Evaluation of poly(styrene-d5) and poly(4-fluorostyrene) as internal standards for microplastics quantification by thermoanalytical methods

Lauschke, Tim; Dierkes, Georg; Schweyen, Peter; Ternes, Thomas A.

doi:10.1016/j.jaap.2021.105310

Cited by 20 publications

(4 citation statements)

References 28 publications

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“…Especially, PS-d 5 is increasingly used as an internal pyrolysis standard. Nevertheless, it was recently shown that this deuterated polymer can lead to HD exchange during pyrolysis, notably in the presence of mineral matrices such as alumina filters or sand [53]. Therefore, the authors suggested using a specific polymer, poly(4-fluorostyrene), given its physicochemical properties being close to PS.…”

Section: Discussionmentioning

confidence: 99%

Quantification of Microplastics by Pyrolysis Coupled with Gas Chromatography and Mass Spectrometry in Sediments: Challenges and Implications

et al. 2022

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Pyrolysis-GC/MS is increasingly used to quantify microplastics (MP) in environmental samples. In general, prior to analysis, purification steps are carried out to reduce the environmental matrix in sediment samples. The conventionally used protocol of density separation followed by digestion of organic matter does not allow for complete isolation of MP from the associated organic and mineral matter. Among the pyrolysis products used as indicator compounds for plastic polymers, some may originate from other substances present in the environmental samples. In this paper, the indicator compounds are reviewed for the most common polymers: PE, PP, PS, PET and PVC and selected taking into account potential interactions with substances present in environmental matrices. Even after a purification step, a residual mineral fraction remains in a sediment sample, including matrix effects. This effect may be positive or negative, depending on the investigated polymer and is thus important to consider when using Pyr-GC/MS for the quantification of MP in sediment samples. It also shows that no external calibration can be used to reliably quantify MP in such samples and that the use of internal standards is compulsory.

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Section: Discussionmentioning

confidence: 99%

Quantification of Microplastics by Pyrolysis Coupled with Gas Chromatography and Mass Spectrometry in Sediments: Challenges and Implications

et al. 2022

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“…Internal standard of poly(styrene-(phenyl-13 C 6 )) ( 13 C 6 -PS) (Merck KGaA) was used, since it is also a polymer, and the pyrolytic behavior is included in this. The internal standard d5-PS, which was used more frequently in the past, is not used because of the hydrogen-deuterium exchange that occurs [28]. TED-GC/MS measurements were done like previously described in literature [29,30].…”

Section: Methodsmentioning

confidence: 99%

Microplastics in sediments of the river Rhine—A workflow for preparation and analysis of sediment samples from aquatic river systems for monitoring purposes

et al. 2023

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Microplastics (MP) can be detected in all environmental systems. Marine and terrestrial aquatic systems, especially the transported suspended solids, have often been the focus of scientific investigations in the past. Sediments of aquatic river systems, on the other hand, were often ignored due to the time‐consuming sample preparation and analysis procedures. Spectroscopic measurement methods counting particle numbers are hardly suitable as detection methods, because there are plenty of natural particles next to a small number of MP particles. Integral methods, such as thermoanalytical methods are determining the particle mass independently of the inorganic components.In this study, a workflow for sample preparation via density separation and subsequent analysis by thermal extraction desorption‐gas chromatography/mass spectrometry is presented, which leads to representative and homogeneous samples and allows fast and robust MP mass content measurements suitable for routine analysis. Polymers were identified and quantified in all samples. Polyethylene and styrene‐butadiene rubber are the dominant polymers, besides polypropylene and polystyrene. Overall, total polymer masses between 1.18 and 337.0 µg/g could be determined. Highest MP concentrations in riverbed sediment are found in sites characterized by low flow velocities in harbors and reservoirs, while MP concentrations in sandy/gravelly bed sediments with higher flow velocities are small.

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“… 16 − 22 However, these thermoanalytical methods are still under development and suffer from matrix interferences and false-positive results. 13 , 16 , 23 − 25 For instance, natural compounds from coniferous trees could lead to PE overquantifications. 26 Furthermore, in the case of PS, Fischer et al showed possible overdeterminations by phenylalanine from proteins during pyrolysis-GC-MS. 27 Regarding PVC, in the current literature, using pyrolysis or TGA, PVC, benzene, or naphthalene has often been used as a quantifier.…”

Section: Introductionmentioning

confidence: 99%

“…In recent years, different optical analytical methods, such as microscopy, Raman spectroscopy, or Fourier transform infrared spectroscopy, have been used for the identification of various types of plastic particles. − Also, analytical methods using mass spectrometry in environmental samples have been developed for different polymer types, such as polyethylene (PE), polypropylene (PP), polystyrene (PS), poly(vinyl chloride) (PVC), poly(ethylene terephthalate) (PET), polycarbonate (PC), or poly(methylmethacrylate) (PMMA) as well as their additives. − Primarily, pyrolysis or thermogravimetric analysis (TGA) has been coupled with gas chromatograpy/mass spectrometry (GC-MS). − However, these thermoanalytical methods are still under development and suffer from matrix interferences and false-positive results. ,,− For instance, natural compounds from coniferous trees could lead to PE overquantifications . Furthermore, in the case of PS, Fischer et al showed possible overdeterminations by phenylalanine from proteins during pyrolysis-GC-MS .…”

Section: Introductionmentioning

confidence: 99%

Quantification of Poly(vinyl chloride) Microplastics via Pressurized Liquid Extraction and Combustion Ion Chromatography

Kamp

Dierkes

Schweyen

et al. 2023

Environ. Sci. Technol.

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A reliable analytical method has been developed to quantify poly(vinyl chloride) (PVC) in environmental samples. Quantification was conducted via combustion ion chromatography (C-IC). Hydrogen chloride (HCl) was quantitatively released from PVC during thermal decomposition and trapped in an absorption solution. Selectivity of the marker HCl in complex environmental samples was ensured using cleanup via pressurized liquid extraction (PLE) with methanol at 100 °C (discarded) and tetrahydrofuran at 185 °C (collected). Using this method, recoveries of 85.5 ± 11.5% and a limit of quantification down to 8.3 μg/g were achieved. A variety of hard and soft PVC products could be successfully analyzed via C-IC with recoveries exceeding >95%. Furthermore, no measurable overdetermination was found for various organic and inorganic matrix ingredients, such as sodium chloride, sucralose, hydroxychloroquine, diclofenac, chloramphenicol, triclosan, or polychlorinated biphenyls. In addition, sediments and suspended particular matter showed PVC concentrations ranging up to 16.0 and 220 μg/g, respectively. However, the gap between determined polymer mass and particle masses could be significant since soft PVC products contain plasticizers up to 50 wt %. Hence, the results of the described method represent a sum of all chlorine-containing polymers, which are extractable under the chosen conditions.

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Evaluation of poly(styrene-d5) and poly(4-fluorostyrene) as internal standards for microplastics quantification by thermoanalytical methods

Cited by 20 publications

References 28 publications

Quantification of Microplastics by Pyrolysis Coupled with Gas Chromatography and Mass Spectrometry in Sediments: Challenges and Implications

Quantification of Microplastics by Pyrolysis Coupled with Gas Chromatography and Mass Spectrometry in Sediments: Challenges and Implications

Microplastics in sediments of the river Rhine—A workflow for preparation and analysis of sediment samples from aquatic river systems for monitoring purposes

Quantification of Poly(vinyl chloride) Microplastics via Pressurized Liquid Extraction and Combustion Ion Chromatography

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