Microwave-assisted solvent extraction and double-shot analytical pyrolysis for the quali-quantitation of plasticizers and microplastics in beach sand samples

Nasa, Jacopo La; Biale, Greta; Mattonai, Marco; Modugno, Francesca

doi:10.1016/j.jhazmat.2020.123287

Cited by 51 publications

(43 citation statements)

References 36 publications

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“…The EGA-MS analyses of unaged and artificially aged bulk polymers were performed with an EGA/PY-3030D micro-furnace pyrolyzer (Frontier Laboratories Ltd., Koriyama, Japan) coupled to a 6890 gas chromatograph and a 5973 mass spectrometric detector (Agilent Technologies, Santa Clara, CA, USA). The experimental conditions were the following: temperature ramp for the furnace from 50 °C to 700 °C at 10 °C/min; interface between the pyrolysis furnace and the GC–MS system set at a temperature 100 °C higher than that of the furnace but limited to a maximum of 300 °C; GC injector operated in split mode (20:1 ratio) at 280 °C [ 25 , 26 ]. The evolved pyrolysis products were directly sent to the mass spectrometer using a UADTM-2.5N deactivated stainless-steel capillary tube (3 m × 0.15 mm, Frontier Laboratories Ltd., Japan) held at 300 °C, and using helium (1 mL/min) as the carrier gas.…”

Section: Methodsmentioning

confidence: 99%

“…The samples (50–100 μg) were placed in deactivated stainless-steel sample cups. Pyrolysis conditions were optimized as follows: pyrolysis temperatures were selected based on the samples analyzed [ 25 , 26 , 27 ]; interface 280 °C; GC injector temperature 280 °C; GC injection operated in split mode with an optimized 10:1 split ratio. The chromatographic separation of the pyrolysis products was performed on a fused silica capillary column HP-5MS (5% diphenyl–95% dimethyl-polysiloxane, 30 m × 0.25 mm internal diameter., 0.25 μm film thickness, J&W Scientific, Agilent Technologies) preceded by a deactivated fused silica pre-column (2 m × 0.32 mm i.d.).…”

Section: Methodsmentioning

confidence: 99%

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A Systematic Study on the Degradation Products Generated from Artificially Aged Microplastics

et al. 2021

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Most of the analytical studies focused on microplastics (MPs) are based on the detection and identification of the polymers constituting the particles. On the other hand, plastic debris in the environment undergoes chemical and physical degradation processes leading not only to mechanical but also to molecular fragmentation quickly resulting in the formation of leachable, soluble and/or volatile degradation products that are released in the environment. We performed the analysis of reference MPs–polymer micropowders obtained by grinding a set of five polymer types down to final size in the 857–509 μm range, namely high- and low-density polyethylene, polystyrene (PS), polypropylene (PP), and polyethylene terephthalate (PET). The reference MPs were artificially aged in a solar-box to investigate their degradation processes by characterizing the aged (photo-oxidized) MPs and their low molecular weight and/or highly oxidized fraction. For this purpose, the artificially aged MPs were subjected to extraction in polar organic solvents, targeting selective recovery of the low molecular weight fractions generated during the artificial aging. Analysis of the extractable fractions and of the residues was carried out by a multi-technique approach combining evolved gas analysis–mass spectrometry (EGA–MS), pyrolysis–gas chromatography–mass spectrometry (Py–GC–MS), and size exclusion chromatography (SEC). The results provided information on the degradation products formed during accelerated aging. Up to 18 wt% of extractable, low molecular weight fraction was recovered from the photo-aged MPs, depending on the polymer type. The photo-degradation products of polyolefins (PE and PP) included a wide range of long chain alcohols, aldehydes, ketones, carboxylic acids, and hydroxy acids, as detected in the soluble fractions of aged samples. SEC analyses also showed a marked decrease in the average molecular weight of PP polymer chains, whereas cross-linking was observed in the case of PS. The most abundant low molecular weight photo-degradation products of PS were benzoic acid and 1,4-benzenedicarboxylic acid, while PET had the highest stability towards aging, as indicated by the modest generation of low molecular weight species.

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Section: Methodsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

A Systematic Study on the Degradation Products Generated from Artificially Aged Microplastics

et al. 2021

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“…Once the thermal zones of interest are obtained, appropriate pyrolysis temperature can be selected based on the EGA profile. Compounds can be identified according to the mass spectrum information and the ions present in a thermal region, (La Nasa et al, 2018;La Nasa et al, 2021).…”

Section: Onmentioning

confidence: 99%

Identification and quantification of plastic additives using pyrolysis-GC/MS: A review

Akoueson

Chbib

Monchy

et al. 2021

Science of The Total Environment

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HAL is a multi-disciplinary open access archive for the deposit and dissemination of scientific research documents, whether they are published or not. The documents may come from teaching and research institutions in France or abroad, or from public or private research centers. L'archive ouverte pluridisciplinaire HAL, est destinée au dépôt et à la diffusion de documents scientifiques de niveau recherche, publiés ou non, émanant des établissements d'enseignement et de recherche français ou étrangers, des laboratoires publics ou privés.

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“…Analyses were performed using a multi-shot pyrolyzer EGA/PY-3030D (Frontier Lab, Japan) coupled with a 6890N gas chromatographic system with a split/splitless injection port and combined with a 5973-mass selective single quadrupole mass spectrometer (Agilent Technologies, USA). For the analysis of the extracts, 100-150 µL of solution were placed in stainless steel cups together with 2.0 µL of a solution of dibutyl phthalate-3,4,5,6-d4 (500 ppm), and dried under nitrogen steam prior to the analyses [28]. The temperatures used for the double shot pyrolysis were 350 °C and 600°C while the interface was set at 280°C.…”

Section: Analytical Techniquesmentioning

confidence: 99%

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

Castelvetro¹,

Corti²,

Nasa³

et al. 2021

Preprint

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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 &lt;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.

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Microwave-assisted solvent extraction and double-shot analytical pyrolysis for the quali-quantitation of plasticizers and microplastics in beach sand samples

Cited by 51 publications

References 36 publications

A Systematic Study on the Degradation Products Generated from Artificially Aged Microplastics

A Systematic Study on the Degradation Products Generated from Artificially Aged Microplastics

Identification and quantification of plastic additives using pyrolysis-GC/MS: A review

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

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