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Analysis of PFAS, Phthalates, Alternative Plasticizers and Organophosphate Esters in Sludge

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Analysis of PFAS, Phthalates, Alternative Plasticizers and Organophosphate Esters in Sludge No. U 6235 January 2020 Analysis of PFAS, phthalates, alternative plasticizers and organophosphate esters in sludge Commissioned by Naturvårdsverket Georgios Giovanoulis, Jenny Aasa, Jon Benskin, Merle Plassmann, Minh Nguyen, Raed Awad and Robin Vestergren Author: Georgios Giovanoulis, Jenny Aasa, Minh Nguyen, and Robin Vestergren Commissioned by Naturvårdsverket Project Participants: Naturvårdsverket Report number: U 6235 © IVL Swedish Environmental Research Institute 2020 IVL Swedish Environmental Research Institute Ltd., P.O Box 210 60, S-100 31 Stockholm, Sweden Phone +46-(0)10-788 65 00 // www.ivl.se This report has been reviewed and approved in accordance with IVL's audited and approved management system. Table of contents Summary ................................................................................................................................ 4 Sammanfattning ..................................................................................................................... 5 1 Introduction ..................................................................................................................... 6 2 Materials & Methods ...................................................................................................... 8 2.1 Sampling ............................................................................................................................................ 8 2.2 Extraction and analysis of phthalates, alternative plasticizers and organophosphate esters .................................................................................................................................................. 8 2.3 Extraction and analysis of PFAS ....................................................................................................... 9 2.3.1 Quantitative/target analysis ....................................................................................................... 9 2.3.2 TOP analysis ........................................................................................................................... 10 2.3.3 EOF analysis ........................................................................................................................... 11 2.3.4 Suspect screening .................................................................................................................... 11 3 Results & discussion ..................................................................................................... 12 3.1 Phthalates and alternative plasticizers ............................................................................................. 12 3.2 Organophosphate esters ................................................................................................................... 13 3.3 PFAS ............................................................................................................................................... 14 3.3.1 Quantitative/target analysis ................................................................................................... 14 3.3.2 TOP analysis ............................................................................................................................ 17 3.3.3 EOF analysis ............................................................................................................................ 18 3.3.4 Suspect screening ................................................................................................................... 20 4 Conclusions................................................................................................................... 21 5 References ..................................................................................................................... 22 Appendix A. Phthalate and alternative plasticizer levels (mg/kg dry weight) ............................................ 24 Appendix B. Organophosphate ester levels (mg/kg dry weight) ................................................................ 25 Appendix C. PFAS levels (ng/g dry weight) .............................................................................................. 26 Appendix D. PFAS levels after TOP (ng/g dry weight) ................................................................................. 28 • Report U 6235 Analysis of PFAS, phthalates, alternative plasticizers and organophosphate esters in sludge Summary Wastewater treatment plants (WWTPs) can be considered a water pollution point source as all potential pollutants from household as well as from certain industry production passes the WWTPs. Therefore, sludge from WWTPs may be enriched with pollutants and is a relevant matrix for screening for both known and hitherto unknown potential hazardous chemicals. If the sludge from municipal WWTPs is to be used as a source of nutrient or other purposes, then it could be necessary to employ methods for removal of micropollutants in the sludge. The present study constitutes an addition to a large-scale experiment focusing on the reduction of pharmaceuticals, antibiotics and hormones in sewage sludge stored over a period of a year. The objective of the present study was to analyse the presence of per- and polyfluoroalkyl substances (PFAS), organophosphate esters, phthalates and alternative plasticizers and their potential degradation/reduction in mesophilic anaerobic digested sludge in different treatments. This study is part of a larger on-going project on reduction of pharmaceuticals and organic pollutants in sludge. Extracts of sludge samples were analysed using three instrumental methods: liquid chromatography coupled to both tandem mass spectrometry (LC-MS/MS) and high-resolution mass spectrometry (LC-HRMS) and gas chromatography coupled to tandem mass spectrometry (GC-MS/MS). Target analysis of several compounds (PFASs, organophosphate esters, phthalates and alternative plasticizers), analysis of total oxidizable precursors of PFASs and a suspect-screening of more than 1000 PFAS were performed at IVL. Extractable organic fluorine (EOF) was also performed on combustion ion chromatography at Stockholm University for quantification of potential unknown fluorinated compounds in the sludge. Decreasing trends for concentrations of organophosphate esters, phthalates, alternative plasticizers and PFAS could be observed in composted sludge over the storage time while the non-composted showed variable time trends for different substance classes. For PFAS, the sum concentrations of target analytes increased by almost an order of magnitude during 12 months of storage in the non- composted sludge. Furthermore, the results from TOP and EOF furthermore suggested that the sludge from both treatment experiments contained a significant fraction PFAS that could not be quantified by the targeted analysis. 4 • Report U 6235 Analysis of PFAS, phthalates, alternative plasticizers and organophosphate esters in sludge Sammanfattning Avloppsreningsverk kan betraktas som en viktig punktkälla för föroreningar i vatten. Slam från avloppsreningsverk kan anrika föroreningar som har en huvudsaklig fördelning till slammet, och är således en relevant matris för screening för både kända och potentiella farliga kemikalier. Om slammet från kommunala avloppsreningsverk skall användas som en källa för näringsämnen eller andra syften kan det vara nödvändigt att avlägsna eller bryta ned potentiellt farliga mikroföroreningar i slammet. Denna studie utgör ett tillägg till ett storskaligt experiment som fokuserar på minskning av läkemedel, antibiotika och hormoner i avloppsslam som lagrats ett år. Kompakt eller poröst slam som rötats antingen termofilt eller mesofilt har i ovan nämnda experimentet lagrats under flera olika betingelser: täckt eller öppet, med och utan tillsats av urea, samt med och utan kompostering. I denna studie har endast poröst mesofilt rötat slam, som antingen har lagrats öppet eller med kompostering, studerats. Syftet med den här studien var att studera om per- och polyfluoralkylsubstanser (PFAS), organofosfatestrar samt ftalater och alternativa mjukgörare bryts ned under lagring. Extrakt av slamprover har analyserats med tre instrumentella metoder: vätskekromatografi kopplad till både tandemsmasspektrometri (LC-MS / MS) och högupplösta masspektrometri (LC-HRMS) samt gaskromatografi kopplad till tandemsmasspektrometri (GC-MS / MS). Förutom riktad kvantitativ analys av flera föreningar har analys av totala oxiderbara prekursorer av PFAS-ämnen och en sk suspect screening av mer än 1000 PFAS genomförts. Andelen extraherbart organiskt bunden fluor (EOF), dvs den totala fluormängden bundet till organiska ämnen, har också bestämts av Stockholms Universitet med förbränningsjonkromatografi för att kvantifiera andelen av potentiellt okända PFAS. Minskande trender för koncentrationer av organofosfatestrar, ftalater och alternativa mjukgörare samt PFAS kunde observeras i slam med kompostbehandlingen medan slammet som lagrats öppet inte visade någon tydlig trend för de ämnen som mättes i denna studie. För PFAS ökade summan av analyserade ämnen med nästan en tiopotens under 12 månaders lagring i det icke-komposterade slammet. Resultaten från TOP och EOF visade även på en betydande andel (91-97%) av hittills oidentifierade PFAS i slam från båda försöken. 5 • Report U 6235 Analysis of PFAS, phthalates, alternative plasticizers and organophosphate esters in sludge 1 Introduction During the purification process in wastewater treatment plants nutrients from the waste water are enriched in the sludge.
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