TY - CONF A1 - Kern, Simon A1 - Guhl, Svetlana A1 - Meyer, Klas A1 - Wander, Lukas A1 - Paul, Andrea A1 - Bremser, Wolfram A1 - Maiwald, Michael T1 - Mathematical and statistical tools for online NMR spectroscopy in chemical processes N2 - Monitoring chemical reactions is the key to chemical process control. Today, mainly optical online methods are applied, which require excessive calibration effort. NMR spectroscopy has a high potential for direct loop process control while exhibiting short set-up times. Compact NMR instruments make NMR spectroscopy accessible in industrial and harsh environ¬ments for advanced process monitoring and control, as demonstrated within the European Union’s Horizon 2020 project CONSENS. We present a range of approaches for the automated spectra analysis moving from conventional multivariate statistical approach, (i.e., Partial Least Squares Regression) to physically motivated spectral models (i.e., Indirect Hard Modelling and Quantum Mechanical calculations). By using the benefits of traditional qNMR experiments data analysis models can meet the demands of the PAT community (Process Analytical Technology) regarding low calibration effort/calibration free methods, fast adaptions for new reactants or derivatives and robust automation schemes. T2 - Advanced Mathematical and Computational Tools in Metrology and Testing conference CY - Glasgow, United Kingdom DA - 29.08.2017 KW - Online NMR Spectroscopy KW - Process Control KW - Partial Least Squares Regression KW - Indirect Hard Modelling KW - Quantum Mechanics KW - First Principles PY - 2018 SN - 978-9-813-27429-7 VL - 89 SP - 229 EP - 234 PB - World Scientific CY - New Jersey AN - OPUS4-51391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - Online Raman spectroscopy for the quantitative evaluation of a Ralstonia cultivation N2 - Spectroscopic methods possess important advantages for the observation of bioprocesses: they are robust, gain many data within a short time scale, and allow for the measurement of multiple relevant information at the same time. Next to Near-infrared spectroscopy, Raman spectroscopy is increasingly applied as a powerful online tool to monitor bioprocesses. However, Raman spectra may be obscured by straylight, cosmic rays and fluorescence. To achieve the best performance, optimal conditions for spectral quality and stability should be pursued. This comprises not only the choice of highly-sensitive equipment, but also the way of implementation into the process. Here we compared the potential of introducing a sterilized fiber optical Raman probe, and a flow-through cell into the bypass of a stirred tank reactor to monitor an autotrophic cultivation of Ralstonia eutropha where gasses are the energy and carbon sources. Raman spectra were continuously recorded over seven days and 22 samples were taken for the reference analytics of biomass, optical density, and protein. In addition, data for of phosphate and ammonium were available. The quantitative Evaluation of Raman spectra by Partial Least Squares Regression (PLSR) yielded comparable results for both approaches, however, there was a general trend of lower prediction errors with the immersion probe. The better performance of the non-contact optic may be either related to a more representative interaction of the measurement optics with the probe or simply to the absence of probe-fouling, which was observed with the immersion optic in the interstice between window and metal frame. T2 - 5th BioProScale Symposium CY - Berlin, Germany DA - 20.03.2018 KW - Raman spectroscopy KW - Bioprocess KW - Chemometrics PY - 2018 UR - www.bioproscale-conference.org AN - OPUS4-44580 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - Bestimmung des Ligningehalts mittels NIR Spektroskopie N2 - Im DFG-Schwerpunktprogramm 1374, Teilprojekt FunWood IV, erfolgt in Kooperation mit dem Institut für Bioanalytik an Hochschule für angewandte Wissenschaften, Coburg und dem Helmholtz-Zentrum für Umweltforschung (UFZ), Leipzig die Untersuchung des Ligningehalts von natürlich gealterten Hölzern. Zu diesem Zweck soll an der BAM eine NIR spektroskopische Methode entwickelt werden, die auch zur Untersuchung großer Stückzahlen geeignet ist. Insgesamt liegen exponierte Proben von 13 verschiedenen Hölzern vor, die sukzessive durch die Kooperationspartner kryovermahlen und getrocknet werden. Für jede der 13 Arten wurden jeweils 300 Holzstücken ausgebracht, exponiert und im Sommer 2018 wieder eingesammelt. Die Ergebnisse sollen als Grundlage für die Bewertung eines Langzeitversuchs zum Einfluss von Waldbewirtschaftungsintensität und Baumartenidentität über mehrere geographische Dimensionen dienen. T2 - Projekttreffen DFG-Schwerpunktprogramm 1374, Teilprojekt FunWood IV CY - Institut für Bioanalytik, Hochschule für angewandte Wissenschaften, Coburg, Germany DA - 15.11.2018 KW - Lignin KW - NIR Spektroskopie KW - Chemometrie PY - 2018 AN - OPUS4-46981 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - NIR-Ringversuch II: Jetzt geht es los ! N2 - Ziele und Durchführung eines geplanten Ringversuchs zur Untersuchung eines Dreikomponentensystems mittels NIR werden vorgestellt. Der Vortrag enthält einen kurzen Rückblick auf einen 2014 durchgeführten Ringversuch, wobei ein flüssiges Zweikomponentensystem untersucht wurde. Im Anschluss erfolgt die Erläuterung der verwendeten Komponenten, es werden Teilnahmebedingungen und mögliche Zeiträume bekannt gegeben. T2 - 14. PAT ERFA CY - Leverkusen, Germany DA - 18.09.2018 KW - NIR KW - Chemometrie KW - Ringversuch PY - 2018 AN - OPUS4-46008 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kern, Simon A1 - Meyer, Klas A1 - Guhl, Svetlana A1 - Gräßer, Patrick A1 - Paul, Andrea A1 - King, R. A1 - Maiwald, Michael T1 - Online low-field NMR spectroscopy for process control of an industrial lithiation reaction—automated data analysis N2 - Monitoring specific chemical properties is the key to chemical process control. Today, mainly optical online methods are applied, which require time- and cost-intensive calibration effort. NMR spectroscopy, with its advantage being a direct comparison method without need for calibration, has a high potential for closed-loop process control while exhibiting short set-up times. Compact NMR instruments make NMR spectroscopy accessible in industrial and rough environments for process monitoring and advanced process control strategies. We present a fully automated data analysis approach which is completely based on physically motivated spectral models as first principles information (Indirect Hard Modelling – IHM) and applied it to a given pharmaceutical lithiation reaction in the framework of the European Union’s Horizon 2020 project CONSENS. Online low-field NMR (LF NMR) data was analysed by IHM with low calibration effort, compared to a multivariate PLS-R (Partial Least Squares Regression) approach, and both validated using online high-field NMR (HF NMR) spectroscopy. KW - Online NMR spectroscopy KW - Process analytical technology KW - Partial Least Squares Regression KW - Indirect Hard Modeling KW - Benchtop NMR Spectroscopy KW - Smart Sensors KW - CONSENS PY - 2018 UR - https://link.springer.com/article/10.1007/s00216-018-1020-z DO - https://doi.org/10.1007/s00216-018-1020-z SN - 1618-2642 SN - 1618-2650 VL - 410 IS - 14 SP - 3349 EP - 3360 PB - Springer CY - Berlin, Heidelberg AN - OPUS4-44847 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Paul, Andrea A1 - Wander, Lukas A1 - Becker, Roland A1 - Goedecke, Caroline A1 - Braun, Ulrike T1 - High-throughput NIR spectroscopic (NIRS) detection of microplastics in soil N2 - The increasing pollution of terrestrial and aquatic ecosystems with plastic debris leads to the accumulation of microscopic plastic particles of still unknown amount. To monitor the degree of contamination analytical methods are urgently needed, which help to quantify microplastics (MP). Currently, time-costly purified materials enriched on filters are investigated both by micro-infrared spectroscopy and/or micro-Raman. Although yielding precise results, these techniques are time consuming, and are restricted to the analysis of a small part of the sample in the order of few micrograms. To overcome these problems, here we tested a macroscopic dimensioned NIR process-spectroscopic method in combination with chemometrics. For calibration, artificial MP/soil mixtures containing defined ratios of polyethylene, polyethylene terephthalate, polypropylene, and polystyrene with diameters < 125 µm were prepared and measured by a process FT-NIR spectrometer equipped with a fiber optic reflection probe. The resulting spectra were processed by chemometric models including support vector machine regression (SVR), and partial least squares discriminant analysis (PLS-DA). Validation of models by MP mixtures, MP-free soils and real-world samples, e.g. and fermenter residue, suggest a reliable detection and a possible classification of MP at levels above 0.5 to 1.0 mass% depending on the polymer. The benefit of the combined NIRS chemometric approach lies in the rapid assessment whether soil contains MP, without any chemical pre-treatment. The method can be used with larger sample volumes and even allows for an online prediction and thus meets the demand of a high-throughput method. KW - Microplastics KW - Soil KW - Chemometrics KW - PLS-DA KW - Support vector machines KW - Near Infrared Spectroscopy PY - 2018 DO - https://doi.org/10.1007/s11356-018-2180-2 SN - 1614-7499 SN - 0944-1344 VL - 26 IS - 8 SP - 7364 EP - 7374 PB - Springer AN - OPUS4-45405 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - A process spectroscopic approach for the monitoring of microplastics  in environmental samples N2 - The potential of Raman and NIR process-spectroscopic as a rapid approach for the estimation of microplastics (MP) in soil matrix were tested. For this purpose, artificial MP/soil mixture samples consisting of standard soils or sand with defined ratios of MP (0,5 – 10 mass% polymer) from polyethylene (PE), polypropylene (PP), polystyrene (PS) and polyethylene terephthalate (PET) were prepared. MP particles with diameters < 2 mm and < 125 µm were obtained from industrial polymer pellets after cryo-milling. Spectra of these mixtures were collected by (i) a process FT-NIR spectrometer equipped with a reflection probe, (ii) by a cw-process Raman spectrometer and (iii) by a time-gated Raman spectrometer using fiber-optic probes. The evaluation of process-spectra was performed by chemometric methods. Whereas MP could be detected by Raman spectroscopy in coastal sand at 0.5 mass%, in standard soil detection of MP was limited to 10 – 5 mass% with the large fraction, but samples containing particles of the 125µm mass-fraction yielded no positive result at all. One reason for the lacking sensitivity could be fluorescence by soil organic matter and thus, in a next test time-gated Raman spectroscopy was applied. However, although being indeed more sensitive to the small particles this method failed at MP < 5 mass% indicating that fluorescence was not the major problem. Finally, FT-NIR was tested. Depending on the polymer, MP contents of 0,5 or 1 mass%, respectively, could be detected in standard soils and polymers identified. Furthermore, this approach could be used for the investigation of mixtures of up to four polymers and in real-world samples from bio-waste fermenter residues. T2 - Einladung zu einem Beratungsgespräch zum Thema Mikroplastik durch die Firma Endress+Hauser Conducta GmbH+Co.KG CY - Gerlingen, Germany DA - 11.06.2018 KW - Chemometrics KW - Microplastics KW - Raman KW - Process-spectroscopy KW - NIR PY - 2018 AN - OPUS4-45406 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koegler, M. A1 - Paul, Andrea A1 - Anane, E. A1 - Birkholz, M. A1 - Bunker, A. A1 - Viitala, T. A1 - Maiwald, Michael A1 - Junne, S. A1 - Neubauer, P. T1 - Comparison of time-gated surface-enhanced Raman spectroscopy (TG-SERS) and classical SERS based monitoring of Escherichia coli cultivation samples N2 - The application of Raman spectroscopy as a monitoring technique for bioprocesses is severely limited by a large background signal originating from fluorescing compounds in the culture media. Here, we compare time-gated Raman (TG-Raman)-, continuous wave NIRprocess Raman (NIR-Raman), and continuous wave micro-Raman (micro-Raman) approaches in combination with surface enhanced Raman spectroscopy (SERS) for their potential to overcome this limit. For that purpose, we monitored metabolite concentrations of Escherichia coli bioreactor cultivations in cell-free supernatant samples. We investigated concentration transients of glucose, acetate, AMP, and cAMP at alternating substrate availability, from deficiency to excess. Raman and SERS signals were compared to off-line metabolite analysis of carbohydrates, carboxylic acids, and nucleotides. Results demonstrate that SERS, in almost all cases, led to a higher number of identifiable signals and better resolved spectra. Spectra derived from the TG-Raman were comparable to those of micro-Raman resulting in well-discernable Raman peaks, which allowed for the identification of a higher number of compounds. In contrast, NIR-Raman provided a superior performance for the quantitative evaluation of analytes, both with and without SERS nanoparticles when using multivariate data analysis. KW - Time-gated Raman (TG-Raman) KW - Surface-enhanced Raman spectroscopy (SERS) KW - Multivariate data analysis KW - Metabolite quantification KW - Escherichia coli PY - 2018 DO - https://doi.org/10.1002/btpr.2665 SN - 1520-6033 SN - 8756-7938 VL - 34 IS - 6 SP - 1533 EP - 1542 PB - Wiley AN - OPUS4-45831 LA - eng 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 - CONF A1 - Maierhofer, Christiane A1 - Thiel, Erik A1 - Altenburg, Simon A1 - Mohr, Gunther A1 - Thiede, Tobias A1 - Mishurova, Tatiana A1 - Paul, Andrea A1 - Kranzmann, Axel A1 - Hilgenberg, Kai A1 - Pittner, Andreas A1 - Bruno, Giovanni A1 - Sommer, Konstantin A1 - Gumenyuk, Andrey T1 - Quality control in additive manufacturing via in-situ monitoring and non-destructive testing N2 - More than 80 representatives of SMEs, industrial companies and research institutes met on September 12 at the workshop "Challenges in Additive Manufacturing: Innovative Materials and Quality Control" at BAM in Adlershof to discuss the latest developments in materials and quality control in additive manufacturing. In special lectures, researchers, users and equipment manufacturers reported on the latest and future developments in additive manufacturing. Furthermore, funding opportunities for projects between SMEs and research institutions on a national and European level were presented. T2 - Challenges in Additive Manufacturing: Innovative Materials and Quality Control CY - Berlin, Germany DA - 12.09.2018 KW - Additive manufacturing KW - Quality control KW - Non-destructive testing KW - In-situ monitoring PY - 2018 AN - OPUS4-46072 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -