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  • Veröffentlichung
    Fast identification of microplastics in complex environmental samples by a thermal degradation method
    (2017) Dümichen, Erik; Bannick, Claus Gerhard; Eisentraut, Paul; Barthel, Anne-Kathrin
    In order to determine the relevance of microplastic particles in various environmental media, comprehensive investigations are needed. However, no analytical method exists for fast identification and quantification. At present, optical spectroscopy methods like IR and RAMAN imaging are used. Due to their time consuming procedures and uncertain extrapolation, reliable monitoring is difficult. For analyzing polymers Py-GC-MS is a standard method. However, due to a limited sample amount of about 0.5 mg it is not suited for analysis of complex sample mixtures like environmental samples. Therefore, we developed a new thermoanalytical method as a first step for identifying microplastics in environmental samples. A sample amount of about 20 mg, which assures the homogeneity of the sample, is subjected to complete thermal decomposition. The specific degradation products of the respective polymer are adsorbed on a solid-phase adsorber and subsequently analyzed by thermal desorption gas chromatography mass spectrometry. For certain identification, the specific degradation products for the respective polymer were selected first. Afterwards real environmental samples from the aquatic (three different rivers) and the terrestrial (bio gas plant) systems were screened for microplastics. Mainly polypropylene (PP), polyethylene (PE) and polystyrene (PS) were identified for the samples from the bio gas plant and PE and PS from the rivers. However, this was only the first step and quantification measurements will follow. © 2017 Elsevier Ltd.
  • Veröffentlichung
    Two birds with one stone - fast and simultaneous analysis of microplastics
    (2018) Eisentraut, Paul; Dümichen, Erik; Ruhl, Aki Sebastian
    Analysis of microplastic particles in environmental samples needs sophisticated techniques and is time intensive due to sample preparation and detection. Alternatives to the most common (micro-) spectroscopic techniques, Fourier transform infrared and Raman spectroscopy, are thermoanalytical methods, in which specific decomposition products can be analyzed as marker compounds for different kinds of plastic types and mass contents. Thermal extraction desorption gas chromatography-mass spectrometry allows the fast identification and quantification of MP in environmental samples without sample preparation. Whereas to date only the analysis of thermoplastic polymers has been realized, this is the first time that even the analysis of tire wear (TW) content in environmental samples has been possible. Various marker compounds for TW were identified. They include characteristic decomposition products of elastomers, antioxidants, and vulcanization agents. Advantages and drawbacks of these marker substances were evaluated. Environmental samples from street runoff were exemplarily investigated, and the results are presented. © 2018 American Chemical Society.
  • Veröffentlichung
    Decomposability versus detectability: First validation of TED-GC/MS for microplastic detection in different environmental matrices
    (2023) Kittner, Maria; Eisentraut, Paul; Braun, Ulrike
    A fast method for microplastic detection is thermal extraction desorption-gas chromatography/mass spectrometry (TED-GC/MS), which uses polymer-specific thermal decomposition products as marker compounds to determine polymer mass contents in environmental samples. So far, matrix impacts of different environmental matrices on TED-GC/MS performance had not yet been assessed systematically. Therefore, three solid freshwater matrices representing different aquatic bodies with varying organic matter contents were spiked with a total of eight polymers. Additionally, for the first time, the two biodegradable polymers polybutylene adipate terephthalate (PBAT) and polylactide (PLA) were analysed using TED-GC/MS. The methodological focus of this work was on detectability, quality of signal formation as well as realisation of quantification procedures and determination of the limit of detection (LOD) values. Overall, TED-GC/MS allowed the unambiguous detection of the environmentally most relevant polymers analysed, even at low mass contents: 0.02wt% for polystyrene (PS), 0.04wt% for the tyre component styrene butadiene rubber (SBR) and 0.2wt% for polypropylene (PP), polyethylene (PE) and PBAT. Further, all obtained LOD values were increased in all matrices compared to the neat polymer without matrix. The LOD of the standard polymers were increased similarly (PS: 0.21-0.34 (micro)g, SBR: 0.27-0.38 (micro)g, PP: 0.32-0.36 (micro)g, PMMA: 0.64-1.30 (micro)g, PET: 0.90-1.37 (micro)g, PE: 3.80-6.99 (micro)g) and their decompositions by radical scission processes were not significantly influenced by the matrices. In contrast, matrix-specific LOD increases of both biodegradable polymers PBAT (LOD: 1.41-7.18 (micro)g) and PLA (0.84-20.46 (micro)g) were observed, probably due to their hetero-functional character and interactions with the matrices. In conclusion, the TED-GC/MS performance is not solely determined by the type of the polymers but also by the composition of the matrix. © 2023 Wiley VCH GmbH