Microplastic analysis in soils : A comparative assessment

Peneva, S. and Le, Q.N.P. and Munhoz, D.R. and Wrigley, O. and Wille, F. and Doose, H. and Halsall, C. and Harkes, P. and Sander, M. and Braun, M. and Amelung, W. (2025) Microplastic analysis in soils : A comparative assessment. Ecotoxicology and Environmental Safety, 289: 117428. ISSN 0147-6513

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Abstract

Microplastic (MiP) contamination poses environmental risks, but harmonizing data from different quantification methods and sample matrices remains challenging. We compared analytical protocols for MiP quantification in soil, consisting of Digital, Fluorescence, Fourier-transform infrared (FTIR), and Raman Microscopy as well as quantitative Pyrolysis-Gas Chromatography-Mass Spectroscopy (Py-GC-MS) and 1-proton nuclear magnetic resonance (1H NMR) spectroscopy as detection techniques. Each technique was coupled with a specific extraction procedure and evaluated for three soils with different textures and organic carbon contents, amended with eight types of large MiPs (0.5–1 mm) – high- and low-density polyethylene (HDPE and LDPE), polypropylene (PP), polystyrene (PS), polyamide (PA), polyethylene terephthalate (PET), polyvinyl chloride (PVC), and a biodegradable mulch film product composed of polybutylene adipate-co-terephthalate/ polylactic acid (PBAT/ PLA). In addition, we included two types of small MiPs (20–250 µm) composed of either LDPE or PBAT/ PLA in the tests. The results showed that protocols for Digital, Fluorescence, and ATR-FTIR microscopy recovered 74–98 % of the large MiPs, with fluorescence yielding the highest recoveries. Raman spectroscopy was most sensitive to soil organic matter residues, requiring more sophisticated sample pretreatment. Fluorescence staining with subsequent Fluorescence microscopy detection effectively recovered most small-sized LDPE-MiP but missed 56–93 % of small PBAT/ PLA particles. For the latter, reliable quantification was achieved only using Soxhlet extraction combined with 1H NMR spectroscopic quantification. Pyrolysis-GC-MS showed intermediate results, displaying low sensitivity to plastic type and lower recoveries as soil clay content increased. We conclude that different methods have different sensitivities for different MiP materials in different soils, i.e. comparisons of MiP loads and threshold settings for MiP loads across methodologies require careful consideration. Yet, our data indicate that adding stained large MiP as an internal standard could enhance extraction control, while Soxhlet-extraction with subsequent 1H NMR analysis is most powerful for controlling future thresholds of small MiP from biodegradable materials.

Item Type:
Journal Article
Journal or Publication Title:
Ecotoxicology and Environmental Safety
Additional Information:
Export Date: 18 December 2024 CODEN: EESAD Correspondence Address: Braun, M.; Institute of Crop Science and Resource Conservation (INRES), Nussallee 13, Germany; email: melanie.braun@uni-bonn.de Funding details: Horizon 2020 Framework Programme, H2020, 55334 Funding details: Horizon 2020 Framework Programme, H2020 Funding details: European Commission, EC, 955334 Funding details: European Commission, EC Funding text 1: This work was supported by the European Union's Horizon 2020, ITN SOPLAS, with grant agreement No. 955334 to the five first authors. The authors thank Elisabeth Shaw and Alexandre Benedetto (Lancaster University) for their help with the fluorescence microscope measurement; Markus Rhode, Ulrich Meinke and Sven Simons (Wessling GmbH) for the expertise provided for the measurements with Raman Microscope and Pyrolysis\u2013Gas Chromatography\u2013Mass Spectroscopy; Prof Violette Geissen for supporting and supervising the work done at Wageningen University and Research. Funding text 2: This work was supported by the European Union\u2019s Horizon 2020, ITN SOPLAS, with grant agreement No. 55334 to the five first authors. The authors thank Elisabeth Shaw and Alexandre Benedetto (Lancaster University) for their help with the fluorescence microscope measurement; Markus Rhode, Ulrich Meinke and Sven Simons (Wessling GmbH) for the expertise provided for the measurements with Raman Microscope and Pyrolysis\u2013Gas Chromatography\u2013Mass Spectroscopy; Prof Violette Geissen for supporting and supervising the work done at Wageningen University and Research.
Uncontrolled Keywords:
/dk/atira/pure/subjectarea/asjc/2700/2739
Subjects:
?? conventional synthetic and biodegradable polymerssoil pollutionspectroscopymicroplasticorganic carbonpolyamidepolyethylene terephthalatepolylactic acidpolypropylenepolystyrenepolyvinylchloridesoil organic matterarticleenvironmental riskfluorescencefluores ??
ID Code:
226538
Deposited By:
Deposited On:
19 Dec 2024 10:40
Refereed?:
Yes
Published?:
Published
Last Modified:
01 Jan 2025 04:00