Analytische Chemie
Filtern
Dokumenttyp
- Vortrag (9)
- Zeitschriftenartikel (8)
- Posterpräsentation (3)
- Forschungsbericht (1)
- Forschungsdatensatz (1)
Schlagworte
- TED-GC/MS (22) (entfernen)
Organisationseinheit der BAM
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.
This is the repository of all experimental raw data used in the Scientific Reports publication "Specific adsorption sites and conditions derived by thermal decomposition of activated carbons and adsorbed carbamazepine" by Daniel Dittmann, Paul Eisentraut, Caroline Goedecke, Yosri Wiesner, Martin Jekel, Aki Sebastian Ruhl, and Ulrike Braun.
It includes
- overview_measurements.xlsx and overview_measurements.ods containing a list of all TGA experiments (TGA, TGA-FTIR, TED-GC-MS, and ramp-kinetics)
- TED-GC-MS.zip containing gas chromatography-mass spectrometry experimtent files for the Chemstation and OpenChrom
- TGA.zip containing thermogravimetric analyses raw data on evolved gas analyses experiments (TGA-FTIR and TED-GC-MS)
- TGA_kinetics.zip containing thermogravimetric analyses raw data on decomposition kinetic experiments (ramp-kinetics)
- TGA-FTIR.zip containing Fourier-transform infrared spectroscopy series files for OMNIC
- XRF.zip containing x-ray flourescence data on elemental composition
Microplastic particles are currently detected in almost all environmental compartments. The results of detection vary widely, as a multitude of very different methods are used with very different requirements for analytical validity.
In this work four thermoanalytical methods are compared and their advantages and limitations are discussed. One of them is thermal extraction-desorption gas chromatography mass spectrometry (TED-GC/MS), an analysis method for microplastic detection that has become established in recent years. In addition, thermogravimetric analysis coupled with Fourier-transform infrared spectroscopy (TGA-FTIR) and mass spectrometry (TGA-MS) were applied, two methods that are less common in this field but are still used in other research areas. Finally, microscale combustion calorimeter (MCC) was applied, a method not yet used for microplastic detection.
The presented results are taken from a recently published interlaboratory comparison test by Becker et al. (2020). Here a reference material consisting of suspended matter and specified added polymer masses was examined, and only the results of the recoveries were presented. In the present paper, however, the results for the individual polymers are discussed in detail and individual perspectives for all instruments are shown.
It was found that TED-GC/MS is the most suitable method for samples with unknown matrix and unknown, variable kinds and contents of microplastic. TGA-FTIR is a robust method for samples with known matrix and with defined kinds of microplastic. TGA-MS may offer a solution for the detection of PVC particles in the future. MCC can be used as a very fast and simple screening method for the identification of a potential microplastic load of standard polymers in unknown samples.
Deuterated polystyrene (D-PS) improves microplastic detection with TED-GC / MS, among other things through higher reproducibility. It is inexpensive (0.1 ct / analysis) and can be dosed quickly and reproducibly thanks to its good solubility (e.g. in toluene). However, certain matrices lead to an exchange of the deuterium with hydrogen. The poster shows the measuring principle, in which matrices H/D-exchange takes place, the results of kinetic studies and ways of preventing or circumventing the H/D-exchange.
The scientific and practical challenge of detecting microplastics (MPs) in the environment in a targeted and rapid manner is solved by innovative coupling of thermogravimetric analysis with mass spectrometric methods.
Fast identification and quantitative determination of most thermoplastic polymers and elastomers is possible by using thermal extraction Desorption gas chromatography–mass spectrometry (TED-GC–MS).
The occurrence of microplastic (MP) in food products, such as beverages in plastic bottles, is of high public concern. Existing analytical methods focus on the determination of particle numbers, requiring elaborate sampling tools, laboratory infrastructure and generally time-consuming imaging detection methods. A comprehensive routine analysis of MP in food products is still not possible. In the present work, we present the development of a smart filter crucible as sampling and detection tool. After filtration and drying of the filtered-off solids, a direct determination of the MP mass content from the crucible sample can be done by thermal extraction desorption gas chromatography mass spectroscopy (TED-GC/MS). The new filter crucible allows a filtration of MP down to particle sizes of 5 µm. We determined MP contents below 0.01 µg/L up to 2 µg/L, depending on beverages bottle type. This may be directly related to the bottle type, especially the quality of the plastic material of the screw cap. Dependent on the plastic material, particle formation increases due to opening and closing operations during the use phase. However, we have also found that some individual determinations of samples were subjected to high errors due to random events. A conclusive quantitative evaluation of the products is therefore not possible at present.
Der Vortrag wurde im Rahmen der Abschlusskonferenz des Forschungsschwerpunktes "Plastik in der Umwelt" des BMBF gehalten. Er fasst die Ergebnisse des Verbundprojektes RUSEKU zusammen. Es wurde die Herstellung verschiedener Testmaterialien für die Mikroplastik (MP) Analytik beschrieben. Im weiteren geht es um verschiedene Ansätze MP kostengünstig und schnell zu detektieren, z.B. mit Nahinfrarotspektroskopie. Nanoplastik konnte mit der Transmissionselektronenmikroskopie sichtbar gemacht werden. Für die praxisnahe Beprobung von Gewässern wurde die Fraktionierte Filtration entwickelt. Integrale Beprobungen können mit dem Sedimentationskasten erfolgen. Als Beispiele für die Beprobung realer Gewässer wurde das urbane Abwassersystem Kaiserslautern, Getränkewasser und Waschmaschinenwasser gezeigt.
Monitoring von Mikroplastik
(2021)
Die große Herausforderung in der Detektion von Mikroplastik (MP)‑Partikeln (1-1000 µm) besteht darin, sie neben Millionen von natürlichen Partikeln in Umweltproben nachzuweisen. Zum Aufspüren von Senken, Eintragspfaden und für Monitoring-Kampagnen ist ein schnelles, automatisiertes Verfahren unerlässlich. Ein solches Verfahren wurde an der Bundesanstalt für Materialforschung und -prüfung (BAM) mit der ThermoExtraktion/Desorption-Gaschromatographie-Massenspektrometrie (TED-GC/MS) in den letzten Jahren entwickelt.