Preprint Article Version 1 Preserved in Portico This version is not peer-reviewed

Polymer Identification and Specific Analysis (PISA) of Microplastic Total Mass in Sediments of the Protected Marine Area of the Meloria Shoals

Version 1 : Received: 7 February 2021 / Approved: 8 February 2021 / Online: 8 February 2021 (13:13:37 CET)

A peer-reviewed article of this Preprint also exists.

Castelvetro, V.; Corti, A.; La Nasa, J.; Modugno, F.; Ceccarini, A.; Giannarelli, S.; Vinciguerra, V.; Bertoldo, M. Polymer Identification and Specific Analysis (PISA) of Microplastic Total Mass in Sediments of the Protected Marine Area of the Meloria Shoals. Polymers 2021, 13, 796. Castelvetro, V.; Corti, A.; La Nasa, J.; Modugno, F.; Ceccarini, A.; Giannarelli, S.; Vinciguerra, V.; Bertoldo, M. Polymer Identification and Specific Analysis (PISA) of Microplastic Total Mass in Sediments of the Protected Marine Area of the Meloria Shoals. Polymers 2021, 13, 796.

Journal reference: Polymers 2021, 13, 796
DOI: 10.3390/polym13050796

Abstract

Microplastics (MPs) quantification in benthic marine sediments is typically performed by time-consuming and moderately accurate mechanical separation and microscopy detection. In this paper we describe the results of our innovative Polymer Identification and Specific Analysis (PISA) of microplastic total mass, previously tested on either less complex sandy beach sediment or less demanding (because of the high MPs content) wastewater treatment plant sludges, applied to the analysis of benthic sediments from a sublittoral area north-west of Leghorn (Tuscany, Italy). Samples were collected from two shallow sites characterized by coarse debris in a mixed seabed of Posidonia oceanica, and by a very fine silty-organogenic sediment, respectively. After sieving at <2 mm the sediment was sequentially extracted with selective organic solvents and the two polymer classes polystyrene (PS) and polyolefins (PE and PP) were quantified by pyrolysis-GC/MS. A contamination in the 8-65 ppm range by PS could be accurately detected. Acid hydrolysis on the extracted residue to achieve total depolymerization of all natural and synthetic polyamides, tagging of all aminated species in the hydrolyzate with a fluorophore, and reversed-phase HPLC (RP-HPLC) analysis, allowed to quantify within the 137-1523 ppm range the individual mass of contaminating Nylon 6 and Nylon 6,6, based on the detected amounts of the respective monomeric amines 6-aminohexanoic acid (AHA) and hexanediamine (HMDA). Finally, alkaline hydrolysis of the residue from acid hydrolysis followed by RP-HPLC analysis of the purified hydrolysate showed contamination by polyethylene terephthalate (PET) in the 12.1-2.7 ppm range, based on the content of its comonomer, terephthalic acid.

Subject Areas

microplastics; marine sediment; pet; nylon 6; nylon 6,6; reversed-phase HPLC; polyolefin; polystyrene; Pyr-GC/MS; polymer degradation

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