Microplastic analysis in soils: A comparative assessment

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...

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Main Authors: Stoyana Peneva, Quynh Nhu Phan Le, Davi R. Munhoz, Olivia Wrigley, Flora Wille, Heidi Doose, Crispin Halsall, Paula Harkes, Michael Sander, Melanie Braun, Wulf Amelung
Format: Article
Language:English
Published: Elsevier 2025-01-01
Series:Ecotoxicology and Environmental Safety
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Online Access:http://www.sciencedirect.com/science/article/pii/S0147651324015045
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author Stoyana Peneva
Quynh Nhu Phan Le
Davi R. Munhoz
Olivia Wrigley
Flora Wille
Heidi Doose
Crispin Halsall
Paula Harkes
Michael Sander
Melanie Braun
Wulf Amelung
author_facet Stoyana Peneva
Quynh Nhu Phan Le
Davi R. Munhoz
Olivia Wrigley
Flora Wille
Heidi Doose
Crispin Halsall
Paula Harkes
Michael Sander
Melanie Braun
Wulf Amelung
author_sort Stoyana Peneva
collection DOAJ
description 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.
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spelling doaj-art-6019052835b2449a9f1de01a7c160d232025-01-23T05:25:30ZengElsevierEcotoxicology and Environmental Safety0147-65132025-01-01289117428Microplastic analysis in soils: A comparative assessmentStoyana Peneva0Quynh Nhu Phan Le1Davi R. Munhoz2Olivia Wrigley3Flora Wille4Heidi Doose5Crispin Halsall6Paula Harkes7Michael Sander8Melanie Braun9Wulf Amelung10Wessling GmbH, AM Umweltpark 1, Bochum 44793, Germany; Institute of Crop Science and Resource Conservation (INRES), Soil Science and Soil Ecology, University of Bonn, Nussallee 13, Bonn 53115, GermanyLancaster Environment Centre, Lancaster University, Lancaster LA1 4YQ, UKSoil Physics and Land Management Group, Wageningen University & Research, P.O. Box 47, Wageningen 6700 AA, the NetherlandsInstitute of Crop Science and Resource Conservation (INRES), Soil Science and Soil Ecology, University of Bonn, Nussallee 13, Bonn 53115, GermanyInsitute of Biogeochemistry and Pollutant Dynamics, ETH Zurich, Zurich 8092, SwitzerlandCo.KG, Feodor-Lynen Straße 23, Hannover 30625, Germany; Wessling Consulting Engineering GmbH &amp, Feodor-Lynen Straß∼e 23, Hannover 30625, GermanyLancaster Environment Centre, Lancaster University, Lancaster LA1 4YQ, UKSoil Physics and Land Management Group, Wageningen University & Research, P.O. Box 47, Wageningen 6700 AA, the NetherlandsInsitute of Biogeochemistry and Pollutant Dynamics, ETH Zurich, Zurich 8092, SwitzerlandInstitute of Crop Science and Resource Conservation (INRES), Soil Science and Soil Ecology, University of Bonn, Nussallee 13, Bonn 53115, Germany; Corresponding author.Institute of Crop Science and Resource Conservation (INRES), Soil Science and Soil Ecology, University of Bonn, Nussallee 13, Bonn 53115, Germany; Agrosphere Institute (IBG-3), Forschungszentrum Jülich GmbH, Wilhelm-Johnen-Str, Jülich 52425, GermanyMicroplastic (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.http://www.sciencedirect.com/science/article/pii/S0147651324015045SpectroscopySoil pollutionConventional synthetic and biodegradable polymers
spellingShingle Stoyana Peneva
Quynh Nhu Phan Le
Davi R. Munhoz
Olivia Wrigley
Flora Wille
Heidi Doose
Crispin Halsall
Paula Harkes
Michael Sander
Melanie Braun
Wulf Amelung
Microplastic analysis in soils: A comparative assessment
Ecotoxicology and Environmental Safety
Spectroscopy
Soil pollution
Conventional synthetic and biodegradable polymers
title Microplastic analysis in soils: A comparative assessment
title_full Microplastic analysis in soils: A comparative assessment
title_fullStr Microplastic analysis in soils: A comparative assessment
title_full_unstemmed Microplastic analysis in soils: A comparative assessment
title_short Microplastic analysis in soils: A comparative assessment
title_sort microplastic analysis in soils a comparative assessment
topic Spectroscopy
Soil pollution
Conventional synthetic and biodegradable polymers
url http://www.sciencedirect.com/science/article/pii/S0147651324015045
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