TY - CONF A1 - Leng, Jing T1 - Structure-Property relationships of Nanocomposites based on Epoxy and layered double hydroxides T2 - 79. Jahrestagung der DPG und DPG-Frühjahrstagung CY - Berlin, Germany DA - 2015-03-15 PY - 2015 AN - OPUS4-32889 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schulz, K. T1 - Impact of thermal and hydrothermal treatment on the crystallinity of mesoporous hematite films T2 - 27. Deutsche Zeolith-Tagung CY - Oldenburg, Germany DA - 2015-02-25 PY - 2015 AN - OPUS4-32931 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Batzdorf, Lisa T1 - Synthesis and Structural Characterization of Cocrystals T2 - International School of Crystallography, 46th Course: The Future of Dynamic Structural Science CY - Erice, Sicily, Italy DA - 2013-05-31 PY - 2013 AN - OPUS4-32502 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fischer, Franziska T1 - In situ Untersuchungen mechanochemischer Reaktionen mittels Pulverdiffraktometrie T2 - ANAKON 2015 CY - Graz, Österreich DA - 2015-03-23 PY - 2015 AN - OPUS4-32938 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Leiterer, Jork T1 - Characterisation of levitated samples for modelling of condensed matter N2 - Many of today’s analytical problems are characterized by small sample volumes and can only be solved through a corresponding miniaturisation of the analytical instrumentation. Handling of small-sample volumes is inherently difficult due to contamination and sorption processes on the walls of containers. Acoustic levitation is a powerful tool for contact-free sample handling of solid, liquid, and selected gaseous samples. In addition, levitation permits a chemical pre-treatment such as enrichment, extraction, and derivatisation as well as combination with other analytical techniques such as optical spectroscopy. Acoustically levitated liquid and solid samples are typically in a range between 0.005-5 µl (diameter 0.2-2 mm respectively) and are suspended in a gaseous environment by a stationary ultrasonic field. Acoustic levitation avoids sample contamination and sorption processes by container walls, but suffers from evaporation and loss of solvents. Nonetheless, it is of great impact for the characterization of small samples. Exact determination of volume is inherently important to find out the resultant concentration in evaporating droplets. Levitation is a possibility to characterise the starting conditions of crystallisation and polymerisation. Even for spectroscopic methods the correct information on shape, size and concentration of samples are indispensable. To determine the size and volume of levitated samples, different methods of contactless droplet size monitoring were developed and compared in detail. They give the initial values for modelling of evaporation effects. In addition, for balancing evaporation and condensation on levitated drops during the experiments, non-contact techniques of solvent and reagent supply have been tested. Here, the advantages of acoustic levitation are demonstrated for on line analysis of crystallisation in a levitated droplet. The evaporation and formation of crystals is observed via time-resolved X-ray diffraction using synchrotron radiation at BESSY. Wall-free crystallisation in an acoustic levitator gives a tool to prove existing models concerning crystallisation processes. Furthermore the occurrence of polymorphic modifications depending on different conditions can be detected in situ under different and adjustable conditions. T2 - 13. Vortragstagung "Modellierung in der Festkörper- und Materialchemie" der GDCh-Fachgruppe Analytische Chemie, Rheinisch-Westfälische Technische Hochschule Aachen CY - Aachen, Germany DA - 2006-09-20 PY - 2006 AN - OPUS4-13805 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - Kristallstruktur von Tris(oxamiddioxim-k2N,N')nickel(II) L(+)-Tartrat, [Ni(H2oxado)3][L(+)-(C4H406)] T2 - DGK- Jahrestagung in Bremen 2007 CY - Bremen, Germany DA - 2007-03-05 PY - 2007 AN - OPUS4-14280 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Juran, S. T1 - Bispidines as a new class of chelating agents for copper radionuclides T2 - 17. Internationale Symposium on Radiopharmaceutical Scienses CY - Aachen, Germany DA - 2007-04-30 PY - 2007 AN - OPUS4-14069 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kraus, Werner T1 - Supramolekulare Netzwerke auf der Basis von Kupfer(II)-Bispidinkomplexen T2 - DGK-Jahrestagung 2007 CY - Bremen, Germany DA - 2007-03-05 PY - 2007 AN - OPUS4-14070 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - Alkalimetalloxoferrate AFeO2 Strukturchemie und Mößbauerspektroskopie T2 - DGK Jahrestagung CY - Berlin, Germany DA - 2007-03-05 PY - 2007 AN - OPUS4-14656 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wenzel, Klaus-Jürgen T1 - Tricalciumphosphat aus Sicht der Röntgendiffraktometrie T2 - 6. Sitzung des AK Biokeramik, BAM CY - Berlin, Germany DA - 2007-04-26 PY - 2007 AN - OPUS4-14706 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Goedecke, Caroline T1 - Detection of microplastic and tire wear particles in road run-off samples using TED-GC-MS N2 - Plastics and rubber are used in many applications, such as packaging, building, construction and mobility. Due to their favourable properties like light weight, flexible processing and low costs their production and consequently their input into the environment has increased significantly over the last decades. In the environment, oxidation processes and mechanical abrasion lead to the decomposition of these plastics into small fragments, called microplastic (< 5 mm). By definition, microplastics only involve thermoplastics and duroplastics but elastomers made out of synthetic polymers (e. g. styrene butadiene rubber), modified natural polymers (e. g. natural rubber) and products of synthetic polymers (e. g. tires) are also part of the current microplastic discussion. The main entry pathway of rubber into the environment is the wear of used tire treads in road traffic. Lassen et al. showed that 60 % of the microplastic emissions in Denmark into the environment come from secondary microplastics generated by tires. Rain events can cause microplastic and rubber to get from the street into the street inlets. Depending on the sewage system, these waters are sometimes not cleaned in the sewage treatment plants and reach the surface waters untreated. To analyse microplastic particles in samples, mainly FTIR or Raman spectroscopic methods are applied at present. Rubber or tire particles in environmental samples cannot be analysed by these methods, because the added carbon black leads to annoying absorption and fluorescent effects. We developed a thermoanalytical method, the so-called TED-GC-MS (thermal extraction desorption gas chromatography mass spectrometry), which allows the simultaneous detection of microplastic and tire wear with almost no sample preparation in about 2.5 h. The TED-GC-MS is a two-step analytical method which consists of a thermobalance and a GC-MS system. Up to 50 mg of an environmental sample is heated up to 600 °C in a nitrogen atmosphere. During pyrolysis, between 300 and 600 °C polymer-specific decomposition products are produced and collected on a solid phase. Afterwards the substances are desorbed, separated and analysed using the GC-MS. The aim of the present work is to present the TED-GC-MS as a time efficient screening method to quantify the industrial most relevant polymers in street run-off samples. Analytical challenges in the determination of polyethylene (PE), polypropylene (PP), polystyrene (PS), polyethylene terephthalate (PET) and polyamide (PA), polymethyl methacrylate (PMMA) and styrene-butadiene-rubber (SBR) as a component of tire wear are honestly discussed. The study area is a 200 m long section of the Clayallee in Berlin, a representative typical urban catchment area. The road run-off in this section flows through the gullies directly into a sample chamber, which directs the runoff in an open channel to the rainwater sewer of this area. The sample chamber allows a sample to be taken directly from the road run-off without mixing with the run-off from other areas. The sample chamber is equipped with an automatic sampler. The automatic sampler is controlled by a conductivity sensor to detect the storm event at an early stage. The sensor gives the sampler a signal to start the sampling program when it gets in contact with water and reaches a certain conductivity threshold. The capacity of the sample container is 100 l and the maximum delivery of the automatic sampler is 2.8 l/min. Afterwards, the water was pumped through various stainless-steel sieves with a diameter of approximately 20 cm and mesh widths of 500, 100, 50 μm. The obtained solids were steam sterilized, freeze-dried and measured with the TED-GC-MS. The results of the TED-GC-MS-measurements are summarized in Figure 1. It shows the polymers which were detected in 1 mg of the dry masses of various street run off samples obtained during a period of 1.5 years. We detected PMMA, PS, PP, PE and SBR, as a component of tire wear in the samples. The quantification of the polymers leads to amounts of PS, PP, PE and SBR between 0 µg and 10 µg. PMMA was only detected in traces. T2 - ICCE 2019 CY - Thessaloniki, Greece DA - 16.06.2019 KW - Microplastics KW - TED-GC-MS KW - Road run-off KW - Chromatography PY - 2019 AN - OPUS4-48301 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weber, Simone T1 - Influence of the pH Value to the Degradation of Ester-Based Thermoplastic Polyurethanes N2 - Microplastics are solid polymeric particles with a size of 1-1000 μm (ISO/TR21960:2020), which can be emitted from mismanaged waste into the environment, where microplastic is now ubiquitous. What happens to the microplastics after ending up in the environment, which risks entail and what effects it has are not sufficiently clarified up to now. The most certain issue is that the plastic particles in the environment are exposed to natural ageing, are fragmenting and degrading, such that the potential risk to ecosystems and humans is increasing due to the formation of smaller and smaller particles, potentially even including nanoplastics, if these are ingested before their further degradation. Therefore, and in view of a possible registration of polymers under REACH in the future, it is necessary to investigate the degradation of thermoplastic polyurethanes (TPU) regarding hydrolysis stability to evaluate possible risks and effects to the environment. In the present studies, one thermoplastic polyurethane – with and without hydrolysis stabilizer – is exposed to different pH buffers at 50°C for 14 days to investigate hydrolysis depending to different pH values (acid, alkali and neutral) based on OECD guideline TG111. The hydrolysis behavior of the TPUs is characterized by surface sensitive techniques and on bulk properties. First degradation effects can be detected by SEC. Hydrolysis, especially under acidic and basic conditions, leads to chain scissions to lower molecular masses. Furthermore, the degradation products which indicate the structure of the bulk material were detected by thermo-analytical methods like TGA-FTIR for the small degradation products and the thermo extraction/desorption-gaschromatography/mass spectrometry (TED-GC/MS) for bigger degradation products. Acidic and basic hydrolysis shows the same degradation behavior which is caused by a preferred scission of the ester and urethane functionalities. Surface-sensitive techniques such as XPS demonstrate less carboxylic acid formation at acidic than at alkaline pH value in the TPU without stabilator, where as the TPU with stabilator ages to the same extent in both pH ranges. Altogether, the hydrolysis of TPUs – independently of added stabilizer or not – in acid and alkali environment is accelerated compared to the neutral hydrolysis. T2 - SETAC CY - Dubin, Ireland DA - 30.04.2023 KW - Degradation KW - Thermoplastic Polyurethane KW - Microplastic KW - Polymer Hydrolysis KW - Polymer 3R KW - REACH PY - 2023 AN - OPUS4-58906 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wiesner, Yosri T1 - Erfassung von Degradationsprodukten und Additiven sowie temperaturspezifische Pyrolyseprodukte mittels TED-GC/MS N2 - Im der Präsentation werden, neben der Möglichkeit der Mikroplastikquantifizierung, auf weitere Anwendungsfelder der Methode TED-GC/MS eigegangen. Dies beinhaltet die Erfassung von Degradationsprodukten UV/O2 geschädigter Polymere und die Detektion von Additiven. Die Optimierung der Methode betreffend Messzeit und materialspezifischer Messanforderung sind ebenfalls Gegenstand. T2 - Kolloquium Massenspektrometrie von Polymeren CY - Berlin, Germany DA - 09.05.2023 KW - TED-GC/MS KW - Polymere KW - Degradation KW - Additive PY - 2023 AN - OPUS4-57480 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -