Automated thermal extraction-desorption gas chromatography mass spectrometry: A multifunctional tool for comprehensive characterization of polymers and their degradation products

Duemichen, Erik; Eisentraut, Paul; Celina, Mathias C.; Braun, Ulrike

doi:10.1016/j.chroma.2019.01.033

Cited by 152 publications

(101 citation statements)

References 25 publications

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“…For the desorption process the loaded solid phase was transported by the autosampler to the thermal desorption gas chromatograph 7890 GC System with mass spectrometer 5977B MSD (Agilent Technologies, USA). The detailed conditions of the GC/MS measurements and further information on the TED-GC/MS can be found elsewhere 39,40 . In this study no internal standard was applied and no quantification was carried out.…”

Section: Evolved Gas Analysesmentioning

confidence: 99%

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Specific adsorption sites and conditions derived by thermal decomposition of activated carbons and adsorbed carbamazepine

Dittmann

Eisentraut

Goedecke

et al. 2020

Sci Rep

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The adsorption of organic micropollutants onto activated carbon is a favourable solution for the treatment of drinking water and wastewater. However, these adsorption processes are not sufficiently understood to allow for the appropriate prediction of removal processes. In this study, thermogravimetric analysis, alongside evolved gas analysis, is proposed for the characterisation of micropollutants adsorbed on activated carbon. Varying amounts of carbamazepine were adsorbed onto three different activated carbons, which were subsequently dried, and their thermal decomposition mechanisms examined. The discovery of 55 different pyrolysis products allowed differentiations to be made between specific adsorption sites and conditions. However, the same adsorption mechanisms were found for all samples, which were enhanced by inorganic constituents and oxygen containing surface groups. Furthermore, increasing the loadings led to the evolution of more hydrated decomposition products, whilst parts of the carbamazepine molecules were also integrated into the carbon structure. It was also found that the chemical composition, especially the degree of dehydration of the activated carbon, plays an important role in the adsorption of carbamazepine. Hence, it is thought that the adsorption sites may have a higher adsorption energy for specific adsorbates, when the activated carbon can then potentially increase its degree of graphitisation. Increasing amounts of pharmaceuticals enter the water bodies and are detected all over the world 1-3. Many of them are persistent and may accumulate within water cycles 4-6. These organic micropollutants already show adverse effects in aquatic ecosystems despite their comparably low concentrations 7-9. Therefore, technical measures are introduced as advanced wastewater treatment 10. One of the favoured techniques is the removal by adsorption onto activated carbon 11,12. Activated carbon has been used in water purification for more than hundred years. In modern times, we face more ecological and economical challenges that require the accurate prediction of removal efficiencies prior to the upgrade of wastewater treatment plants. Hence, several approaches have been applied to gain fast and efficient predictions through laboratory experiments and the optimization of operating parameters through data driven modeling 13-16. The removal of the target substances has been shown to be strongly influenced by the composition of the waters and that of the activated carbons used in the removal 17,18. The underlying adsorption processes have been extensively described in theory and investigated experimentally 19,20. However, adsorption in the liquid phase has been proven to be much more complicated than adsorption in gas phases, especially in complex water matrices that are governed by the presence of dissolved organic matter, the ionic strength and the pH value 21-23. Hence, both the adsorbate solution and the adsorbent, are mutually influenced. Moreover, activated carbon has a highly heterogeneous pore stru...

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Section: Evolved Gas Analysesmentioning

confidence: 99%

“…I. Tetradecane (39) and the group of aliphatics (decomposition products without aromatic moieties) are released predominantly from the HK+CBZ-5 system. They are not detected in the systems with CCP 90D.…”

Section: Decomposition Mechanisms Of the 2 Nd Mass Loss Stagementioning

confidence: 99%

Specific adsorption sites and conditions derived by thermal decomposition of activated carbons and adsorbed carbamazepine

Dittmann

Eisentraut

Goedecke

et al. 2020

Sci Rep

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“…PS analysis via liquid chromatography/mass spectrometry with an atmospheric pressure photoionization source, for instance, resulted in an intra-and inter-day repeatability of 1.8-2.4 % and 15.5-25.6 %, respectively (n = 5; Schirinzi et al, 2019). With TED-GC/MS, Duemichen et al (2019) achieved RSDs ranging from 6 to 12 % for various PP pyrolysates. The authors suggested using an internal standard to further optimize RSDs.…”

Section: Repeatabilitymentioning

confidence: 99%

“…In such cases, thermoanalytical techniques such as thermogravimetry/mass spectrometry (David et al, 2018(David et al, , 2019, pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS; Scholz-Böttcher, 2017, 2019), or combinations of TGA with GC/MS namely thermal desorption-gas chromatography/mass spectrometry (TED-GC/MS; Dümichen et al, 2015;Duemichen et al, 2019) may demonstrate their inherent benefits. All these methods are based on thermal decomposition of polymer mixtures at temperatures >500 • C and their quantification via indicator pyrolysates.…”

Section: Introductionmentioning

confidence: 99%

“…All these methods are based on thermal decomposition of polymer mixtures at temperatures >500 • C and their quantification via indicator pyrolysates. Currently, instrumental detection limits range from 3 to 200 ng for PS (Fischer and Scholz-Böttcher, 2019;Duemichen et al, 2019) and up to 0.5-50 µg for PE, PP, and PET (Duemichen et al, 2019;David et al, 2018). In contrast to optical methods, thermoanalytical techniques are assumed to be more robust against impurities from sample matrix.…”

Section: Introductionmentioning

confidence: 99%

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A simple method for the selective quantification of polyethylene, polypropylene, and polystyrene plastic debris in soil by pyrolysis-gas chromatography/mass spectrometry

Steinmetz

Kintzi

Muñoz

et al. 2019

Preprint

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The lack of adequate analytical methods for the quantification of plastic debris in soil challenges a better understanding of their occurrence and fate in the terrestrial environment. With this proof-of-principle study, we developed a simple and fast method for the selective quantification of the three most environmentally relevant polymers polyethylene (PE), polypropylene (PP), and polystyrene (PS) in soil using pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS). In order to facilitate the preparation of calibration series and to better account for the heterogeneity of soil matrix, polymers were dissolved in 1,2,4-trichlorobenzene (TCB) at 120 °C. Thereby, liquid sample aliquots from up to 4 g of solid sample became amenable to pyrolysis without further preparation. To evaluate the performance of this approach, three reference soils with 1.73–5.16 % organic carbon (Corg) were spiked at 50 and 250 μg g−1 of each polymer and extracted with TCB. A prior cleanup step with methanol, flocculation with KAl(SO4)2, and Fenton digestion were tested for their suitability to reduce potentially interfering Corg. Calibration curves responded linearly (adj. R2 > 0.996) with instrumental detection limits of 1–86 ng corresponding to method detection limits of 1–86 μg g−1. The measurement repeatability was 3.2–7.2 % relative standard deviation. Recoveries of 70–128 % were achieved for plastic contents of 250 μg g−1 extracted with TCB without prior cleanup from soils with less than 2.5 % Corg. A higher Corg particularly interfered with the quantification of PE. The addition of non-target polymers (polyethylene terephthalate, polyvinyl chloride, poly(methyl methacrylate), and tire wear particles) did not interfere with the quantification of the analytes highlighting the selectivity of the method. Further research is needed to determine low plastic contents in soils exceeding 2.5 % Corg. With 1–3 h processing time per sample, our method has the potential for routine analyses and screening studies of agricultural systems to be complemented with microspectroscopic techniques for additional information on particle shapes and sizes.

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Techniques for Microplastics Detection in Urban Water Systems

Li²,

Liu³

et al. 2022

Microplastics in Urban Water Management

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Automated thermal extraction-desorption gas chromatography mass spectrometry: A multifunctional tool for comprehensive characterization of polymers and their degradation products

Cited by 152 publications

References 25 publications

Specific adsorption sites and conditions derived by thermal decomposition of activated carbons and adsorbed carbamazepine

Specific adsorption sites and conditions derived by thermal decomposition of activated carbons and adsorbed carbamazepine

A simple method for the selective quantification of polyethylene, polypropylene, and polystyrene plastic debris in soil by pyrolysis-gas chromatography/mass spectrometry

Techniques for Microplastics Detection in Urban Water Systems

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