Abstract
The increasing concern over microplastics (MPs) contamination in agricultural soils due to excessive plastic use is a worldwide concern. The objective of this study was to determine which analytical technique is most effective for the analysis of MPs in agricultural soils. Near-infrared spectroscopy (NIR), scanning electron microscopy (SEM), multispectral analysis, and X-ray diffraction were used to analyze sections of clay soil containing varying percentages of virgin white MPs from 0 to 100%. X-ray analysis only detected MPs at high concentrations (20%). However, NIR at 2.300 nm and multispectral analysis at 395 nm demonstrated greater accuracy and sensitivity in distinguishing between all MPs levels. SEM revealed that MPs have an amorphous structure that is distinct from crystalline soil, potentially influencing their interactions with other soil constituents. These findings highlight the value of NIR and multispectral analysis in accurately identifying and measuring MPs in soil. Efficient management plans rely on increased awareness of MPs' environmental impact.
This is a preview of subscription content, log in via an institution to check access.
Similar content being viewed by others
Data availability
No datasets were generated or analysed during the current study.
References
Barker, M., & Rayens, W. (2003). Partial least squares for discrimination. Journal of Chemometrics, 17(3), 166–173. https://doi.org/10.1002/cem.785
Bellon-Maurel, V., Fernandez-Ahumada, E., Palagos, B., Roger, J. M., & McBratney, A. (2010). Critical review of chemometric indicators commonly used for assessing the quality of the prediction of soil attributes by NIR spectroscopy. TrAC. Trends in Analytical Chemistry, 29(9), 1073–1081. https://doi.org/10.1016/j.trac.2010.05.006
Bhat, M. A. (2024). Airborne microplastic contamination across diverse university indoor environments: A comprehensive ambient analysis. Air Quality, Atmosphere and Health. https://doi.org/10.1007/s11869-024-01548-9
Bonse, U. (2008). X-ray imaging: past and present. Developments in X-Ray Tomography VI. https://doi.org/10.1117/12.794694
Bosker, T., Bouwman, L. J., Brun, N. R., Behrens, P., & Vijver, M. G. (2019). Microplastics accumulate on pores in seed capsule and delay germination and root growth of the terrestrial vascular plant Lepidium sativum. Chemosphere, 226, 774–781. https://doi.org/10.1016/j.chemosphere.2019.03.163
Braun, T., Ehrlich, L., Henrich, W., Koeppel, S., Lomako, I., Schwabl, P., & Liebmann, B. (2021). Detection of microplastic in human placenta and meconium in a clinical setting. Pharmaceutics, 13(7), 921. https://doi.org/10.3390/pharmaceutics13070921
Brochado, M. G. S., Miranda, C. O. de, Cardoso, J. K. F., Mendes, K. F., & Souza, J. J. L. de. (2023). Agricultural Soils: Impacts on the Environment. In Sousa, R. N. de , Pessoa, T. N. & Mendes, K. F. (Eds.), Agricultural soils: Impacts on the Environment (pp. 140–180). Environmental Remediation Technologies, Regulations and Safety; Air, Water and Soil Pollution Science and Technology. https://doi.org/10.52305/VXLZ8058
Caixeta, D., Caixeta, F., & Menezes Filho, F. (2018, June 20). Nano e microplásticos nos ecossistemas: impactos ambientais e efeitos sobre os organismos. Enciclopédia Biosfera, 15(27), 19–34. https://doi.org/10.18677/encibio_2018a92
Choi, B., Gil, D., Lee, J. J., & Kim, C. (2024). Selective visual staining of polyurethane microplastics by novel colorimetric and near-infrared (NIR) fluorescent dye: Application to environmental water and natural soil samples. Journal of Hazardous Materials, 471, 134332. https://doi.org/10.1016/j.jhazmat.2024.134332
Çobanoğlu, H., Belivermiş, M., Sıkdokur, E., Kılıç, N., & Çayır, A. (2021). Genotoxic and cytotoxic effects of polyethylene microplastics on human peripheral blood lymphocytes. Chemosphere, 272, 129805. https://doi.org/10.1016/j.chemosphere.2021.129805
Conforti, M., Matteucci, G., & Buttafuoco, G. (2017). Using laboratory Vis-NIR spectroscopy for monitoring some forest soil properties. Journal of Soils and Sediments, 18(3), 1009–1019. https://doi.org/10.1007/s11368-017-1766-5
Corradini, F., Bartholomeus, H., Huerta Lwanga, E., Gertsen, H., & Geissen, V. (2019). Predicting soil microplastic concentration using vis-NIR spectroscopy. Science of the Total Environment, 650, 922–932. https://doi.org/10.1016/j.scitotenv.2018.09.101
de Souza Machado, A. A., Lau, C. W., Kloas, W., Bergmann, J., Bachelier, J. B., Faltin, E., Becker, R., Görlich, A. S., & Rillig, M. C. (2019). Microplastics can change soil properties and affect plant performance. Environmental Science and Technology, 53(10), 6044–6052. https://doi.org/10.1021/acs.est.9b01339
Demattê, J. A. M., Nanni, M. R., da Silva, A. P., de Melo Filho, J. F., Dos Santos, W. C., & Campos, R. C. (2010). Soil density evaluated by spectral reflectance as an evidence of compaction effects. International Journal of Remote Sensing, 31(2), 403–422. https://doi.org/10.1080/01431160902893469
Dris, R., Gasperi, J., Mirande, C., Mandin, C., Guerrouache, M., Langlois, V., & Tassin, B. (2017). A first overview of textile fibers, including microplastics, in indoor and outdoor environments. Environmental Pollution, 221, 453–458. https://doi.org/10.1016/j.envpol.2016.12.013
Fournier, E., Leveque, M., Ruiz, P., Ratel, J., Durif, C., Chalancon, S., Amiard, F., Edely, M., Bezirard, V., Gaultier, E., Lamas, B., Houdeau, E., Lagarde, F., Engel, E., Etienne-Mesmin, L., Blanquet-Diot, S., & Mercier-Bonin, M. (2023). Microplastics: What happens in the human digestive tract? First evidences in adults using in vitro gut models. Journal of Hazardous Materials, 442, 130010. https://doi.org/10.1016/j.jhazmat.2022.130010
Gandariasbeitia, M., Besga, G., Albizu, I., Larregla, S., & Mendarte, S. (2017). Prediction of chemical and biological variables of soil in grazing areas with visible- and near-infrared spectroscopy. Geoderma, 305, 228–235. https://doi.org/10.1016/j.geoderma.2017.05.045
He, D., Luo, Y., Lu, S., Liu, M., Song, Y., & Lei, L. (2018). Microplastics in soils: Analytical methods, pollution characteristics and ecological risks. TrAC Trends in Analytical Chemistry, 109, 163–172. https://doi.org/10.1016/j.trac.2018.10.006
He, S., Wei, Y., Yang, C., & He, Z. (2022). Interactions of microplastics and soil pollutants in soil-plant systems. Environmental Pollution, 315, 120357. https://doi.org/10.1016/j.envpol.2022.120357
Heffernan, A., Gomez-Ramos, M., Symeonides, C., Hare, D., Vijayasarathy, S., Thompson, K., Mueller, J., Ponsonby, A., & Sly, P. (2020). Harmonizing analytical chemistry and clinical epidemiology for human biomonitoring studies. A case-study of plastic product chemicals in urine. Chemosphere, 238, 124631. https://doi.org/10.1016/j.chemosphere.2019.124631
Jacob, O., Stefaniak, E. A., Seghers, J., La Spina, R., Schirinzi, G. F., Chatzipanagis, K., Held, A., Emteborg, H., Koeber, R., Elsner, M., & Ivleva, N. P. (2024). Towards a reference material for microplastics’ number concentration—Case study of PET in water using Raman microspectroscopy. Analytical and Bioanalytical Chemistry/analytical & Bioanalytical Chemistry. https://doi.org/10.1007/s00216-024-05251-7
Kim, Y. N., Yoon, J. H., & Kim, K. H. (2021). Microplastic contamination in soil environment—A review. Soil Science Annual, 71(4), 300–308. https://doi.org/10.37501/soilsa/131646
Kuhn, M. (2008). Building Predictive Models inRUsing thecaretPackage. Journal of Statistical Software, 28(5). https://doi.org/10.18637/jss.v028.i05
Kurniawan, S. B., Abdullah, S. R. S., Imron, M. F., & Ismail, N. I. (2021, January). Current state of marine plastic pollution and its technology for more eminent evidence: A review. Journal of Cleaner Production, 278, 123537. https://doi.org/10.1016/j.jclepro.2020.123537
Kurzweg, L., Hauffe, M., Schirrmeister, S., Adomat, Y., Socher, M., Grischek, T., Fery, A., & Harre, K. (2024). Microplastic analysis in sediments of the Elbe River by electrostatic separation and differential scanning calorimetry. Science of the Total Environment, 172514. https://doi.org/10.1016/j.scitotenv.2024.172514
Li, L., Li, M., Deng, H., Cai, L., Cai, H., Yan, B., Hu, J., & Shi, H. (2018). A straightforward method for measuring the range of apparent density of microplastics. Science of the Total Environment, 639, 367–373. https://doi.org/10.1016/j.scitotenv.2018.05.166
Li, W., Wufuer, R., Duo, J., Wang, S., Luo, Y., Zhang, D., & Pan, X. (2020). Microplastics in agricultural soils: Extraction and characterization after different periods of polythene film mulching in an arid region. Science of the Total Environment, 749, 141420. https://doi.org/10.1016/j.scitotenv.2020.141420
Medeiros, A. D. D., Silva, L. J. D., Ribeiro, J. P. O., Ferreira, K. C., Rosas, J. T. F., Santos, A. A., & Silva, C. B. D. (2020). Machine learning for seed quality classification: An advanced approach using merger data from FT-NIR spectroscopy and X-ray imaging. Sensors, 20(15), 4319. https://doi.org/10.3390/s20154319
Montagner, C., Dias, M., Paiva, E., & Vidal, C. (2021). Microplásticos: Ocorrência Ambiental e Desafios Analíticos. Química Nova, 44, 1328–1352.
Otsu, N. (1979). A threshold selection method from gray-level histograms. IEEE Transactions on Systems, Man, and Cybernetics, 9(1), 62–66. https://doi.org/10.1109/tsmc.1979.4310076
Park, H., & Crozier, K. B. (2013). Multispectral imaging with vertical silicon nanowires. Scientific Reports, 3(1). https://doi.org/10.1038/srep02460
Paul, A., Wander, L., Becker, R., Goedecke, C., & Braun, U. (2018). High-throughput NIR spectroscopic (NIRS) detection of microplastics in soil. Environmental Science and Pollution Research, 26(8), 7364–7374. https://doi.org/10.1007/s11356-018-2180-2
Persiani, E., Cecchettini, A., Ceccherini, E., Gisone, I., Morales, M. A., & Vozzi, F. (2023). Microplastics: a matter of the heart (and vascular system). Biomedicines, 11(2), 264. https://doi.org/10.3390/biomedicines11020264
Piccini, C., Metzger, K., Debaene, G., Stenberg, B., Götzinger, S., Borůvka, L., Sandén, T., Bragazza, L., & Liebisch, F. (2024). In‐field soil spectroscopy in Vis–NIR range for fast and reliable soil analysis: A review. European Journal of Soil Science, 75(2). https://doi.org/10.1111/ejss.13481
Pivokonsky, M., Cermakova, L., Novotna, K., Peer, P., Cajthaml, T., & Janda, V. (2018). Occurrence of microplastics in raw and treated drinking water. Science of the Total Environment, 643, 1644–1651. https://doi.org/10.1016/j.scitotenv.2018.08.102
Qi, Y., Yang, X., Pelaez, A. M., Huerta Lwanga, E., Beriot, N., Gertsen, H., Garbeva, P., & Geissen, V. (2018). Macro- and micro- plastics in soil-plant system: Effects of plastic mulch film residues on wheat (Triticum aestivum) growth. Science of the Total Environment, 645, 1048–1056. https://doi.org/10.1016/j.scitotenv.2018.07.229
Rezaei, M., Riksen, M. J., Sirjani, E., Sameni, A., & Geissen, V. (2019). Wind erosion as a driver for transport of light density microplastics. Science of the Total Environment, 669, 273–281. https://doi.org/10.1016/j.scitotenv.2019.02.382
Rillig, M. C., & Lehmann, A. (2020). Microplastic in terrestrial ecosystems. Science, 368(6498), 1430–1431. https://doi.org/10.1126/science.abb5979
Rillig, M. C., Leifheit, E., & Lehmann, J. (2021). Microplastic effects on carbon cycling processes in soils. PLOS Biology, 19(3), e3001130. https://doi.org/10.1371/journal.pbio.3001130
Savitzky, A., & Golay, M. J. E. (1964). Smoothing and differentiation of data by simplified least squares procedures. Analytical Chemistry, 36(8), 1627–1639. https://doi.org/10.1021/ac60214a047
Senathirajah, K., Attwood, S., Bhagwat, G., Carbery, M., Wilson, S., & Palanisami, T. (2021). Estimation of the mass of microplastics ingested—A pivotal first step towards human health risk assessment. Journal of Hazardous Materials, 404, 124004. https://doi.org/10.1016/j.jhazmat.2020.124004
Shan, J., Zhao, J., Liu, L., Zhang, Y., Wang, X., & Wu, F. (2018). A novel way to rapidly monitor microplastics in soil by hyperspectral imaging technology and chemometrics. Environmental Pollution, 238, 121–129. https://doi.org/10.1016/j.envpol.2018.03.026
Silva, V. H., Murphy, F., Amigo, J. M., Stedmon, C., & Strand, J. (2020). Classification and quantification of microplastics (<100 μm) using a focal plane array-fourier transform infrared imaging system and machine learning. Analytical Chemistry, 92(20), 13724–13733. https://doi.org/10.1021/acs.analchem.0c01324
Souza Machado, A. A., Lau, C. W., Till, J., Kloas, W., Lehmann, A., Becker, R., & Rillig, M. C. (2018). Impacts of microplastics on the soil biophysical environment. Environmental Science and Technology, 52(17), 9656–9665. https://doi.org/10.1021/acs.est.8b02212
Stuart, B. H. (2004). Infrared spectroscopy: Fundamentals and applications (p. 248). John Wiley & Sons.
Tatem, A., Goetz, S., & Hay, S. (2008). Fifty years of earth-observation satellites. American Scientist, 96(5), 390. https://doi.org/10.1511/2008.74.390
Thompson, R. C., Olsen, Y., Mitchell, R. P., Davis, A., Rowland, S. J., John, A. W. G., McGonigle, D., & Russell, A. E. (2004). Lost at sea: Where is all the plastic? Science, 304(5672), 838–838. https://doi.org/10.1126/science.1094559
Vignesh, K., Prapanchan, V., Selvan, V. I., Karmegam, N., Kim, W., Barcelo, D., & Govarthanan, M. (2024). Microplastics, their abundance, and distribution in water and sediments in North Chennai, India: An assessment of pollution risk and human health impacts. Journal of Contaminant Hydrology, 263, 104339. https://doi.org/10.1016/j.jconhyd.2024.104339
Viscarra Rossel, R., Behrens, T., Ben-Dor, E., Brown, D., Demattê, J., Shepherd, K., Shi, Z., Stenberg, B., Stevens, A., Adamchuk, V., Aïchi, H., Barthès, B., Bartholomeus, H., Bayer, A., Bernoux, M., Böttcher, K., Brodský, L., Du, C., Chappell, A., & Ji, W. (2016). A global spectral library to characterize the world’s soil. Earth-Science Reviews, 155, 198–230. https://doi.org/10.1016/j.earscirev.2016.01.012
**ao, M., Shahbaz, M., Liang, Y., Yang, J., Wang, S., Chadwicka, D. R., Jones, D., Chen, J., & Ge, T. (2021). Effect of microplastics on organic matter decomposition in paddy soil amended with crop residues and labile C: A three-source-partitioning study. Journal of Hazardous Materials, 416, 126221. https://doi.org/10.1016/j.jhazmat.2021.126221
Xu, J., Yang, A., Yan, Y., Xu, Y., Tang, M., Li, P., Zhao, L., Zhang, X., & Ren, Z. (2024). Quantification and Identification of Microplastics in Organic Fertilizers: The Implication for the Manufacture and Safe Application. Water, Air and Soil Pollution, 235(3). https://doi.org/10.1007/s11270-024-06977-x
Zhang, B., Wu, D., Yang, X., Teng, J., Liu, Y., Zhang, C., Zhao, J., Yin, X., You, L., Liu, Y., & Wang, Q. (2019). Microplastic pollution in the surface sediments collected from Sishili Bay, North Yellow Sea, China. Marine Pollution Bulletin, 141, 9–15. https://doi.org/10.1016/j.marpolbul.2019.02.021
Zhang, Y., Zhang, X., Li, X., & He, D. (2022). Interaction of microplastics and soil animals in agricultural ecosystems. Current Opinion in Environmental Science and Health, 26, 100327. https://doi.org/10.1016/j.coesh.2022.100327
Zhao, S., Li, J., Xue, X., Sun, D., Liu, W., Zhu, C., Yang, Y., & **e, X. (2023). Molecular characteristics of natural organic matter in the groundwater system with geogenic iodine contamination in the Datong Basin, Northern China. Chemosphere, 333, 138834. https://doi.org/10.1016/j.chemosphere.2023.138834
Zhao, S., Zhang, Z., Chen, L., Cui, Q., Cui, Y., Song, D., & Fang, L. (2022). Review on migration, transformation and ecological impacts of microplastics in soil. Applied Soil Ecology, 176, 104486. https://doi.org/10.1016/j.apsoil.2022.104486
Acknowledgements
The authors would like to thank the São Paulo Research Foundation (FAPESP, 2024/08299-0) and Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq).
Funding
The authors have not disclosed any funding.
Author information
Authors and Affiliations
Contributions
MGDSB, BGN, ADCL, AGG, RCDS, DCFDSS, and KFM conceived and designed the experiments. MGDSB, BGN, ADCL, AGG, RCDS, DCFDSS, and KFM performed the experiments. AB, FG, and EF planned and conducted the simulations. MGDSB, BGN, ADCL, AGG, RCDS, DCFDSS, and KFM contributed to sample preparation. MGDSB, BGN, RCDS, and KFM contributed to the interpretation of results. MGDSB took the lead in manuscript writing. All authors provided critical feedback and assisted in sha** the research, analysis, and manuscript.
Corresponding author
Ethics declarations
Conflict of interest
The authors declare no competing interests.
Additional information
Publisher's Note
Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.
Rights and permissions
Springer Nature or its licensor (e.g. a society or other partner) holds exclusive rights to this article under a publishing agreement with the author(s) or other rightsholder(s); author self-archiving of the accepted manuscript version of this article is solely governed by the terms of such publishing agreement and applicable law.
About this article
Cite this article
da Silva Brochado, M.G., de Noronha, B.G., da Costa Lima, A. et al. What is the most effective analytical method for quantification and identification of microplastics in contaminated soils?. Environ Geochem Health 46, 260 (2024). https://doi.org/10.1007/s10653-024-02082-4
Received:
Accepted:
Published:
DOI: https://doi.org/10.1007/s10653-024-02082-4