Abstract
The extraction of plastic microparticles, so-called microplastics, from sludge is a challenging task due to the complex, highly organic material often interspersed with other benign microparticles. The current procedures for microplastic extraction from sludge are time consuming and require expensive reagents for density separation as well as large volumes of oxidizing agents for organic removal, often resulting in tiny sample sizes and thus a disproportional risk of sample bias. In this work, we present an improved extraction method tested on return activated sludge (RAS). The treatment of 100 ml of RAS requires only 6% hydrogen peroxide (H2O2) for bleaching at 70 °C, followed by density separation with sodium nitrate/sodium thiosulfate (SNT) solution, and is completed within 24 h. Extracted particles of all sizes were chemically analyzed with confocal Raman microscopy. An extraction efficiency of 78 ± 8% for plastic particle sizes 20 µm and up was confirmed in a recovery experiment. However, glass shards with a diameter of less than 20 µm remained in the sample despite the density of glass exceeding the density of the separating SNT solution by 1.1 g/cm3. This indicates that density separation may be unreliable for particle sizes in the lower micrometer range.
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Barboza LGA, Gimenez BCG (2015) Microplastics in the marine environment: current trends and future perspectives. Mar Pollut Bull. doi:10.1016/j.marpolbul.2015.06.008
Browne MA, Crump P, Niven SJ, Teuten E, Tonkin A, Galloway T, Thompson R (2011) Accumulation of microplastic on shorelines worldwide: sources and sinks. Environ Sci Technol 45:9175–9179
Brun N, Youssef I, Chevrel M-C, Chapron D, Schrauwen C, Hoppe S, Bourson P, Durand A (2013) In situ monitoring of styrene polymerization using Raman spectroscopy: multi-scale approach of homogeneous and heterogeneous polymerization processes. J Raman Spectrosc 44:909–915
Carr SA, Liu J, Tesoro AG (2016) Transport and fate of microplastic particles in wastewater treatment plants. Water Res 91:174–182
Claessens M, Van Cauwenberghe LV, Vandegehuchte MB, Janssen CR (2013) New techniques for the detection of microplastics in sediments and field collected organisms. Mar Pollut Bull 70:227–233
Cole M, Webb H, Lindeque PK, Fileman ES, Halsband C, Galloway TS (2014) Isolation of microplastics in biota-rich seawater samples and marine organisms. Sci Rep 4:4528
Corcoran PL, Biesinger MC, Grifi M (2009) Plastics and beaches: a degrading relationship. Mar Pollut Bull 58(1):80–84
Corcoran PL, Norris T, Ceccanese T, Walzak MJ, Helm PA, Marvin CH (2015) Hidden plastics of Lake Ontario, Canada and their potential preservation in the sediment record. Environ Pollut 204:17–25
De Gelder J, De Gussem K, Vandenabeele P, Moens L (2007) Reference database of Raman spectra of biological molecules. J Raman Spectrosc 38:1133–1147
Dubaish F, Liebezeit G (2013) Suspended microplastics and black carbon particles in the Jade System, Southern North Sea. Water Air Soil Pollut 224:1–8
Eerkes-Medrano D, Thompson RC, Aldridge DC (2015) Microplastics in freshwater systems: a review of the emerging threats, identification of knowledge gaps and prioritization of research needs. Water Res 75:63–82
Elias H-G (2003) Makromoleküle: band 3: industrielle polymere und synthesen, 6th edn. WILEY-VCH Verlag GmbH & Co. KGaA, WILEY
Garrett TR, Bhakoo M, Zhang Z (2008) Bacterial adhesion and biofilms on surfaces. Prog Nat Sci 18:1049–1056
Hori K, Matsumoto S (2010) Bacterial adhesion: from mechanism to control. Biochem Eng J 48:424–434
Imhof HK, Schmid J, Niessner R, Ivleva NP, Laforsch C (2012) A novel, highly efficient method for the separation and quantification of plastic particles in sediments of aquatic environments. Limnol Oceanogr Methods 10:524–537
Klein S, Worch E, Knepper TP (2015) Occurrence and spatial distribution of microplastics in river shore sediments of the Rhine-Main Area in Germany. Environ Sci Technol 49:6070–6076
Kniggendorf A-K, Meinhardt-Wollweber M (2011) Of microparticles and bacteria identification—(resonance) Raman micro-spectroscopy as a tool for biofilm analysis. Water Res 45:4571–4582
Kniggendorf A-K, Meinhardt-Wollweber M, Yuan X, Roth B, Seifert A, Fertig N, Zeilinger C (2014) Temperature-sensitive gating of hCx26: high-resolution Raman spectroscopy sheds light on conformational changes. Biomed Opt Express 5(7):2054–2065
Kniggendorf A-K, Nogueira R, Kelb C, Schadzek P, Meinhardt-Wollweber M, Ngezahayo A, Roth B (2016) Confocal Raman microscopy and fluorescent in situ hybridization: a complementary approach for biofilm analysis. Chemosphere 161:112–118
Lafuente B, Downs RT, Yang H, Stone N (2015) The power of databases: the RRUFF project. In: Armbruster T, Danisi RM (eds) Highlights in mineral crystallography. de Gruyter, Berlin
Lippert T, Ortelli E, Raimondi J-C, Wambach J, Wei J, Wokaun A (1999) Imaging-XPS/Raman investigation on the carbonization of polyimide after irradiation at 308 nm. Appl Phys A. doi:10.1007/s003399900220
Löder M, Gerdts G (2015) Methodology used for the detection and identification of microplastics: a critical appraisal. In: Bergman M, Gutow L, Klages M (eds) Marine anthropogenic litter. Springer, Berlin, pp 447–448
McCormick A, Hoellein TJ, Mason SA, Schluep J, Kelly JJ (2014) Microplastic is an abundant and distinct microbial habitat in an urban river. Environ Sci Technol 48(2):11863–11871
Mohee R, Unmar G (2007) Determining biodegradability of plastic materials under controlled and natural composting environments. Waste Manag 27:1486–1493
Nuelle M-T, Dekiff JH, Remy D, Fries E (2014) A new analytical approach for monitoring microplastics in marine sediments. Environ Pollut 184:161–169
Obbard RW, Sadri S, Wong YQ, Khitun AA, Baker I, Thompson RC (2014) Global warming releases microplastic legacy frozen in Arctic Sea ice. Earth’s Future 2(6):315–320
Oldak D, Kaczmarek H, Buffeteau T, Sourisseau C (2005) Photo-and bio-degradation processes in polyethylene, cellulose and their blends studied by ATR-FTIR and Raman spectroscopies. J Mater Sci 40:4189–4198
Parnell S, Min K, Cakmak M (2003) Kinetic studies of polyurethane polymerization with Raman spectroscopy. Polymer 44:5137–5144
Sanchez W, Bender C, Porcher J-L (2014) Wild gudgeons (Gobio gobio) from French rivers are contaminated with microplastics: preliminary study and first evidence. Environ Res 128:98–100
Sato H, Shimoyama M, Kamiya T, Amari T, Sasic S, Ninomiya T, Siesler HW, Ozaki Y (2002) Raman spectra of high-density, low-density, and linear low-density polyethylene pellets and prediction of their physical properties by multivariate analysis. J Appl Polym Sci 86:443–448
Semensatto DL, Dias-Brito D (2007) Alternative saline solutions to float foraminiferal tests. J Foraminifer Res 37(3):265–269
Singh RP, Agrawal M (2008) Potential benefits and risks of land application of sewage sludge. Waste Manag 28:347–358
Taylor ML, Gwinnett C, Robinson LF, Woodall LC (2016) Plastic microfibre ingestion by deep-sea organisms. Sci Rep 6(33997):1–8
Thompson RC, Olsen Y, Mitchell RP, Davis A, Rowland SJ, John AWG, McGonigle D, Russel AE (2004) Lost at sea: where is all the plastic? Science 304(5672):838
Van Echelpoel W, Vandegehuchte M, De Gueldre G, Van Cauwenberghe L (2014) Microplastics in a biological wastewater treatment plant and the surrounding freshwater environment in Flanders: quantitative assessment. Master’s dissertation submitted in partial fulfillment of the requirements for the degree of Master of Science in “Technology for Integrated Water Management.” http://lib.ugent.de/catalog/rug01:002147111
Yonkos LT, Friedel EA, Perez-Reyes AC, Ghosal S, Arthur CD (2014) Microplastics in four estuarine rivers in the Chesapeake Bay, USA. Environ Sci Technol 48:14195–14202
Zhang K, Feldner A, Fischer S (2011) FT Raman spectroscopic investigation of cellulose acetate. Cellulose 18:995–1003
Zhang K, Gong W, Lv J, Xiong X, Wu C (2015) Accumulation of floating microplastics behind the Three Gorges Dam. Environ Pollut 204:117–123
Acknowledgements
The authors thank Karin Kock and Benjamin Schwanda for their technical assistance to their work. The work of Dr. Kniggendorf was funded by the Federal Ministry of Education and Research (BMBF) of Germany within the project of OPTIMUS (Project Number: 13N13811). The work of Surya Sujathan was funded by the DAAD Sandwich Model Scholarships for Master’s Students of the IITs and IIMs, 2015 (Personal Ref No: 91590631).
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Sujathan, S., Kniggendorf, AK., Kumar, A. et al. Heat and Bleach: A Cost-Efficient Method for Extracting Microplastics from Return Activated Sludge. Arch Environ Contam Toxicol 73, 641–648 (2017). https://doi.org/10.1007/s00244-017-0415-8
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DOI: https://doi.org/10.1007/s00244-017-0415-8