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Optimized extraction, quantification and characterization of seven environmentally relevant metallic nanoparticles in sewage sludge: Occurrence, composition and environmental risk assessment

Lučić, Mavro; Milačič Ščančar, Radmila; Ščančar, Janez; Fiket, Željka; Arah, Bor; Vidmar, Janja (2025) Optimized extraction, quantification and characterization of seven environmentally relevant metallic nanoparticles in sewage sludge: Occurrence, composition and environmental risk assessment. Journal of Hazardous Materials, 497 . ISSN 0304-3894

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Abstract

The quantitative analysis of metallic nanoparticles (MNPs) in environmental matrices is crucial for understanding their occurrence, fate, and ecological risks. This study presents the protocol for extracting and quantifying seven environmentally relevant MNPs (Ag, Au, Ce, Cu, Pb, Ti and Zn NPs) from sewage sludge using single-particle inductively coupled plasma mass spectrometry (sp-ICP-MS). Several extraction parameters and solutions, including milli-Q water, tetrasodium pyrophosphate (TSPP), and tetramethylammonium hydroxide (TMAH), were systematically evaluated. TSPP at 2.5 mM in a 1:100 sludge-to-reagent ratio was identified as optimal, providing high particle number recovery (>75%) and mass recovery (>84.5%) while minimizing particle transformation. Application to Croatian wastewater treatment plant sludge samples resulted in particle concentrations of 1×107 to 3×1010 particles/g, with extracted MNPs representing <2% of total metal content for most elements. Scanning electron microscopy coupled with energy dispersive X-ray spectroscopy revealed that Ag, Cu, Pb, Ti and Zn-based NPs are possibly of anthropogenic origin, which was corroborated by enrichment factor analysis. Risk assessment indicated negligible to low ecological risks under current agricultural scenarios, though highly soluble species (Ag and Zn NPs) may pose greater long-term environmental risks. This methodology addresses critical gaps in environmental monitoring capabilities for engineered NPs.

Item Type: Article
Additional Information: Project: Slovenian Research and Innovation Agency – ARIS Program P1-0143
Uncontrolled Keywords: Metallic nanoparticle; Single-particle ICP-MS; Sewage sludge; Extraction optimization; Environmental risk assessment
Subjects: NATURAL SCIENCES > Chemistry
NATURAL SCIENCES > Chemistry > Analytic Chemistry
NATURAL SCIENCES > Chemistry > Inorganic Chemistry
NATURAL SCIENCES > Interdisciplinary Natural Sciences
NATURAL SCIENCES > Interdisciplinary Natural Sciences > Environmental Science
Divisions: Division for Marine and Enviromental Research
Projects:
Project titleProject leaderProject codeProject type
Program mobilnosti – odlazna mobilnost viših asistenataMavro LučićMOBODL-2023-08-5702HrZZ
Depositing User: Mavro Lučić
Date Deposited: 30 Oct 2025 08:47
URI: http://fulir.irb.hr/id/eprint/10104
DOI: 10.1016/j.jhazmat.2025.139734

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