Abstract
Il progetto di ricerca DIORAMA mira a stabilire nuove linee guida nelle indagini analitiche sulle microplastiche (MP) e sulle MP invecchiate nelle matrici acquatiche, affrontando l'urgente necessità di implementare metodi analitici standardizzati e affidabili da applicare nelle campagne di monitoraggio. A questo scopo, il progetto valuterà l'alterazione delle caratteristiche fisico-chimiche delle MP nel tempo, con un particolare focus sui cambiamenti indotti dagli effetti di degradazione nei segnali analitici registrati. Il progetto indagherà gli effetti della morfologia, delle dimensioni e della composizione delle MP, nonché delle condizioni di invecchiamento, come fattori influenti in due diversi e complementari metodi analitici: l'imaging iperspettrale nel vicino infrarosso (NIR-HSI) e la pirolisi analitica accoppiata con la Cromatografia a Gas e la Spettrometria di Massa (Py-GC-MS). Verranno studiati i fattori sperimentali che influenzano l'efficacia e le prestazioni della rilevazione delle MP tramite NIR-HSI e pirolisi analitica per identificare le condizioni più adatte per monitorare la degradazione dei polimeri. I risultati metteranno in evidenza specifiche vie di degradazione, fornendo nuove informazioni sul comportamento delle MP nell'ambiente. La ricerca porterà alla definizione di protocolli armonizzati e integrati, proponendo nuove strategie negli studi analitici comparativi intra-laboratorio.
Results achieved
The DIORAMA (A Deep Dive into the Study of Microplastics in Aqueous Matrices) project successfully achieved its main objective of advancing analytical methodologies for the detection, characterization and monitoring of microplastics by integrating near-infrared hyperspectral imaging (NIR-HSI), pyrolysis–gas chromatography–mass spectrometry (Py-GC-MS), complementary spectroscopic techniques and advanced chemometric data analysis. The project provided a comprehensive understanding of how polymer composition, particle size, morphology and environmental aging influence the analytical response of different techniques, establishing a robust basis for the development of harmonized analytical protocols for microplastic analysis. A major achievement of the project was the preparation and characterization of a large collection of reference microplastic materials, including virgin polymers, microplastics derived from consumer products and tire wear particles. Artificial aging protocols based on controlled UV irradiation and outdoor weathering were successfully implemented to reproduce realistic environmental degradation processes, allowing the identification of spectral and thermal markers associated with polymer oxidation and degradation. Significant progress was also achieved in the optimization of analytical methodologies. Experimental conditions for NIR hyperspectral imaging and micro-FTIR imaging were optimized to improve the detection of aged microplastics while reducing acquisition times. In parallel, Py-GC-MS methodologies were optimized for both qualitative and quantitative analysis through the development of calibration models, the identification of diagnostic pyrolysis markers and the investigation of co-pyrolysis effects in polymer mixtures. The comparison between spectroscopic and pyrolytic approaches demonstrated the complementarity of the two techniques and enabled the definition of integrated analytical workflows for the characterization of both reference materials and real environmental samples. One of the most innovative outcomes of the project was the development of dedicated chemometric and image-processing strategies for automated microplastic detection. Several multivariate approaches, including Principal Component Analysis (PCA), Multivariate Curve Resolution (MCR), Normalized Difference Images (NDI) and SIMCA one-class classification models, were implemented to improve particle detection, background segmentation and polymer classification. Dedicated MATLAB routines enabled automated particle identification and counting, significantly improving the reliability and speed of spectral image analysis. The project also strengthened collaborations with several national and international research institutions, industrial partners and European research networks, including the COST Action PRIORITY, contributing to the harmonization of analytical methodologies for environmental microplastic monitoring. The developed protocols were successfully applied to real environmental samples provided through international collaborations, demonstrating their applicability beyond laboratory-prepared materials. The project also placed strong emphasis on dissemination and capacity building. Results were widely communicated through numerous oral and poster presentations at major international conferences, national scientific meetings, and specialized workshops, contributing to the visibility of the project within the analytical chemistry and environmental science communities. A particularly significant achievement was the organization of the international Training School "Chemometrics for Microplastics Detection and Monitoring", held at the University of Brescia in collaboration with the COST Action PRIORITY (CA20101). The school brought together early-career researchers and experts from several European countries, providing advanced training on hyperspectral imaging, chemometric data analysis, and supervised modelling for microplastic detection, while fostering knowledge exchange and strengthening the European research network on microplastic monitoring. Among the published papers, "Abiotic degradation and accelerated ageing of microplastics from biodegradable and recycled materials in artificial seawater" (Science of the Total Environment, 2024) provided new insights into polymer degradation mechanisms, while additional publications addressed methodological developments in chemometrics and hyperspectral imaging for advanced spectral analysis. Two further manuscripts focusing on integrated Mid-IR/NIR chemometric strategies and quantitative assessment of artificially aged microplastics are currently in preparation. Overall, the DIORAMA project successfully delivered innovative analytical methodologies, advanced chemometric tools and harmonized workflows for microplastic characterization. The integration of spectral imaging, analytical pyrolysis and data-driven approaches significantly improves the rapid, non-destructive and reliable identification of microplastics, providing valuable tools to support future environmental monitoring strategies and the standardization of analytical protocols for microplastic pollution assessment.Project details
Unibo Team Leader: Giorgia Sciutto
Unibo involved Department/s:
Dipartimento di Chimica "Giacomo Ciamician"
Coordinator:
ALMA MATER STUDIORUM - Università di Bologna(Italy)
Total Eu Contribution: Euro (EUR) 239.416,00
Total Unibo Contribution: Euro (EUR) 95.753,00
Project Duration in months: 27
Start Date:
30/11/2023
End Date:
28/02/2026
