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One of the main challenges in this field is the absence of standardized methods, reference materials, and comparative data. This study aimed to develop, optimize, and validate a methodological framework for the extraction and identification of MPs in wastewater matrices. Reference MPs were produced from the polymers such as polyethylene terephthalate (PET), high-density polyethylene (HDPE), low-density polyethylene (LDPE), polyvinyl chloride (PVC), polypropylene (PP), and polystyrene (PS). To evaluate the integrity of these MPs after digestion, five Fenton reagent protocols were tested, and the carbonyl index was applied. For density-based separation, sodium chloride (NaCl) and zinc chloride (ZnCl\n                    <jats:sub>2<\/jats:sub>\n                    ) solutions at different concentrations were used in a density separation device. The MPs obtained presented irregular fragments ranging from 0.1 to 3.0\u00a0mm. FTIR analysis performed before and after Fenton digestion showed no significant spectral deviations. The optimal Fenton conditions involved temperatures between 40 and 60\u00a0\u00b0C and 2\u00a0h of reaction time. ZnCl\n                    <jats:sub>2<\/jats:sub>\n                    provided the best performance for particle recovery, ensuring high separation efficiency. The optimized methodology was subsequently validated using raw wastewater and dewatered sewage sludge collected from a full-scale WWTP. The validation demonstrated effective organic matter removal, successful recovery of spiked MPs, and reliable identification of native MPs present in the environmental samples. Overall, the proposed methodology proved to be a robust and reliable approach for the extraction and characterization of MPs in complex wastewater matrices, providing methodological support for future monitoring programs and contributing to the development of standardized protocols for MPs analysis.\n                  <\/jats:p>","DOI":"10.1007\/s00244-026-01208-2","type":"journal-article","created":{"date-parts":[[2026,7,21]],"date-time":"2026-07-21T10:22:24Z","timestamp":1784629344000},"update-policy":"https:\/\/doi.org\/10.1007\/springer_crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Development of a Methodology for Analyzing Microplastics in Sewage Treatment Plants"],"prefix":"10.1007","volume":"91","author":[{"ORCID":"https:\/\/orcid.org\/0009-0005-4778-680X","authenticated-orcid":false,"given":"Ivanilson","family":"da Silva de Aquino","sequence":"first","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-1917-7821","authenticated-orcid":false,"given":"Otilie Eichler","family":"Vercillo","sequence":"additional","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8515-7888","authenticated-orcid":false,"given":"Wellington Marcos","family":"da Silva","sequence":"additional","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-0449-9219","authenticated-orcid":false,"given":"Alisson Mendes","family":"Rodrigues","sequence":"additional","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-5388-6165","authenticated-orcid":false,"given":"Ariuska Karla Barbosa","family":"Amorim","sequence":"additional","affiliation":[],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"297","published-online":{"date-parts":[[2026,7,21]]},"reference":[{"key":"1208_CR1","doi-asserted-by":"publisher","first-page":"142206","DOI":"10.1016\/j.chemosphere.2024.142206","volume":"359","author":"A Al-Amri","year":"2024","unstructured":"Al-Amri A, Yavari Z, Reza Nikoo M, Karimi M (2024) Microplastics removal efficiency and risk analysis of wastewater treatment plants in Oman. 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