TY - JOUR A1 - Gottu Mukkula, A. R. A1 - Kern, Simon A1 - Salge, M. A1 - Holtkamp, M. A1 - Guhl, Svetlana A1 - Fleischer, C. A1 - Meyer, Klas A1 - Remelhe, M. A1 - Maiwald, Michael A1 - Engell, S. T1 - An Application of Modifier Adaptation with Quadratic Approximation on a Pilot Scale Plant in Industrial Environment N2 - The goal of this work is to identify the optimal operating input for a lithiation reaction that is performed in a highly innovative pilot scale continuous flow chemical plant in an industrial environment, taking into account the process and safety constraints. The main challenge is to identify the optimum operation in the absence of information about the reaction mechanism and the reaction kinetics. We employ an iterative real-time optimization scheme called modifier adaptation with quadratic approximation (MAWQA) to identify the plant optimum in the presence of plant-model mismatch and measurement noise. A novel NMR PAT-sensor is used to measure the concentration of the reactants and of the product at the reactor outlet. The experiment results demonstrate the capabilities of the iterative optimization using the MAWQA algorithm in driving a complex real plant to an economically optimal operating point in the presence of plant-model mismatch and of process and measurement uncertainties. KW - Process Analytical Technology KW - Online NMR Spectroscopy KW - Process Industry KW - Iterative real-time optimization KW - Modifier adaptation KW - Plant-model mismatch KW - Reactor control KW - CONSENS PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-524531 DO - https://doi.org/10.1016/j.ifacol.2020.12.685 SN - 1522-2640 VL - 53 IS - 2 SP - 11773 EP - 11779 PB - Elsevier CY - Amsterdam AN - OPUS4-52453 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Henning, L. M. A1 - Smales, Glen Jacob A1 - Colmenares, M. G. A1 - Bekheet, M. F. A1 - Simon, U. A1 - Gurlo, A. T1 - Synthesis and properties of COK-12 large-pore mesocellularsilica foam N2 - Large, ink-bottle-shaped pores in mesocellular foams (MCFs) are desired for various applications requiring enhanced mass transfer or the immobilization of larger compounds. Hence, the cylindrical pores of COK-12, an ordered mesoporous silica structurally comparable to SBA-15 but synthesized at room-temperature at quasi-neutral pH, are chemically swollen into ink-bottle pores. Therefore, p-xylene is used as a more sustainable swelling agent compared to popular alternatives. Its high boiling point allows for an additional thermal aging step to amplify the mesostructure enlargement without needing additional chemicals. For COK-12, the MCFs obtained at room temperature reach an unprecedented plateau for the modal mesopore cell and window diameter of 19.9 and 5.5 nm, respectively, with an underlying broad pore size distribution and distorted hexagonal lattice up to 14.5 nm, involving hexagonal and spherical structures. The combined chemical and thermal swelling resulted in the selective enlargement of the window diameter to more than 200% and a slightly increased cell diameter, pore size distribution, and hexagonal lattice distortion in comparison to the room temperature synthesis. Such materials are thought to be promising alternatives to SBA-15-based MCFs, often utilizing toxic catalysts during synthesis. The presented results pave the way for enhanced adsorptive, catalytic, and drug delivery performances for COK-12-based materials. KW - SAXS KW - MOUSE KW - Mesocellular foam KW - Mesoporous silica PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569590 DO - https://doi.org/10.1002/nano.202200223 SP - 1 EP - 11 AN - OPUS4-56959 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dietzmann, Simon A1 - Mehmood, Asad A1 - Guilherme Buzanich, Ana A1 - Emmerling, Franziska A1 - Fellinger, Tim-Patrick A1 - Thomas, A. T1 - Characterization of Solid-State Complexes by XAS N2 - Atomically dispersed metal-nitrogen doped carbons (M-N-C) are promising catalysts for the activation of small molecules such as O2 and CO2. These single atom catalysts (SAC) operate at the interface between homogenous and heterogenous catalysts. Currently, many examples of M-N-C are known with good oxygen reduction reaction activity but lacking a controlled synthesis of the specific active sites of the precatalyst. Recently, our group facilitated the synthesis of pure pyrrolic M-N4 sites using Zn ions as imprinters.[1] These amorphous materials obtained by active site imprinting method are characterized at the BAMline (Bessy II) by X-ray absorption spectroscopy (XAS). In-situ/operando measurements will be crucial in future work for a better understanding of the dynamic changes of the active site. T2 - InSynX Workshop 2023 CY - Sao Paulo, Brazil DA - 06.03.2023 KW - Solid-State Complexes PY - 2023 AN - OPUS4-58933 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Simon, Fabian A1 - Gehrenkemper, Lennart A1 - Becher, S. A1 - Dierckes, G. A1 - Langhammer, Nicole A1 - Cossmer, Antje A1 - von der Au, Marcus A1 - Göckener, B. A1 - Fliedner, A. A1 - Rüdel, H. A1 - Koschorreck, J. A1 - Meermann, Björn T1 - Quantification and characterization of PFASs in suspended particulate matter (SPM) of German rivers using EOF, dTOPA, (non-)target HRMS N2 - In this study, we compare analytical methods for PFAS determination–target analysis, non-target screening (NTS), direct total oxidizable precursor assay (dTOPA) and extractable organically bound fluorine (EOF). Therefore, suspended particulate matter (SPM) samples from German rivers at different locations in time series from2005 to 2020 were analyzed to investigate temporal and spatially resolved trends. In this study 3 PFAS mass balances approaches were utilized: (i) PFAA target vs. PFAS dTOPA, (ii) PFAS target vs. EOF and (iii) PFAS target vs. PFAS dTOPA vs. organofluorines NTS vs. EOF. Mass balance approach (i) revealed high proportions of precursor substances in SPM samples. For the time resolved analysis an increase from 94% (2005) to 97% in 2019 was observable. Also for the spatial resolved analysis precursor proportions were high with >84% at all sampling sites. Mass balance approach (ii) showed that the unidentified EOF (uEOF) fraction increased over time from82% (2005) to 99% (2019). Furthermore, along the river courses the uEOF increased. In the combined mass balance approach (iii) using 4 different analytical approaches EOF fractions were further unraveled. The EOF pattern was fully explainable at the sampling sites at Saar and Elbe rivers. For the time resolved analysis, an increased proportion of the EOF was now explainable. However, still 27% of the EOF for the time resolved analysis and 25% of the EOF for the spatial resolved analysis remained unknown. Therefore, in a complementary approach, both the EOF and dTOPA reveal unknown gaps in the PFAS mass balance and are valuable contributions to PFAS risk assessment. Further research is needed to identify organofluorines summarized in the EOF parameter. KW - PFAS KW - HR-CS-GFMAS KW - Fluorine KW - SPM KW - LC-MS/MS PY - 2023 DO - https://doi.org/10.1016/j.scitotenv.2023.163753 SN - 1879-1026 SN - 0048-9697 VL - 885 SP - 1 EP - 12 PB - Elsevier Science CY - Amsterdam AN - OPUS4-57429 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Herbig, B. A1 - Jörres, R. A. A1 - Schierl, R. A1 - Simon, M. A1 - Langner, Jeanette A1 - Seeger, Stefan A1 - Nowak, D. A1 - Karrasch, S. T1 - Psychological and cognitive effects of laser printer emissions: A controlled exposure study N2 - The possible impact of ultrafine particles from laser printers on human health is controversially discussed although there are persons reporting substantial symptoms in relation to these emissions. A randomized, single-blinded, cross-over experimental design with two exposure conditions (high-level and low-level exposure) was conducted with 23 healthy subjects, 14 subjects with mild asthma, and 15 persons reporting symptoms associated with laser printer emissions. To separate physiological and psychological effects, a secondary physiologically based categorization of susceptibility to particle effects was used. In line with results from physiological and biochemical assessments, we found no coherent, differential, or clinically relevant effects of different exposure conditions on subjective complaints and cognitive performance in terms of attention, short-term memory, and psychomotor performance. However, results regarding the psychological characteristics of participants and their situational perception confirm differences between the participants groups: Subjects reporting symptoms associated with laser printer emissions showed a higher psychological susceptibility for adverse reactions in line with previous results on persons with multiple chemical sensitivity or idiopathic environmental intolerance. In conclusion, acute psychological and cognitive effects of laser printer emissions were small and could be attributed only to different participant groups but not to differences in exposure conditions in terms of particle number concentrations. KW - Cognitive performance KW - Exposure KW - Idiopathic environmental intolerance KW - Laser printer emission KW - Multiple chemical sensitivity KW - Subjective complaints PY - 2018 DO - https://doi.org/10.1111/ina.12429 SN - 1600-0668 SN - 0905-6947 VL - 28 IS - 1 SP - 112 EP - 124 PB - John Wiley & Sons, Inc. CY - 111 RIVER ST, HOBOKEN 07030-5774, NJ USA AN - OPUS4-43945 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon A1 - Wander, Lukas A1 - Meyer, Klas A1 - Guhl, Svetlana A1 - Gottu Mukkula, A. R. A1 - Holtkamp, M. A1 - Salge, M. A1 - Fleischer, C. A1 - Weber, N. A1 - King, R. A1 - Engell, S. A1 - Paul, Andrea A1 - Pereira Remelhe, M. A1 - Maiwald, Michael T1 - Flexible Automation with compact NMR instruments N2 - Modular plants using intensified continuous processes represent an appealing concept to produce pharmaceuticals. It can improve quality, safety, sustainability, and profitability compared to batch processes, and it enables plug-and-produce reconfiguration for fast product changes. To facilitate this flexibility by real-time quality control, we developed a solution that can be adapted quickly to new processes and includes a compact Nuclear Magnetic Resonance (NMR) spectrometer for online quality monitoring as well as a new model-based control approach. The NMR sensor is a benchtop device enhanced to the requirements of automated chemical production including ro-bust evaluation of sensor data. Here, we present alternatives for the quantitative determination of the analytes using modular, physically motivated models. These models can be adapted to new substances solely by the use of their corresponding pure component spectra, which can either be derived from experimental spectra as well as from quantum mechanical models or NMR predictors. Modular means that spec-tral models can simply be exchanged together with alternate reagents and products. Beyond that, we comprehensively calibrated an NIR spectrometer based on online NMR process data for the first time within an industrial plant. The integrated solution was developed for a metal organic reac-tion running on a commercial-scale modular pilot plant and it was tested under industrial conditions. T2 - 7th Annual PANIC Conference CY - Hilton Head Island, South Carolina, USA DA - 03.03.2019 KW - Online NMR Spectroscopy PY - 2019 AN - OPUS4-47715 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gottu Mukkula, A. R. A1 - Engell, S. A1 - Kern, Simon A1 - Guhl, Svetlana A1 - Meyer, Klas A1 - Maiwald, Michael T1 - PAT-basierte iterative Optimierung der Fahrweise eines kontinuierlichen organischen Syntheseprozesses N2 - Im Zuge der Digitalisierung der Prozessindustrie werden zunehmend modellbasiere Echtzeitoptimierungsverfahren eingesetzt, sog. „Advanced Process Control“. Mithilfe der sogenannten Modifier-Adaptation ist eine iterative Betriebspunktoptimierung auch mit ungenauen Modellen möglich, sofern zuverlässige Prozessdaten zur Verfügung stehen. Am Beispiel eines smarten Online-NMR-Sensors, der in einem EU-Projekt von der BAM entwickelt wurde, konnte das Konzept in einer modularen Produktionsanlage zur Herstellung eines pharmazeutischen Wirkstoffs erfolgreich getestet werden. T2 - ProcessNet-Jahrestagung und 33. DECHEMA-Jahrestagung der Biotechnologen CY - Aachen, Germany DA - 10.09.2018 KW - Prozessanalytik KW - Echtzeitoptimierungsverfahren KW - Modifier-Adaptation KW - Prozess-Steuerung KW - Betriebspunktoptimierung KW - CONSENS PY - 2018 UR - https://onlinelibrary.wiley.com/doi/abs/10.1002/cite.201855233 DO - https://doi.org/10.1002/cite.201855233 SN - 0009-286X VL - 90 SP - 1237 EP - 1237 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-45902 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Kern, Simon A1 - Wander, Lukas A1 - Meyer, Klas A1 - Guhl, Svetlana A1 - Gottu Mukkula, A. R. A1 - Holtkamp, M. A1 - Salge, M. A1 - Fleischer, C. A1 - Weber, N. A1 - Engell, S. A1 - Paul, Andrea A1 - King, R. A1 - Maiwald, Michael T1 - Raw data of pilot plant runs for CONSENS project (Case study 1) N2 - In case study one of the CONSENS project, two aromatic substances were coupled by a lithiation reaction, which is a prominent example in pharmaceutical industry. The two aromatic reactants (Aniline and o-FNB) were mixed with Lithium-base (LiHMDS) in a continuous modular plant to produce the desired product (Li-NDPA) and a salt (LiF). The salt precipitates which leads to the formation of particles. The feed streams were subject to variation to drive the plant to its optimum. The uploaded data comprises the results from four days during continuous plant operation time. Each day is denoted from day 1-4 and represents the dates 2017-09-26, 2017-09-28, 2017-10-10, 2017-10-17. In the following the contents of the files are explained. KW - Process Analytical Technology KW - Multivariate Data Analysis KW - Nuclear Magnetic Resonance KW - Near Infrared Spectroscopy KW - Continuous Manufacturing KW - CONSENS PY - 2018 DO - https://doi.org/10.5281/zenodo.1438233 PB - Zenodo CY - Geneva AN - OPUS4-48063 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Berger, Wolfgang A1 - Simon, Franz-Georg A1 - Weimann, Karin A1 - Alsema, E. A. T1 - A novel approach for the recycling of thin film photovoltaic modules N2 - A sustainable recycling of photovoltaic (PV) thin film modules gains in importance due to the considerable growing of the PV market and the increasing scarcity of the resources for semiconductor materials. The paper presents the development of two strategies for thin film PV recycling based on (wet) mechanical processing for broken modules, and combined thermal and mechanical methods for end-of-life modules. The feasibility of the processing steps was demonstrated in laboratory scale as well as in semi-technical scale using the example of CdTe and CIS modules. Pre-concentrated valuables In and Te from wet mechanical processing can be purified to the appropriate grade for the production of new modules. An advantage of the wet mechanical processing in comparison to the conventional procedure might be the usage of no or a small amount of chemicals during the several steps. Some measures are necessary in order to increase the efficiency of the wet mechanical processing regarding the improvement of the valuable yield and the related enrichment of the semiconductor material. The investigation of the environmental impacts of both recycling strategies indicates that the strategy, which includes wet mechanical separation, has clear advantages in comparison to the thermal treatment or disposal on landfills. KW - Recycling KW - Photovoltaic KW - Thin film modules KW - CdTe KW - CIS KW - Mechanical processing KW - Life cycle analysis PY - 2010 DO - https://doi.org/10.1016/j.resconrec.2009.12.001 SN - 0921-3449 VL - 54 IS - 10 SP - 711 EP - 718 PB - Elsevier CY - Amsterdam [u.a.] AN - OPUS4-21439 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chubarenko, B. A1 - Kileso, A. A1 - Esiukova, E. A1 - Pinchuk, V. A1 - Simon, Franz-Georg T1 - Dataset on geosynthetic material debris contamination of the South-East Baltic shore N2 - The database gives information on the contamination of the shore of the South-Eastern Baltic with the debris of geosynthetic materials for the period 2018–2020. This new type of coastal pollution enters the natural environment due to the destruction of coastal protection structures and construction activities. The database contains sections: (1) a list of types of geosynthetic material residues, their photographic images and photographs illustrating examples of finds in natural conditions [1 List_geosynthetic_debris_SEB], (2) monitoring data on the contamination of the beach strip with the debris of geotextiles, braids from gabions, geocontainers (big bags), geocells and geogrids for the beaches of the South-Eastern Baltic for the period 2018–2020 [2 Monitoring_geosynthetic_debris_SEB]; (3) statistical distributions of the found geosynthetic debris by size [3 Scales_geosynthetic_debris_SEB] and (4) results of test surveys on the shores of Lithuania and Poland adjacent to Kaliningrad Oblast. All data refer to the beaches of the Kaliningrad Oblast (Russia), including the Russian parts of the Vistula and Curonian Spits, but also contains information on a one-time assessment of the pollution of the beaches of the adjacent territories: the Polish shore from the Poland-Russia border on the Vistula Spit to the mouth of the Vistula River, the Lithuanian shore from the border Lithuania-Russia on the Curonian Spit to the border of Latvia-Lithuania. Materials were collected during field surveys within the ERANET-RUS_Plus joint project EI-GEO, ID 212 (RFBR 18-55-76002 ERA_a, BMBF 01DJ18005). KW - Geosynthetics KW - Geotextiles KW - Contamination KW - Marine littering PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-541947 DO - https://doi.org/10.1016/j.dib.2021.107778 SN - 2352-3409 VL - 40 SP - 1 EP - 7 PB - Elsevier Inc. CY - Amsterdam AN - OPUS4-54194 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -