detailed description of the sampling sites is given below. Solumstrand RA Solumstrand waste water treatment plant is located in Drammen municipality and receives waste water from large areas of Drammen such as Bragernes, Konnerud, Strømsø, Fjell, Tangen, Nøsted and Solum. Waste water that is not going to Solumstrand is led to Muusøya waste water treatment plant. Solumstrand mainly receives water from households (about 70 %). About 30 % of the waste water that passes trough Solumstrand is mainly from the industry, but the plant also receives waste water from Lindum waste disposal site and a hospital (Buskerud HF). Waste water is treated chemically and the cleaning process can be divided as follows: grid, sand- and fat trap, flocculation and sedimentation. The sludge is dewatered by use of centrifuge. In 2009 the plant treated a water volume of about 8.95 millions m 3. The plant is dimensioned for about PE (population equivalent) and a maximum water volume of 3000 m 3 /h. Retention time for the water in the plant is about 4 hours. Discharge water is lead out in the Drammensfjord outside Solumstrand at about 40 m water depth and 200 m from the shoreline. Lindum Ressurs & Gjenvinning Lindum Ressurs & Gjenvinning is located in Drammen municipality. The facility receives various kinds of wastes from the Drammen region. The waste that cause run off to seepage water can be categorized as slightly polluted masses, residual waste, waste from sand trap and grid, sand from sand blasting, compost, waste put permanently in bio cell and waste to industry bio cell (degradable waste and sludge). A total of about m 3 or tonnes waste were delivered to the site in The seepage water is not aerated nor is it treated by any sedimentation (sedimentation basin), but the seepage water is pumped directly to Solumstrand waste water treatment plant. Drammensfjorden Drammensfjorden is a typical sill fjord with a very narrow sill against the outer part of Oslofjord in the area of Svelvik. Inside the sill the fjord is formed as a deep basin with water depth over 60 m in most parts, and a maximum depth of approximately 120 m. The bottom water is mostly anoxic, meaning that there is limited water exchange with the outer part of the Oslofjord. The fjord receives waste water from Solumstrand RA (water treatment plant) and Lindum Ressurs & Gjenvinning (waste disposal site). 25

28 The city of Drammen has a population of about 62,000, and is located next to the fjord, in the area where the Drammenselva flows into the fjord. Drammenselva is a relatively large river with an average yearly flow of m 3 /s. This flow amounts to about 97 % of the fresh water going into the fjord. The second main source of fresh water to the fjord is the Lierelva, which contributes to about 2 % of the fresh water going into the fjord. Drammenselva flows through several small communities mainly agricultural areas, but also various types of industry, including wood processing. Lierelva mainly flows through agricultural areas. Drammen city and Elkjøp store BFR is sampled from indoor air in Elkjøp Drammen and outdoor air is sampled from the centre of Drammen city. Some details of Drammen are given above. Elkjøp is Scandinavia's largest trading company for consumer electronics and electrical appliances, and had a turnover of NOK 17.6 billion in 2007/08. Operating income was NOK billion. The Group has established retail operations in Norway, Sweden, Denmark, Finland, Iceland and the Faroe Islands with the main business being related to huge department stores. All of the 233 department stores, including the store in Drammen, in the Nordic countries are mainly supplied from its own distribution business, with a central warehouse in Jönköping (Sweden). Approximately 6,000 employees are employed in Elkjøp group, which is owned by British DSG International plc., One of Europe's largest retailers in consumer electronics. Hurum Energigjenvinning Hurum Energigjenvinning KS is a plant for incineration of waste. It is located on Hurum in the vicinity of the Drammen fjord. The plant is based on the Energos technology. Energos plants are built in modules with one or more processing line in parallel to meet customer s requirements regarding energy production and fuel processing capacity. The energy content of the fuel is converted into electricity and/or heat delivery for local use, e.g. district heating or industrial applications. The plant at Hurum was started in 2001, and treats approximately 40,000 tonnes domestic and industrial waste each year. The annual energy production is approximately 90 Gwh. Identifying emissions from the plant are particles, inorganic gasses (such as CO), acid gasses (such as SOx, HCl and NOx), heavy metals, dioxins and PAH s Hokksund area Hellik Teigen AS Hellik Teigen AS is a car demolishing site located at Losmoen in Hokksund. It receives and recycles iron and other metals from scrapped cars, household appliances and raw metal materials such as steel, cast iron, stainless steel and copper, aluminium, brass and different types of alloys. Hellik Teigen also receives computer and electronic waste, wood and rubber. According to staff members, the plant primarily receives the cars after the main environmental contaminants have been removed. All water run-off at the site is collected and treated (sand trap, oil skimmer, flotation, venturi scrubber) before it is discharged to the small river Loselva. At low water levels in the river (which is influenced by the tidal amplitude) the discharge pipe is well above the water level. Loselva flows into the upper part of Drammenselva which in turn flows into the Drammen fjord. 26

29 5.1.3 Lillehammer area Lillehammer RA Lillehammer water treatment plant was established in 1977 as a mechanical and chemical plant for treatment of waste water, dimensioned for PE. In general, the process steps are as follows: removal by grid and sand trap, primary sedimentation and secondary and final sedimentation tank/basin, sludge treatment with gravitational thickening, drainer and centrifuges. In 1993, the plant was expanded to include the Kaldnes Moving Bed biofilm process for removal of nitrogen. In addition, the capacity of the plant was upgraded to PE. The volume of the basin in the plant is about 11,000 m 3, Q dim = 1200 m 3 /h and Q max = 1900 m 3 /h. Lillehammer water treatment plant receives water from the municipality of Gausdal, some parts of Øyer and Ringsaker, and the municipality of Lillehammer. Besides treatment of domestic waste water, the plant also receives waste water from the food industry, textile industry, laundries, hospital, treatment plant for wet organic waste and waste disposal sites. The water treatment plant has it own sewage tank, and receives sewage from the abovementioned municipalities as well as thickened sludge from another water treatment plant. The reported volume of treated water in 2008 was m 3. The requirement for the plant is removal of 95 % of phosphorus (<0.25 mg/l), 70 % BOF, 75 % KOF, and 70 % nitrogen. Treated water is discharged in Mjøsa (lake) about 200 m from land and at 20 m water depth. Dewatered sludge is transported to an intermunicipal sludge treatment plant where it is treated further. Mjøsa and Losna Mjøsa is Norway s largest lake with a surface area of 365 km 2. The lake is about 117 km long and the deepest part is officially measured to 468 m. The largest river flows into Mjøsa in the northern part, near Lillehammer, and is named Gudbrandsdalslågen. Losna is in fact a part of Gudbrandalslågen. Several other rivers flow into Mjøsa, such as Rinna, Vismunda, Stokkeelva, Hunnselva, Leanelva in the west,and Moelva, Brumunda, Svartelva and Starelva in the east. The only river that flows out of Mjøsa is Vorma (in the southern end). Mjøsa is known for its population of large trout and lake herring which are popular among anglers Tromsø area Langnes RA Langnes waste water treatment plant is located in Tromsø in northern Norway. Waste water is cleaned mechanically by four Maskozoll coarse screens with 1 mm openings and then by 2 Hydrotech screens with 0.12 mm openings. Waste water going into the plant comes mainly from households. Treated volume of water was in 2009 about m 3. Sludge is treated by a thickening tank and polymer is added before it is run trough the coarse screens for dewatering. The plant is dimensioned for about PE. There is no certain good numbers of water retention times because the water flows straight trough screens and is led trough 530 m of 630 mm PE pipeline before it is discharged at 20 m water depth in Sandnessundet. 27

30 Sandnessundet Sandnessundet is a strait between Tromsøya and Kvaløya in northern Norway. The strait is about 14 km long and is dominated by rather strong tidal currents with a speed of up to 2 5 knots. Waste water from Langnes RA is discharged to Sandnessundet Bergen area Flesland airport Flesland airport is located in the western part of Norway near the city of Bergen. The airport was included in this investigation due to the existing fire drill area at the airport. The fire drill area has been used for many years on a regular basis. In a fire drill exercise, various kinds of fire fighting powders and foam are used. The existing fire drill area is connected to an oil separator. Seepage water is drained to a stream which leads to Langavatnet, a lake located just adjacent to the airport. Langavatnet Langavatnet is located within the Flesland airport area. The lake receives seepage water from Flesland airport. Langavatnet drains to the sea through Fleslandselva which flows into the sea near Flesland brygge Flesland brygge Flesland brygge is located just west of Flesland airport, and is the area where Fleslandselva flows into the sea. Puddefjorden Puddefjorden is an approximately 3.5 km large part of Byfjorden in Bergen. It is located close to Bergen city and is surrounded by various kinds of industries. Puddefjorden is a polluted fjord and is included in the plan for remediation of polluted sediments in Bergen. Puddefjorden is located northeast of Flesland airport Haugesund area Res-Q Res-Q is located near Bleivik to the north of Haugesund city. Res-Q is a facility where fire and explosion safety courses and drills are held. It is the only facility in Norway that regularly hosts courses where fire foam with FTS (as a substitution in fire foam) is used. Run-off from the facility is lead to two sedimentation basins before discharge to sea in Bleivika at about 15 m depth. An oil skimmer and centrifugation is used for cleaning the runoff. Sediment from the sediment basins is removed twice a year and handled as hazardous waste. PFCs were earlier found in sediment from the facility (SFT, 2007). Bleivika Bleivika is the receiving water for the discharges from Res-Q. The area is partly sheltered by some small island, but the discharge point from Res-Q is located in a more exposed area outside the Islands at 15 m depth. 28

31 5.2 Sampling and sample treatment In general the sample strategy presented in Table 2 was followed. More detailed description of the sampling is given in the chapters below. Table 2 Overview of general sampling strategy. Type of sampling Strategy Waste water Composite sample of inlet and outlet water from 1 week in 3 periods => 6 samples. About 7 litres were sampled in glass bottles wrapped in aluminium foil (BFR) and 1 litre in PE bottles (PFC) Sludge One sample from 1 week in 3 periods => 3 samples. Stored in glass bottles wrapped in aluminium foil (BFR) and PE containers (PFC) Seepage water 3 replica of a composite sample from 1 week => 3 samples. About 7 litres were sampled in glass bottles wrapped in aluminium foil (BFR) and 1 litre in PE bottles (PFC) Sediment- disposal site 3 replica of a composite sample from 1 week => 3 samples. Stored in glass bottles wrapped in aluminium foil (BFR) and PE containers (PFC) Moss and pine needles Last year s growth from 4 stations in different direction and distance from plant => 4 samples. 1 litre of sample from each station was packed in aluminium foil. Samples of pine needles and stair step moss (Hylocómium splendens) Soil 10 samples in increasing distance from the fire drill site => 10 samples. Sample stored in PE container (PFC only) Sediment receiving water 3 replicas from 3 stations with increasing distance from discharge point => 9 samples. Stored in glass bottles wrapped in aluminium foil (BFR) and PE containers (PFC) Fish liver 20 fish from receiving waters analysed as 4 sub samples of 5 fish => 4 samples. Fish was caught by local fishermen after instruction from DNV. Material worked up at DNV s Biology laboratory and stored in glass bottles wrapped in aluminium foil (BFR) and PE containers (PFC) Blue mussel Composite sample of 30 shells from 3 stations in receiving water = 3 samples. Shells were sampled by local fishermen. Material worked up at DNV s Biology laboratory and stored in glass bottles wrapped in aluminium foil (BFR) and PE containers (PFC) Crab 20 crabs from receiving waters analysed as 4 sub samples of 5 crab meat => 4 samples. Crabs where caughtby local fishermen. Material worked up at DNV s Biology laboratory and stored in glass bottles wrapped in aluminium foil (BFR) and PE containers (PFC) Air 1 week of sampling from 3 different periods => 3 samples The following general remarks are given regarding sampling: Clean gloves and suit were used for each sampling. No cosmetics were allowed to be used prior to or during sampling. Watches and other electronic equipment were not allowed used during sampling. The samples were stored in a cool and dark place in the time between sampling. All samples were frozen when they arrived at DNV office prior to analysis. All samples were kept frozen until arrival at the analysis laboratory 29

32 5.2.1 Drammen area The sampling locations are presented in Figure 4 and Figure 5. Figure 4 Overview of sampling locations in the inner Drammensfjord and city of Drammen, Drammen area. 30

33 Figure 5 Overview of sampling locations around Hurum Energigjenvinning, Drammen area. 31

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