TY - CONF A1 - Paul, Andrea T1 - Multivariate approaches in the evaluation of (hyper)spectral data for microplastics analysis - options and limitations N2 - Die zunehmende Anreicherung von Gewässern und Böden mit Plastikmüll führt zur Anhäufung von mikroskopisch kleinen Plastikpartikeln, sogenannter Mikroplastik (MP). Es werden dringend analytische Methoden benötigt, die helfen MP zu identifizieren und zu quantifizieren. Gegenwärtig kommen dafür hauptsächlich thermoanalytische und mikro¬skopische Verfahren, wie Mikro-Infrarotspektroskopie oder Mikro-Raman zum Einsatz. Letztere sind in der Regel an zeitaufwendige Probenanreicherungen und -aufbereitungen gebunden, es können nur kleine Probenmengen (Mikrogramm) untersucht werden und die Auswertung der erzielten Spektren kann anspruchsvoll sein. Im Rahmen dieser Präsentation werden zwei Ansätze vorgestellt, die über die multi-variate Analyse spektroskopischer Daten i) einen neuen methodischen Ansatz zum Screening von MP in belasteten Böden sowie ii) eine alternative Auswertung großer (Mikro)-spektroskopischer Datensätze ermöglichen. Zunächst wird ein NIR-spektroskopisches Verfahrens vorgestellt, das es gestattet MP bestehend aus Polyethylen, Polyethylenterephthalat, Polypropylen und Polystyrol im Bereich bis zu 0,5 Massenprozent zu detektieren. Aufgrund kurzer Messzeiten und robuster Technik besitzt dieser Ansatz das Potenzial, im Gegensatz zu den thermoanalytischen und mikrospektroskopischen Methoden, größere Probenmengen mit minimaler Vor¬behandlung zu untersuchen. Der zweite Ansatz befasst sich mit der Auswertung großen Datensätze, wie sie typischerweise als Resultat der Mikro-FTIR unter Nutzung moderner FPA-Detektoren erhalten werden. Die Mikro-FTIR-Technik beruht auf der spektralen Aufnahme, Abbildung und an¬schließenden Identifizierung von Schwingungsbanden, die für synthetische Polymere typisch sind. Die Bilddatensätze sind groß und enthalten Spektren von unzähligen Partikeln natürlichen und synthetischen Ursprungs. Zur Ergänzung bestehender Ansätze, die z.B. auf Recherchen von Spektren¬bibliotheken basieren, wurde die explorative multivariate Datenanalyse getestet. Als Kernkonzept wurde hierbei die Dimensionalitäts¬reduktion verwendet. Die Ergebnisse stellen nicht nur eine orthogonale Methode zur Kontrolle der Ergebnisse dar, die auf Grundlage einer automatisierten Bibliothekssuche erzielt wurden, sondern ergaben darüber hinaus eine Gruppe von Spektren, die nicht in den vorhandenen Spektrenbibliotheken erfasst wurden. N2 - The increasing enrichment of water bodies and soils with plastic waste leads to the accumulation of microscopic plastic particles, so-called microplastics (MP). There is an urgent need for analytical methods that help to identify and quantify MP. At present, mainly thermo-analytical and microscopic methods such as micro-infrared spectroscopy or micro-Raman are used for this purpose. The latter are usually tied to time-consuming sample enrichment and preparation, only small sample quantities (micrograms) can be examined and the evaluation of the obtained spectra can be demanding. In the context of this presentation, two approaches are presented which, via the multi-variate analysis of spectroscopic data, allow i) a new methodological approach to screening MP in contaminated soils and ii) an alternative evaluation of large (micro)-spectroscopic data sets. First, a NIR spectroscopic method is presented which allows MP consisting of polyethylene, polyethylene terephthalate, polypropylene and polystyrene to be detected in the range of up to 0.5 mass percent. Due to short measurement times and robust technology, this approach has the potential, in contrast to thermo-analytical and micro-spectroscopic methods, to examine larger sample quantities with minimal pre-treatment. The second approach deals with the evaluation of large data sets, as typically obtained as a result of micro-FTIR using modern FPA detectors. The micro-FTIR technique is based on the spectral recording, imaging and subsequent identification of vibration bands typical of synthetic polymers. The image data sets are large and contain spectra of numerous particles of natural and synthetic origin. Exploratory multivariate data analysis has been tested to complement existing approaches based on e.g. spectrum library searches. The core concept used was dimensionality reduction. The results not only represent an orthogonal method for checking the results obtained by an automated library search, but also revealed a group of spectra that were not recorded in the existing spectrum libraries. T2 - analytica conference 2020 CY - Online meeting DA - 19.10.2020 KW - Microplastics KW - Multivariate Datenanalyse KW - NIR KW - Hyperspectral data PY - 2020 AN - OPUS4-51516 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Paul, Andrea A1 - Broszies, T. A1 - Ostermann, Markus A1 - Vogdt, F.U. A1 - Maiwald, Michael T1 - Unterscheidung von Mineralwollen mit Nahinfrarot-Spektroskopie (NIRS) T1 - Differentiation of mineral wool by near-infrared spectroscopy (NIRS) N2 - Für die Rückführung von aus Rückbauprojekten anfallender künstlicher Mineralwolle in ihren Herstellungsprozess ist es notwendig, Stein- und Glaswolle zu unterscheiden und voneinander getrennt zu halten. Zu diesem Zweck wurde das Potential von NIR-Spektroskopie (NIRS) für einen werks- oder baustellenseitigen Einsatz getestet. NIRS wird aufgrund kurzer Messzeiten, minimaler Probenvorbereitung und hoher Robustheit der Spektrometer häufig in der Prozessanalytik eingesetzt. Untersucht wurden 70 verschiedene Mineralwollen, wobei sich der Probenumfang sowohl aus werksneuen Proben mit Herstellerangaben als auch unbekannten Proben ohne Spezifikation zusammensetzen, die auf verschiedenen Baustellen in den Jahren 2016–2017 entnommen oder von Deponien zur Verfügung gestellt worden waren. Als Referenzmethode wurde die Röntgenfluoreszenzanalyse verwendet, um den Mineralwolle-Typ über den Elementgehalt nach VDI 3492 zu identifizieren. Mit Hilfe eines multivariaten Datenanalyseverfahrens konnte schließlich eine Methode etabliert werden, die eine zuverlässige Identifikation von unbekannten Mineralwollen anhand deren NIR-Spektren als Stein- bzw. Glaswolle ermöglicht. N2 - For the recirculation of artificial mineral wool resulting from deconstruction projects to the production process, it is necessary to distinguish between rock wool and glass wool. For this purpose, the potential of NIR spectroscopy (NIRS) was tested for the application directly on construction site or in factory. NIRS is often used in process analytics due to short measurement times, minimal sample preparation and high robustness of the spectrometers. In this study 70 mineral wool samples were examined, including both new samples with manufacturer`s specifications and unknown samples without specifications, which were taken at various German construction sites between 2016 and 2017 or which were provided by landfills. X-ray fluorescence spectroscopy was used as a reference method to identify the mineral wool type via the element content according to VDI 3492. With the help of a multivariate data analysis method finally a method was established, which allows a reliable identification of unknown mineral wool based on its NIR spectra as rock or glass wool. KW - Recycling KW - NIR KW - Baustoffe KW - Chemometrie PY - 2020 VL - 95 IS - 12 SP - 463 EP - 472 PB - VDI Fachmedien GmbH & Co. KG CY - Düsseldorf AN - OPUS4-51851 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea A1 - Breitfeld, S. A1 - Sauer, Andreas A1 - Becker, Roland A1 - Kalbe, Ute A1 - Bremser, Wolfram A1 - Braun, Ulrike T1 - A Raman spectroscopic method for the monitoring of microplastics in soil N2 - Due to the increasing presence of microplastic particles (MP) in the Environment and the unknown risks arising from them, there is an urgent need for analytical methods that allow for an efficient identification and quantification of microplastics (MP), i.e. particles < 5 mm, in environmental samples. So far, mostly timeconsuming (micro) infrared or micro-Raman spectroscopic methods are applied. Here an faster alternative Approach is presented based on a Raman processspectrometer with fiber-optical probes in combination with multivariate data analysis. T2 - 12. Kolloquium Prozessanalytik CY - Berlin, Germany DA - 28.11.2016 KW - Raman spectroscopy KW - Microplastics KW - Soil KW - Chemometrics KW - PLS-DA PY - 2016 SP - P10, 59 EP - 60 AN - OPUS4-38392 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hoehse, M. A1 - Paul, Andrea A1 - Gornushkin, Igor B. A1 - Panne, Ulrich T1 - Multivariate classification of pigments and inks using combined Raman spectroscopy and LIBS N2 - The authenticity of objects and artifacts is often the focus of forensic analytic chemistry. In document fraud cases, the most important objective is to determine the origin of a particular ink. Here, we introduce a new approach which utilizes the combination of two analytical methods, namely Raman spectroscopy and laser-induced breakdown spectroscopy (LIBS). The methods provide complementary information on both molecular and elemen tal composition of samples. The potential of this Hyphen ation of spectroscopic methods is demonstrated for ten blue and black ink samples on white paper. LIBS and Raman spectra from different inks were fused into a single data matrix, and the number of different groups of inks was determined through multivariate analysis, i.e., principal component analysis, soft independent modelling of class analogy, partial least-squares discriminant analysis, and support vector machine. In all cases, the results obtained with the combined LIBS and Raman spectra were found to be superior to those obtained with the individual Raman or LIBS data sets. KW - Pigments KW - Raman KW - LIBS KW - Chemometrics PY - 2012 DO - https://doi.org/10.1007/s00216-011-5287-6 SN - 1618-2642 SN - 1618-2650 VL - 402 IS - 4 SP - 1443 EP - 1450 PB - Springer CY - Berlin AN - OPUS4-25440 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wander, Lukas A1 - Paul, Andrea A1 - Rurack, Knut A1 - Biyikal, Mustafa A1 - Juritsch, Elevtheria A1 - Bernstein, Thomas A1 - Bartholmai, Matthias A1 - Noske, Reinhard T1 - Kompaktsensor zur Online-Überwachung von Nitroaromaten N2 - Nitroaromaten und insbesondere Trinitrotoluol (TNT) sind weit verbreitete Spreng- und Umweltschadstoffe. Die größte Herausforderung bei der Detektion von TNT in der Gasphase ist der geringe Dampfdruck. Derzeit werden vielerorts günstige, schnelle, handliche und einfach zu bedienende Alternativen zur klassischen TNT-Analytik entwickelt. Aktuell existieren keine einheitlichen Richtlinien für Sprengstoffsensoren. Hier wird die Entwicklung eines Messplatzes zur Validierung von Sprengstoffsensoren sowie die Erprobung eines kompakten Mustersensors vorgestellt. T2 - 12. Kolloquium Prozessanalytik CY - Berlin, Germany DA - 28.11.2016 KW - Nitroaromaten KW - Fluoreszenzlöschung KW - Sensor PY - 2016 SP - P11, 61 EP - 62 AN - OPUS4-38402 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - Multivariate Datenanalyse von UV/VIS-Spektren zur Bestimmung der Photoisomere von Tearalenon T2 - 8. Kolloquium Prozessanalytik, BAM CY - Berlin, Germany DA - 2012-12-03 PY - 2012 AN - OPUS4-28096 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Paul, Andrea A1 - Dziallas, C. A1 - Zwirnmann, E. A1 - Gjessing, E.T. A1 - Grossart, H.-P. T1 - UV irradiation of natural organic matter (NOM): impact on organic carbon and bacteria N2 - UV-induced transformation of dissolved organic matter (DOC) is often accompanied by reduction of molecular weight and aromaticity and an increase of low-molecular weight (LMW) matter that can be utilized as a substrate by heterotrophic bacteria. Moreover, the generation of reactive transients and mineralization of DOC occurs. For a better understanding of the modification that starts after irradiation and to distinguish between possible chemical and biological modifications, we selected different natural organic matter (NOM) from Norway and Germany. The aqueous solutions were treated by UV irradiation and divided into two aliquot samples. NaN3 anti-bacterial treatment was applied to one sample, and high-pressure size-exclusion chromatography (HPSEC) analysis was used for both. In all samples, we found typical modifications of NOM after UV irradiation. Incubation (>7 days) of UV-irradiated NOM samples resulted in lower levels of LMW matter and increased aromaticity. Parallel to these changes of carbon fractions, an increase in bacterial cell numbers was observed. Addition of NaN3 to NOM, however, inhibited the reduction of LMW matter, indicating that microbial activity accounted for the observed changes in NOM. Analysis of the bacterial community composition by denaturing gradient gel electrophoresis (DGGE) of the amplified 16S rRNA genes revealed that bacterial communities of non-irradiated and UV-irradiated NOM were different and that UV selected for specific members of α-proteobacteria, β-proteobacteria, and Bacteriodetes. Our results imply that after UV-irradiation of NOM, specific bacterial members are well adapted to low pH, high LMW DOC concentrations, and oxidative stress, and therefore thrive well on UV-irradiated humic matter. KW - Humic matter KW - Bacteria KW - High-pressure size-exclusion chromatography (HPSEC) KW - UVC KW - Denaturing gradient gel electrophoresis (DGGE) KW - Sequencing PY - 2012 DO - https://doi.org/10.1007/s00027-011-0239-y SN - 1015-1621 SN - 0036-7842 VL - 74 IS - 3 SP - 443 EP - 454 PB - Springer CY - Basel ; Heidelberg AN - OPUS4-26182 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 - TY - JOUR A1 - Goedecke, Caroline A1 - Mülow-Stollin, Ulrike A1 - Hering, S. A1 - Richter, Janine A1 - Piechotta, Christian A1 - Paul, Andrea A1 - Braun, Ulrike T1 - A first pilot study on the sorption of environmental pollutants on various microplastic materials N2 - With the drastic increase in plastic production, the input of plastic particles into the environment has become a recognised problem. Xenobiotics are able to sorb to polymer materials, and this process is further enhanced where they Encounter microplastics (plastic fragments <5 mm). In this work we studied the sorption of metformin, a type-2 diabetes drug, and difenoconazole, a fungicide, onto the virgin polymer materials polyamide (PA), polypropylene (PP), and polystyrene (PS). Additionally, PP was cryo-milled and PA was treated with acid to investigate the influence of an increase in surface area and chemical modification. The material properties were also studied by dynamic scanning calorimetry (DSC), gel permeation chromatography (GPC) and Fourier transform infrared spectroscopy (FTIR). Sorption experiments were performed on the basis of a full factorial design examining the effect of agitation, pH value, and salinity. Experimental results showed that difenoconazole sorbs readily to all microplastics, whereas the more polar analyte metformin did not show any affinity to the materials used. For difenoconazole the governing factor in all cases is agitation, while both pH and salinity exhibited only a slight influence. The modification of polymers leads to enhanced sorption, indicating that an increase in surface area (cryo-milled PP) or inner volume (acid-treated PA) strongly favours adsorption. Moreover, long-term experiments demonstrated that the time until equilibrium is reached depends strongly on the particle size. KW - Difenoconazole KW - Metformin KW - Plastic debris KW - Polymer KW - Dynamic scanning calorimetry PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-402393 DO - https://doi.org/10.4172/2380-2391.1000191 SN - 2380-2391 VL - 4 IS - 1 SP - Article 1000191, 1 EP - 8 PB - Omics International CY - Los Angeles AN - OPUS4-40239 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gentzmann, Marie A1 - Paul, Andrea A1 - Serrano, Juan A1 - Adam, Christian T1 - Understanding scandium leaching from bauxite residues of different geological backgrounds using statistical design of experiments N2 - The leaching behavior of scandium (Sc) from bauxite residues can differ significantly when residues of different geological backgrounds are compared. The mineralogy of the source rock and the physicochemical environment during bauxitization affect the association of Sc in the bauxite i.e., how Sc is distributed amongst different mineral phases and whether it is incorporated in and/or adsorbed onto those phases. The Sc association in the bauxite is in turn crucial for the resulting Sc association in the bauxite residue. In this study systematic leaching experiments were performed on three different bauxite residues using a statistical design of experiments approach. The three bauxite residues compared originated from processing of lateritic and karstic bauxites from Germany, Hungary, and Russia. The recovery of Sc and Fe was determined by ICP-OES measurements. Mineralogical changes were analyzed by X-ray-diffraction and subsequent Rietveld refinement. The effects of various parameters including temperature, acid type, acid concentration, liquid-to-solid ratio and residence time were studied. A response surface model was calculated for the selected case of citric acid leaching of Hungarian bauxite residue. The investigations showed that the type of bauxite residue has a strong influence. The easily leachable fraction of Sc can vary considerably between the types, reaching ~20–25% in German Bauxite residue and ~50% in Russian bauxite residue. Mineralogical investigations revealed that a major part of this fraction was released from secondary phases such as cancrinite and katoite formed during Bayer processing of the bauxite. The effect of temperature on Sc and Fe recovery is strong especially when citric acid is used. Based on the exponential relationship between temperature and Fe-recovery it was found to be particularly important for the selectivity of Sc over Fe. Optimization of the model for a maximum Sc recovery combined with a minimum Fe recovery yielded results of ~28% Sc recovery at <2% Fe recovery at a temperature of 60 ◦C, a citric acid normality of 1.8, and a liquid-to-solid ratio of 16 ml/g. Our study has shown that detailed knowledge about the Sc association and distribution in bauxite and bauxite residue is key to an efficient and selective leaching of Sc from bauxite residues. KW - Bauxite residue KW - Scandium KW - Leaching KW - Design of experiments KW - Red mud PY - 2022 DO - https://doi.org/10.1016/j.gexplo.2022.107041 SN - 0375-6742 VL - 2022 IS - 240 SP - 1 EP - 13 PB - Elsevier Science CY - Amsterdam AN - OPUS4-55531 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nadejde, C. A1 - Neamtu, M. A1 - Hodoroaba, Vasile-Dan A1 - Schneider, Rudolf A1 - Paul, Andrea A1 - Ababei, G. A1 - Panne, Ulrich T1 - Tannic acid- and natural organic matter-coated magnetite as green Fenton-like catalysts for the removal of water pollutants N2 - The use of magnetic materials as heterogeneous catalysts has attracted increasing attention in the last years since they proved to be promising candidates for water treatment. In the present study, two types of surface-modified magnetite (Fe3O4) nanoparticles, coated with non-hazardous naturally occurring agents—either tannic acid (TA) or dissolved natural organic matter—were evaluated as magnetic heterogeneous catalysts. Chemical synthesis (co-precipitation) was chosen to yield the nanocatalysts due to its well-established simplicity and efficiency. Subsequently, the properties of the final products were fully assessed by various characterization techniques. The catalytic activity in heterogeneous oxidation of aqueous solutions containing a model pollutant, Bisphenol A (BPA), was comparatively studied. The effect of operational parameters (catalyst loading, H2O2 dosage, and UV light irradiation) on the Degradation performance of the oxidation process was investigated. The optimum experimental parameters were found to be 1.0 g/L of catalysts and 10 mM H2O2, under UV irradiation. The highest mineralization rates were observed for Fe3O4-TA catalyst. More than 80 % of BPA was removed after 30 min of reaction time under the specified experimental conditions. The obtained results showed that the two catalysts studied here are suitable candidates for the removal of pollutants in wastewaters by means of heterogeneous reaction using a green sustainable treatment method. KW - Nanocatalysts KW - Photo-Fenton oxidation KW - Wastewater KW - Bisphenol A degradation KW - Environment KW - Mitigation PY - 2015 UR - http://link.springer.com/article/10.1007/s11051-015-3290-0 DO - https://doi.org/10.1007/s11051-015-3290-0 VL - 17 IS - 12 SP - 476 (1) EP - 476 (10) PB - Springer AN - OPUS4-38758 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neamtu, Mariana A1 - Nadejde, C. A1 - Hodoroaba, Vasile-Dan A1 - Schneider, Rudolf A1 - Paul, Andrea A1 - Ababei, G. A1 - Panne, Ulrich T1 - Green Fenton-like magnetic nanocatalysts: Synthesis, characterization and catalytic application N2 - Five iron oxalate core–shell magnetite nanoparticles catalysts are evaluated as magnetic heterogeneous materials. Simple and efficient procedures for the preparation of magnetic iron oxalate coated nanoparticles are presented. The catalysts are fully characterized using various investigation techniques. Additionally, the formation of photo-sensitized oxygen by spin-trapping using electron spin resonance is investigated. The catalytic activity of two model substrates (carbamazepine and bisphenol A) is also evaluated. The effect of operational parameters (catalyst and H2O2 concentration, UVA light) on the degradation performance of the oxidation process is investigated. The obtained reaction rates depend on the nature of the compound and increase with iron oxide shell thickness of the catalyst. Moreover, these materials show a significant activity during two consecutive tests. The optimum experimental parameters are found to be 1.0 g L−1 of catalysts, 10 mM H2O2, under UVA irradiation. More than 99% of both substrates are removed after 30 min of reaction time under the experimental conditions given above. The results obtained show that the catalysts are suitable candidates for the removal of pollutants in wastewaters by means of the Fenton heterogeneous reaction. KW - Five iron oxalate core–shell magnetite nanoparticles catalysts are evaluated as magnetic heterogeneous KW - Characterization KW - Micropollutants PY - 2015 DO - https://doi.org/10.1016/j.apcatb.2015.04.050 SN - 0926-3373 SN - 1873-3883 VL - 176-177 SP - 667 EP - 677 PB - Elsevier AN - OPUS4-40072 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - Hybridmodell zur Bestimmung des Ligningehalts von Kiefernholz N2 - Die Untersuchungen sind durch das das DFG Schwerpunktprogramm 1374 für Biodiversitätsforschung motiviert. Anhand des überwachten Abbaus von Totholz soll untersucht werden, welche Auswirkung unterschiedliche Formen und Intensitäten der Landnutzung auf die Biodiversität innerhalb von drei Exploratorien zeigen. Bei den vorangegangenen Studien wurden Nahrungs¬netzte auf organismischer Ebene sowie Klima- und Umgebungsdaten untersucht und die Veränderung des ausgebrachten Totholzes als Masseverlust erfasst. Es wird jedoch erwartet, dass in Anhängigkeit der beteiligten Organismen und Umgebungsparameter verschiedene Mechanismen des Holzabbaus vorliegen, die in unterschiedlichen Abbauraten der Holzkomponenten Lignin, Cellulose und Hemicellulose resultieren. Aus diesem Grund ist die quantitative Untersuchung des Ligningehalts an Hölzern ein wesentlicher Schritt für ein verbessertes Verständnis der Biodiversität in den untersuchten Exploratorien. Um der hohen Probenanzahl, die sich aus der Kontrolle von jeweils 100 Proben (Plots) in den drei Exploratorien für Hölzer aus 13 Baumarten ergibt, gerecht zu werden, wird eine schnelle und effiziente Untersuchungsmethode benötigt. Diese wird derzeit in Form einer NIR-spektroskopischen Bestimmung des Ligningehalts entwickelt. Um basierend auf den NIR Spektren vermahlener Holzproben Lignin und weitere Holzkomponenten korrekt vorherzusagen, muss zunächst basierend auf nasschemischen Analysen ein chemometrisches Modell kalibriert werden. Dazu ist die Charakterisierung von mindestens 20 – 30 Proben, die eine hohe Varianz des Ligningehalts aufweisen, notwendig. Im Vortrag werden erste Untersuchungs¬ergebnisse für die Vorhersage des Ligningehalts von Kiefernhölzern, die für ein Jahr in dem Exploratorium Schorfheide exponiert wurden, vorgestellt. Die anschließende explorative Datenanalyse (PCA) unter Verwendung von insgesamt 28 Variablen zur Beschreibung klimatischer und Umgebungsparameter weist eine Reihe interessanter Korrelationen auf. Demnach ist der Ligningehalt auf der ersten Hauptkomponente (29% erklärte Varianz) positiv mit dem C/N-Verhältnis und negativ mit Landnutzungsindex korreliert. Masseverlust und Temperatur hingegen dominieren die zweite Hauptkomponente (12% erklärte Varianz). T2 - 4. Innovationsakademie Lignocellulose CY - Berlin, Germany DA - 11.04.2019 KW - NIR Spektroskopie KW - Lignin KW - Datenanalyse PY - 2019 AN - OPUS4-47963 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - NIR-Ringversuch II: Erste Ergebnisse N2 - Vorstellung der Ergebnisse des Ringversuchs NIR II für den Analyten Paracetamol. Neben den "S-Shape" Darstellungen für die Levels A, B und C werden En-Werte und eine Darstellung der relativen Unsicherheiten (Horwitz) gezeigt. Alle beteiligten Labors zeichnen sich durch eine hohe Performance aus. T2 - 15. Ttreffen PAT RFA CY - Lonza, Visp, Switzerland DA - 17.09.2019 KW - Nahinfrarotspektroskopie KW - Ringversuch PY - 2019 AN - OPUS4-49043 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neamtu, M. A1 - Macaev, F. A1 - Boldescu, V. A1 - Hodoroaba, Vasile-Dan A1 - Nadejde, C. A1 - Schneider, Rudolf A1 - Paul, Andrea A1 - Ababei, G. A1 - Panne, Ulrich T1 - Removal of pollutants by the new Fenton-like highly active catalysts containing an imidazolium salt and a Schiff base N2 - Two iron-based molten salts comprising an imidazolium and Schiff base were evaluated as catalysts for removal of carbamazepine (CBZ) from water. The catalysts were fully characterized using scanning electron microscopy (SEM), energy-dispersive X-ray spectrometry (EDX), nuclear magnetic resonance spectroscopy (NMR), electrospray ionisation–mass spectrometry (ESI–MS), differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FTIR) and nitrogen adsorption–desorption isotherms (BET). Additionally, the formation of photo-sensitized oxygen was investigated by spin-trapping using electron spin resonance (ESR). The catalytic activity in heterogeneous oxidation of the micropollutant (CBZ) was also evaluated. The effects of catalyst loading, pH, H2O2 dosage and UV light on the oxidation of the selected compound were investigated. After 15 min of UVA irradiation in the presence of 200 μM H2O2, CBZ was completely removed over both catalysts. KW - Fe-based highly active ionic liquids KW - Characterization of catalysts KW - Removal KW - Singlet oxygen KW - Carbamazepine PY - 2016 DO - https://doi.org/10.1016/j.apcatb.2015.10.032 SN - 0926-3373 VL - 183 SP - 335 EP - 342 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-35382 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nadejde, C. A1 - Neamtu, M. A1 - Hodoroaba, Vasile-Dan A1 - Schneider, Rudolf A1 - Paul, Andrea A1 - Ababei, G. A1 - Panne, Ulrich T1 - Green Fenton-like magnetic nanocatalysts: Synthesis, characterization and catalytic application N2 - Five iron oxalate core–shell magnetite nanoparticles catalysts are evaluated as magnetic heterogeneous materials. Simple and efficient procedures for the preparation of magnetic iron oxalate coated nanoparticles are presented. The catalysts are fully characterized using various investigation techniques. Additionally, the formation of photo-sensitized oxygen by spin-trapping using electron spin resonance is investigated. The catalytic activity of two model substrates (carbamazepine and bisphenol A) is also evaluated. The effect of operational parameters (catalyst and H2O2 concentration, UVA light) on the degradation performance of the oxidation process is investigated. The obtained reaction rates depend on the nature of the compound and increase with iron oxide shell thickness of the catalyst. Moreover, these materials show a significant activity during two consecutive tests. The optimum experimental parameters are found to be 1.0 g L-1 of catalysts, 10 mM H2O2, under UVA irradiation. More than 99% of both substrates are removed after 30 min of reaction time under the experimental conditions given above. The results obtained show that the catalysts are suitable candidates for the removal of pollutants in wastewaters by means of the Fenton heterogeneous reaction. KW - Magnetic core–shell nanocatalysts KW - Characterization KW - Fenton oxidation KW - Micropollutants KW - Water treatment PY - 2015 DO - https://doi.org/10.1016/j.apcatb.2015.04.050 SN - 0926-3373 SN - 1873-3883 VL - 176-177 SP - 667 EP - 677 PB - Elsevier CY - Amsterdam AN - OPUS4-33820 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 - JOUR 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 - Pereira Remelhe, M. A1 - Maiwald, Michael T1 - Flexible automation with compact NMR spectroscopy for continuous production of pharmaceuticals N2 - Modular plants using intensified continuous processes represent an appealing concept for the production of pharmaceuticals. It can improve quality, safety, sustainability, and profitability compared to batch processes; besides, 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 is based on a compact nuclear magnetic resonance (NMR) spectrometer. The NMR sensor is a benchtop device enhanced to the requirements of automated chemical production including robust evaluation of sensor data. Beyond monitoring the product quality, online NMR data was used in a new iterative optimization approach to maximize the plant profit and served as a reliable reference for the calibration of a near-infrared (NIR) spectrometer. The overall approach was demonstrated on a commercial-scale pilot plant using a metal-organic reaction with pharmaceutical relevance. KW - NMR Spectroscopy KW - NIR Spectroscopy KW - Real-time process monitoring KW - Real-time quality control KW - Continuous processes KW - CONSENS KW - Data Fusion PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-480623 DO - https://doi.org/10.1007/s00216-019-01752-y SN - 1618-2642 SN - 1618-2650 VL - 411 IS - 14 SP - 3037 EP - 3046 PB - Springer Nature CY - Heidelberg AN - OPUS4-48062 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gojani, Ardian A1 - Palásti, David J. A1 - Paul, Andrea A1 - Galbács, G. A1 - Gornushkin, Igor B. T1 - Analysis and classification of liquid samples by spatial heterodyne spectroscopy N2 - Spatial heterodyne spectroscopy (SHS) is used for quantitative analysis and classification of liquid samples. SHS is a version of a Michelson interferometer with no moving parts and with diffraction gratings in place of mirrors. The instrument converts frequency-resolved information into spatially resolved one and records it in the form of interferograms. The back-extraction of spectral information is done by the Fast Fourier transform. A SHS instrument is constructed with the resolving power 5000 and spectral range 522 - 593 nm. Two original technical solutions are used as compared to previous SHS instruments: the use of a high frequency diode pumped solid state (DPSS) laser for excitation of Raman spectra and a microscope-based collection system. Raman spectra are excited at 532 nm at the repetition rate 80 kHz. Raman shifts between 330 cm-1 and 1600 cm-1 are measured. A new application of SHS is demonstrated: for the first time it is used for quantitative Raman analysis to determine concentrations of cyclohexane in isopropanol and glycerol in water. Two calibration strategies are employed: univariate based on the construction of a calibration plot and multivariate based on partial least square regression (PLSR). The detection limits for both cyclohexane in isopropanol and glycerol in water are at a 0.5 mass% level. In addition to the Raman-SHS chemical analysis, classification of industrial oils (biodiesel, poly(1-decene), gasoline, heavy oil IFO380, polybutenes, and lubricant) is performed using their Raman-fluorescence spectra and principal component analysis (PCA). The oils are easily discriminated as they show distinct non-overlapping patterns in the space of principal components. KW - Spectroscopy KW - Atomic KW - Laser induced breakdown KW - Lasers PY - 2019 DO - https://doi.org/10.1177/0003702819863847 SN - 1943-3530 VL - 73 IS - 12 SP - 1409 EP - 1419 PB - Sage AN - OPUS4-48599 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nadejde, C. A1 - Neamtu, Mariana A1 - Hodoroaba, Vasile-Dan A1 - Schneider, Rudolf A1 - Paul, Andrea A1 - Ababei, G. A1 - Panne, Ulrich T1 - Green Fenton-like catalysts for the removal of water pollutants N2 - Two types of surface modified magnetite (Fe3O4) nanoparticles, coated with either tannic acid (TA) or dissolved natural organic matter (NOM), were evaluated as magnetic heterogeneous catalysts. Simple and efficient procedures for the synthesis of the magnetic catalysts were employed, their properties being fully assessed by various characterization techniques. The catalytic activity in heterogeneous oxidation of aqueous solutions containing Bisphenol A (BPA) over the catalysts was comparatively studied. The optimum experimental parameters were: 1g/L of catalysts, 10 mM H2O2, under UV irradiation. The highest mineralization rates were observed for Fe3O4-TA catalyst. More than 80% of BPA were removed after 30 minutes of reaction time under the specified experimental conditions. The results showed that the obtained catalysts are suitable candidates for the removal of pollutants in wastewaters by means of heterogeneous reaction T2 - TechConnect World Innovation Conference Nanotech 2015 CY - Washington, DC, Maryland, USA DA - 14.06.2015 KW - Nanocatalysts KW - Characterization KW - Fenton oxidation KW - Wastewater KW - Bisphenol A degradation PY - 2015 SN - 978-1- 4987-4733-2 SN - 978-1-4987-4728-8 VL - 2 SP - 87 EP - 90 PB - CRC Press, Taylor&Francis Group AN - OPUS4-40074 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Haferkamp, Sebastian A1 - Paul, Andrea A1 - Michalchuk, Adam A1 - Emmerling, Franziska T1 - Unexpected polymorphism during a catalyzed mechanochemical Knoevenagel condensation N2 - The transformation of a base-catalyzed, mechano-assisted Knoevenagel condensation of mono-fluorinated benzaldehyde derivatives (p-, m-, o-benzaldehyde) with malonodinitrile was investigated in situ and in real time. Upon milling, the para-substituted product was found to crystallize initially into two different polymorphic forms, depending on the quantity of catalyst used. For low catalyst concentrations, a mechanically metastable phase (monoclinic) was initially formed, converting to the mechanically stable phase (triclinic) upon further grinding. Instead, higher catalyst concentrations crystallize directly as the triclinic product. Inclusion of catalyst in the final product, as evidenced by mass spectrometric analysis, suggests this complex polymorphic pathway may be due to seeding effects. Multivariate analysis for the in situ Raman spectra supports this complex formation pathway, and offers a new approach to monitoring multi-phase reactions during ball milling. KW - Ball milling KW - C-C coupling KW - In situ KW - Mechanochemistry KW - Multivariate data analysis PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-481872 DO - https://doi.org/10.3762/bjoc.15.110 SN - 1860-5397 VL - 15 SP - 1141 EP - 1148 PB - Beilstein Insitut CY - Frankfurt am Main AN - OPUS4-48187 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Altmann, Korinna A1 - Goedecke, Caroline A1 - Bannick, C.-G. A1 - Abusafia, A. A1 - Scheid, C. A1 - Steinmetz, H. A1 - Paul, Andrea A1 - Beleites, C. A1 - Braun, U. T1 - Identification of microplastic pathways within a typical European urban wastewater system N2 - In recent years, thermoextraction/desorption-gas chromatography/mass spectrometry (TED-GC/MS) has been developed as a rapid detection method for the determination of microplastics (MP) mass contents in numerous environmentally relevant matrices and, in particular, for the measurement of polymers in water samples without time-consuming sample preparation. The TED-GC/MS method was applied to investigate a typical European municipal wastewater system for possible MP masses. Such investigations are important in view of the recent revision of the Urban Wastewater Treatment Directive. Four different representative sampling sites were selected: greywater (domestic wastewater without toilet), combined sewer, and influent and effluent of a wastewater treatment plant (WWTP). All samples were collected by fractional filtration. Filtration was carried out over mesh sizes of 500, 100, 50, and in some cases, 5 µm. Polyethylene (PE), polypropylene (PP), and polystyrene (PS) were detected in all samples, with the PE fraction dominating in all cases. Styrene-butadiene rubber which serves as an indication of tire abrasion, was only found in the influent of the WWTP. The highest MP mass contents were found in the combined sewer, so MP can become a source of pollution during heavy rain events when the capacity limits of the effluent are reached, and the polluted effluent is released uncontrolled into the environment. Based on the studies, MP retention from the WWTP could be estimated to be approximately 96%. Few trends in polymer type or mass contents were detected within the different fractions of the samples or when comparing samples to each other. KW - Microplastics KW - Microplastic analysis KW - TED-GC/MS KW - Microplastic pathways KW - Mass contents PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568289 DO - https://doi.org/doi.org/10.1002/appl.202200078 SP - 1 EP - 10 PB - Wiley-VCH CY - Weinheim AN - OPUS4-56828 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bremser, Wolfram A1 - Paul, Andrea A1 - Neugebauer, Michael A1 - Maiwald, Michael A1 - Brudel, M. T1 - Immer im Bild mittels Prozess-Spektroskopie - Spektroskopische Methoden für die Prozessanalytik N2 - Spektroskopische Methoden sind in der Regel zerstörungsfrei und liefern stetig Informationen, die zur Prozess-Steuerung eingesetzt werden können. Präzise Messungen unter Prozessbedingungen wurden vor allem durch die Entwicklung leistungsfähiger Sonden und Durchfluss-Systeme möglich. In Kombination mit multivariater Datenanalyse lassen sich diese Methoden auch zur Identifizierung und Quantifizierung von Stoffströmen einsetzen. PY - 2012 SN - 0016-3538 VL - 56 IS - 6 SP - 436 EP - 439 PB - GIT-Verlag CY - Darmstadt AN - OPUS4-26243 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -