TY - CONF A1 - Maiwald, Michael T1 - Quantitative NMR Spectroscopy (qNMR) as an Indispensable Instrumental Analytical Method and its Metrological Application N2 - Introduction NMR spectroscopy is one of the most important analytical methods in organic chemistry. While most analyses are carried out qualitatively with the aim of substance identification and structure elucidation, quantitative NMR spectroscopy (qNMR) is increasingly gaining importance in research and industry. qNMR provides the most universally applicable form of direct purity determination without need for reference materials of impurities or the calculation of response factors but only exhibiting suitable NMR properties. Methods One of the most attractive features of quantitative NMR spectroscopy is that the NMR peak areas can be used directly for concentration quantification without further calibration. Another advantage of NMR spectroscopy is that the method has a high linearity between absolute signal area and sample concentration, which makes it an absolute analytical comparison method that is independent of the matrix. This enables automated robust data evaluation strategies that can be used for online applications of qNMR spectroscopy. Jancke et al. proposed NMR spectroscopy as a relative primary analytical method because it can be fully described by mathematical equations from which a complete uncertainty budget can be derived, allowing it to be used at the highest metrological level. Weber et al. discussed in detail important aspects of the procedure that enable the realisation of low measurement uncertainties in qNMR measurements. Since certification of CRM requires expanded mea¬sure¬ment uncertainties of less than 0.5 % (relative), the work of Weber et al. demonstrated for the first time that qNMR can fulfil this criterion. Results To date, further comparative studies have been carried out in metrology and industry, demonstrating the performance of quantitative NMR spectroscopy and further reducing measurement uncertainties. The development of validation concepts and the commercial availability of suitable certified reference materials facilitate the application, especially in the usually highly regulated industrial environment. Users can thus accelerate the development of analytical methods. The talk will cover a wide range of topics from current metrological activities to new challenges for qNMR spectroscopy and also deals with aspects such as validation and accreditation. Innovative aspects • qNMR provides the most universally applicable form of direct purity determination • Expanded measurement uncertainties lower than 0.15 % (relative) possible • Benchtop NMR instruments increasingly used for qNMR spectroscopy T2 - ANAKON 2023 CY - Vienna, Austria DA - 11.04.2023 KW - Quantitative NMR Spectroscopy KW - qNMR KW - Process Analytical Technology KW - NMR Validation KW - NMR Accreditation KW - Purity KW - ANAKON PY - 2023 AN - OPUS4-57304 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Online NMR spectroscopy paves the way for short development times in industrial reaction and process monitoring N2 - Modular chemical production is a tangible implementation of the digital transformation of the specialty chemicals process industry. In particular, it enables acceleration of process development and thus faster time to market by flexibly interconnecting and orchestrating standardized physical modules and bringing them to life. For this purpose, specific (chemical) sensors of process analytics are needed, preferably without lengthy calibration or spectroscopic model development. An excellent example of a "direct" analytical method is online nuclear magnetic resonance (NMR) spectroscopy. NMR spectroscopy meets the requirements of a direct analytical method because of the direct correlation between the signal area in the spectrum ("counting" the nuclear spins) and the analyte amount of substance concentrations. It is also extremely linear over the concentration range. With the availability of compact benchtop NMR instruments, it is now possible to bring NMR spectroscopy directly into the field, in close proximity to specialized laboratory facilities, pilot plants, and even industrial-scale production facilities. The first systems are in TRL 8 (Qualified System with Proof of Functionality in the Field). The presentation will discuss the many building blocks of online nuclear magnetic resonance spectroscopy, from flow cells to automated data analysis. T2 - SFB 1527 HyPERiON “High Performance Compact Magnetic Resonance“ Online Seminar CY - Karlsruhe, Germany DA - 06.07.2023 KW - Online NMR Spectroscopy KW - Process Monitoring KW - Reaction Monitoring KW - Industry 4.0 KW - Automation KW - Modular Production PY - 2023 AN - OPUS4-57862 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - Remelting Miwo - Methoden für die Vor-Ort Analytik N2 - In Deutschland werden jährlich rund 20 Millionen Tonnen künstliche Mineralwolle für die Dämmung von Dächern und Fassaden sowie für Brandschutzprodukte verwendet. Um künstliche Mineralwolle aus Rückbaumaßnahmen in den Produktionsprozess zurückführen zu können, ist eine Trennung in Glas- und Steinwolle erforderlich, um eine Vermischung der beiden Produkte, die unterschiedliche Schmelztemperaturen aufweisen, zu vermeiden. Anstatt die Mineralwolle in spezielle Labors zu schicken, was zeitaufwendig und teuer ist, wurde das Potenzial eines tragbaren Nahinfrarot-Spektrometers (NIR) für den Einsatz vor Ort getestet. 140 verschiedene Mineralwolleproben wurden untersucht, um eine NIR-basierte Methode für die Vor-Ort-Unterscheidung zwischen Glas- und Steinwolle zu etablieren. Die Validierung der Methode mit Testproben und die Anwendung auf Materialien, die aus BigBags für Deponien entnommen wurden, haben gezeigt, dass die Methode präzise und robust ist. Als Referenzmethode wurde die Röntgenfluoreszenzspektroskopie (RFA) mit einer Kalibrierung auf der Grundlage der VDI 3492 verwendet. T2 - 23. Projektetage der Bauforschung CY - Online meeting DA - 14.03.2023 KW - NIR KW - RFA KW - Mineralwolle PY - 2023 AN - OPUS4-57372 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bornemann-Pfeiffer, Martin T1 - Modular production involving benchtop NMR Current Application Examples Driven by Digitalization N2 - The demand for increasing product diversity in the chemical and pharmaceutical industry calls for new production processes that enable greater flexibility. Therefore, plants are needed which can be adapted to new processes in a fast manner and be scaled up and down easily to volatile market demands. Modular production techniques in combination with advanced process analytical technology (PAT) are considered as a promising solution able to fulfil these requirements. The success and acceptance of modular concepts in both new and existing plants is dependent of its reliability, easy applicability, and standardization. In recent past, enormous efforts were made to overcome existing barriers in a superordinate level, e.g. DEXPI, ENPRO, or MTP naming just a few. Here, we’d like to present a few, more hands-on, application examples which are shown in Figure 1 aiming to increase process flexibility and applicability. T2 - AK Prozessanalytik Jahrestagung 2022 CY - Amersfoort, The Netherlands DA - 19.09.2022 KW - Process analytical technology KW - NMR spectroscopy KW - Digitization KW - Additive manufacturing PY - 2022 AN - OPUS4-55976 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ziel, Ruben P. A1 - Zalewska, Ewelina A1 - van der Veen, Adriaan M. H. A1 - Kipphardt, Heinrich A1 - Tuma, Dirk A1 - Esteban, Andres Rojo A1 - Fernandez Vicente, Teresa Esperanza A1 - Mace, Tatiana A1 - Sutour, Christophe A1 - Marioni, Fabrice A1 - Fükö, Judit A1 - Szücs, László A1 - Büki, Tamás A1 - Szilágyi Nagyné, Zsófia A1 - Cieciora, Dariusz A1 - Ochman, Grzegorz A1 - Romanowski, Przemysław A1 - Lis, Anna A1 - Garnuszek, Magdalena A1 - Valkova, Miroslava A1 - Ackermann, Andreas A1 - Pascale, Celine A1 - Niederhauser, Bernhard A1 - Tarhan, Tanil A1 - Boztepe, Aylin A1 - Beránek, Jan A1 - Bárta, Miroslav T1 - International comparison EURAMET.QM-K3.2019 - Automotive exhaust gases N2 - EURAMET.QM-K3.2019 was a repeat of the key comparison EURAMET.QM-K3 on the composition of automotive exhaust gases. New in EURAMET.QM-K3.2019 was the addition of the amount fraction oxygen to the programme. The key comparison reference values were obtained independently, using static gravimetry and appropriate corrections from purity analysis and are linked to those of CCQM-K3.2019. The key comparison results show equivalence between the measurement standards maintained by the participating national metrology institutes. The demonstrated equivalence can be used to underpin services related to automotive exhaust gases as well as generically through the flexible scheme ("track A"). KW - CCQM KW - Automotive gases PY - 2023 DO - https://doi.org/10.1088/0026-1394/60/1A/08030 SN - 1681-7575 VL - 60 IS - 1A SP - 1 EP - 63 PB - IOP Publishing CY - Bristol AN - OPUS4-58904 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Sensors, Analytics and Certified Reference Materials safeguarding the quality infrastructure in the hydrogen economy N2 - The prerequisites for a successful energy transition and the economic use of hydrogen as a clean green energy carrier and for H2 readiness are a rapid market ramp-up and the establishment of the required value chains. Reliable quality and safety standards for innovative technologies are the prerequisite for ensuring supply security, for environmental compatibility and sustainable climate protection, for building trust in these technologies and thus enable product and process innovations. With the Competence Centre "H2Safety@BAM", BAM is creating the safety-related prere-quisites for the successful implementation of hydrogen technologies at national as well as European level. BAM uses decades of experience in dealing with hydrogen technologies to develop the necessary quality and safety standards. The presentation will draw a bow from the typical basic tasks of BAM in the field of competence "Sensors, analytics and certified reference materials", such as maintenance and dissemination of the national gas composition standards for calorific value determination as Designated Institute for Metrology in Chemistry within the framework of the Metre Convention, to the further development of measurement and sensor technology for these tasks. For the certification of reference materials, a mostly slow and time-consuming but solid reference analysis is common. With hydrogen and its special properties, completely new requirements are added. In addition, fast and simple online analysis is required for process control, for example to register quality changes, e.g., during load changes or refuelling processes. T2 - Indo-German International Conference on Metrology for the Deployment of Green Hydrogen and Renewable Fuels in India CY - Online meeting DA - 04.04.2022 KW - Quality Infrastructure KW - Gas Reference Material KW - Hydrogen KW - Energy Gases KW - Sensors KW - Hydrogen Storage Materials PY - 2022 UR - https://www.imeko-gh2fuels.ptb.de/ AN - OPUS4-54596 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Integrated and networked systems and processes – A perspective for digital transformation of our chemical and pharmaceutical production N2 - Chemical and pharmaceutical companies have to find new paths to survive successfully in a changing environment, while also finding more flexible ways of product and process development to bring their products to market more quickly – especially high-quality high-end products like fine chemicals or pharmaceuticals. The potential of digital technologies belongs to these. A current approach uses flexible and modular chemical production units, which can produce different high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce the time to market of new products. At the same time, we need to move towards knowledge-based production that takes into account all essential equipment, process and control data from plants and laboratories and makes valuable expertise available and transferable. The potential of data from production together with its contextual information is often not yet consistently used today for a comprehensive understanding of production. By giving examples this paper outlines a possible more holistic approach to digitalisation and the use of machine-based methods in the production of specialty chemicals and pharmaceuticals through the introduction of integrated and networked systems and processes. T2 - GDCh Science Forum 2021 - GDCh Wissenschaftsforum 2021 CY - Online meeting DA - 29.08.2021 KW - Process analytical technology KW - Online NMR spectroscopy KW - Process industry KW - Industry 4.0 KW - Digital transformation KW - Autonomous chemistry PY - 2021 AN - OPUS4-53171 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Klaus, Christian T1 - QI Digital: Cross-Location IT Infrastructure and Asset Administration Shell as a Digital Twin N2 - Im Rahmen der von der BAM und anderen Partnern ins Leben gerufenen Initiative „Digitale Qualitätsinfrastruktur“ liegt der Fokus u.a. auf der Entwicklung von neuen Zertifizierungsworkflows. Dabei ist eine besondere Bedeutung dem Zusammenführen von Operational Technology (OT) und Informationstechnik (IT) beizumessen. Zur Datenintegration aus der Sensor-Feldebene einer Versuchs-Wasserstofftankstelle wurde eine solche Infrastruktur zunächst in einer Laborumgebung aufgebaut. Dieser Vortrag beschreibt die Implementierung des standardisierten und von der Plattform Industrie 4.0 empfohlenen digitalen Zwillings "Verwaltungsschale" an dieser Wasserstofftankstelle. Außerdem wird die Implementierung einer standortübergreifenden IT-Infrastruktur über VPN/5G beschrieben. T2 - BAM Kolloquium Abteilung 1 CY - Berlin, Germany DA - 10.06.2025 KW - Datenintregration KW - IT KW - Infrastruktur KW - OT KW - Open Source KW - Software KW - VPN KW - Verwaltungsschale PY - 2025 AN - OPUS4-63495 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR ED - Schmid, Thomas ED - Dariz, P. T1 - Special issue: Modern Raman spectroscopy of minerals N2 - Dear Colleagues, Raman spectroscopy provides vibrational fingerprints of chemical compounds, enabling their identification via a comparison with reference spectra. This analytical tool has high potential not only in the identification of minerals from natural sources but also for studying the complex microstructure and mineral distribution of both ancient and modern man-made materials, ranging from, e.g., historical ceramics and mortars to modern solar cell materials. In addition to the chemical identity of minerals, Raman spectra are affected by crystal orientations, substoichiometric to stoichiometric compositional changes (e.g., in solid solution series), traces of foreign ions, stress, strain, and crystallinity, enabling a comprehensive physicochemical characterisation of minerals. This Special Issue includes method developments and applications in the field of modern Raman spectroscopy of minerals in a broad sense, from natural mineral deposits to inorganic phases in materials; covers both spectroscopic and imaging studies; and provides a platform for discussing the possibilities and limits of the technique in the context of the existing analytical arsenal. Thomas Schmid Petra Dariz KW - Analytical sciences KW - Raman spectroscopy KW - Raman microspectroscopy KW - Mineral identification KW - Mineral paragenesis PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-519117 UR - https://www.mdpi.com/journal/minerals/special_issues/Raman_Spectroscopy_Minerals VL - 10 SP - 1 EP - 156 PB - MDPI CY - Basel AN - OPUS4-51911 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Chao, Madlen T1 - Entwicklung und Validierung eines Online-LIBS-Verfahrens für die Bestimmung von Nährelementen in Böden N2 - In den letzten Jahrzehnten ist die Nachfrage nach kostengünstigen und flächendeckenden Kartierungsmöglichkeiten im Hinblick auf eine ertragssteigernde und umweltfreundlichere Bewirtschaftung von landwirtschaftlichen Nutzflächen stark gestiegen. Hierfür eignen sich spektroskopische Methoden wie die Röntgenfluoreszenzanalyse (RFA), Raman- und Gammaspektroskopie sowie die laserinduzierte Plasmaspektroskopie (LIBS). In Abhängigkeit von der Funktionsweise der jeweiligen Methoden werden Informationen zu verschiedensten Bodeneigenschaften wie Nährelementgehalt, Textur und pH-Wert erhalten. Ziel dieser Arbeit ist die Entwicklung eines Online-LIBS-Verfahrens zur Nährelementbestimmmung und Kartierung von Ackerflächen. Die LIBS ist eine schnelle und simultane Multielementanalyse bei der durch das Fokussieren eines hochenergetischen Laserpulses Probenmaterial von der Probenoberfläche ablatiert wird und in ein Plasma überführt wird. Beim Abkühlen des Plasmas wird Strahlung emittiert, welche Rückschlüsse über die elementare Zusammensetzung der Probe gibt. Diese Arbeit ist im Teilprojekt I4S (Intelligenz für Böden) im Forschungsprogramm BonaRes (Boden als nachhaltige Ressource für die Bioökonomie) des Bundesministerium für Bildung und Forschung (BMBF) entstanden. Es wurden insgesamt 651 Bodenproben von verschiedenen Test-Agrarflächen unterschiedlichster Standorte Deutschlands gemessen, ausgewertet und zu Validierungszwecken mit entsprechender Referenzanalytik wie die Optische Emissionsspektroskopie mittels induktiv gekoppeltem Plasma (ICP-OES) und die wellenlängendispersive Röntgenfluoreszenzanalyse (WDRFA) charakterisiert. Für die Quantifizierung wurden zunächst die Messparameter des LIBS-Systems auf die Bodenmatrix optimiert und für die Elemente geeignete Linien ausgewählt sowie deren Nachweisgrenzen bestimmt. Es hat sich gezeigt, dass eine absolute Quantifizierung basierend auf einem univariaten Ansatz aufgrund der starken Matrixeffekte und der schlechten Reproduzierbarkeit des Plasmas nur eingeschränkt möglich ist. Bei Verwendung eines multivariaten Ansatz wie der Partial Least Squares Regression (PLSR) für die Kalibrierung konnten für die Nährelemente im Vergleich zur univariaten Variante Analyseergebnisse mit höherer Güte und geringeren Messunsicherheiten ermittelt werden. Die Untersuchungen haben gezeigt, dass das multivariate Modell weiter verbessert werden kann, indem mit einer Vielzahl von gut analysierten Böden verschiedener Standorte, Bodenarten und einem breiten Gehaltsbereich kalibriert wird. Mithilfe der Hauptkomponentenanalyse (PCA) wurde eine Klassifizierung der Böden nach der Textur realisiert. Weiterhin wurde auch eine Kalibrierung mit losem Bodenmaterial erstellt. Trotz der Signalabnahme konnten für die verschiedenen Nährelemente Kalibriergeraden mit ausreichender, analytischer Güte erstellt werden. Für den Einsatz auf dem Acker wurde außerdem der Einfluss von Korngröße und Feuchtigkeit auf das LIBS-Signal untersucht. Die unterschiedlichen Korngrößen haben nur einen geringen Einfluss auf das LIBS-Signal und das Kalibriermodell lässt sich durch entsprechende Proben leicht anpassen. Dagegen ist der Einfluss der Feuchtigkeit deutlich stärker und hängt stark von der Bodenart ab, sodass für jede Bodenart ein separates Kalibriermodell für verschiedene Feuchtigkeitsgehalte erstellt werden muss. Mithilfe der PCA kann der Feuchtigkeitsgehalt im Boden grob abgeschätzt werden und die entsprechende Kalibrierung ausgewählt werden. Diese Arbeit liefert essentielle Informationen für eine Echtzeit-Analyse von Nährelementen auf dem Acker mittels LIBS und leistet einen wichtigen Beitrag zu einer fortschrittlichen und zukunftsfähigen Nutzung von Ackerflächen. KW - Boden KW - Chemometrie KW - LIBS KW - Nährelemente KW - Düngeempfehlung KW - Precision Agriculture KW - Prozessanalytik PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:517-opus4-476772 DO - https://doi.org/https://doi.org/10.25932/publishup-47677 SP - 1 EP - 130 PB - Universität Potsdam CY - Potsdam AN - OPUS4-52183 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meyer, Klas T1 - Flexible Prozessanalytik für die pharmazeutische Produktion - Benchtop-NMR-Spektroskopie im industriellen Einsatz N2 - Im Rahmen des EU-Projekts „CONSENS – Integrated Control and Sensing“ wurde ein vollautomatisiertes, gemäß Atmosphère-Explosibles(ATEX)-Regeln zertifiziertes Analysatormodul auf Basis eines kommerziellen Benchtop-Kernspinresonanzspektrometers (Engl. nuclear magnetic resonance, NMR) entwickelt und im Umfeld einer modularen containerbasierten Produktionsanlage validiert. Auf Basis der gewonnenen Daten konnten sowohl eine iterative Optimierung der Prozessparameter erfolgen als auch Referenzdaten für die Kalibrierung eines Nahinfrarot-Spektrometers gewonnen werden. KW - Prozessanalytik KW - NMR-Spektroskopie KW - Modulare Produktion KW - Kalibriertransfer PY - 2022 VL - 12 IS - 3 SP - 122 EP - 129 PB - Editio Cantor Verlag CY - Aulendorf AN - OPUS4-55402 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Integrated and Networked Systems and Processes - How NMR Spectroscopy Can Transform our Chemical and Pharmaceutical Production N2 - Chemical and pharmaceutical companies need to find new ways to survive successfully in a changing environment, while finding more flexible ways of product and process development to bring their products to market faster - especially high-value, high-end products such as fine chemicals or pharmaceuticals. This is complicated by changes in value chains along a potential circular economy. One current approach is flexible and modular chemical production units that use multi-purpose equipment to produce various high-value products with short downtimes between campaigns and can shorten time-to-market for new products. Online NMR spectroscopy will play an important role for plant automation and quality control, as the method brings very high linearity, matrix independence and thus works almost calibration-free. Moreover, these properties ideally enable automated and machine-aided data analysis for the above-mentioned applications. Using examples, this presentation will outline a possible more holistic approach to digitalization and the use of machine-based processes in the production of specialty chemicals and pharmaceuticals through the introduction of integrated and networked systems and processes. T2 - 43rd FGMR Annual Discussion Meeting CY - Karlsruhe, Germany DA - 12.09.2022 KW - Digital Transformatioin KW - Process Industry KW - Pharmaceuticals KW - Specialty Chemicals KW - Automation KW - Online NMR Spectroscopy KW - Industry 4.0 PY - 2022 AN - OPUS4-55715 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Modular process control with compact NMR spectroscopy - From field integration to automated data analysis N2 - Chemical companies must find new paths to stay productive in a rapidly changing environment. One of these is the potential of digital technologies. Flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce time to market. Process safety is improved due to smaller amounts processed and the abilities of efficient heat-transfer allow for otherwise difficult-to-produce compounds. To exploit these advantages, a fully automated process control along with real-time quality control is mandatory and should be based on “chemical” information. The advances of a fully automated NMR analyzer were demonstrated, using a given pharmaceutical reaction step operated within a modular pilot plant. A commercially available benchtop NMR spectrometer was integrated to the requirements of an automated chemical production environment such as explosion safety, field communication, and robust data evaluation. Obtained results were used for direct loop advanced process control and real-time optimization of the process. NMR spectroscopy appeared as excellent online analytical tool and allowed a modular data analysis approach, which even served as reliable reference method for further PAT applications. Using the available datasets, a second data analysis approach based on artificial neural networks (ANN) was evaluated.Therefore, amount of data was augmented to be sufficient for training. The results show comparable performance, while improving the calculation time tremendously. In future, such fully integrated and interconnecting “smart” systems and processes can increase the efficiency of the production of specialty chemicals and pharmaceuticals. T2 - 5th European Conference on Process Analytics and Control Technology (EuroPACT) CY - Online meeting DA - 15.11.2021 KW - NMR spectroscopy KW - Benchtop-NMR KW - Modular production KW - Process Analytical Technology PY - 2021 AN - OPUS4-53776 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maiwald, Michael T1 - Next Generation Automation - Arbeitskreis 3.7: Smarte Sensorik, Aktorik und Kommunikation N2 - Der AK 3.7 ist ein "erweiterter" AK und je zur Hälfte mit NAMUR-Vertretern und Vertretern der Geräte- und Softwarehersteller besetzt. Er wurde ins Leben gerufen, um Begrifflichkeiten der digitalen Transformation aufzugreifen, wie etwa Smarte Sensorik, Sensordatenfusion, Schwarmsensorik oder Softsensorik. Eine erste Aufgabe bestand darin, einige exemplarische Anwendungsfälle der Nutzung smarter Eigenschaften von Feldgeräten sowie deren zukünftige Kommunikationsmöglichkeiten sowohl mit Bezug auf Bestandsanlagen als auch mit Blick auf einen potentiellen Technologiewechsel zu betrachten. Neuer Scope des AK 3.7 ist eine "Next Generation Automation" um einen potentiellen Technologiewechsel rechtzeitig vorauszudenken. Dieses erfolgt unter vollständiger gedanklicher Trennung von heutiger Automatisierung und auch vom NOA-Konzept. Ebenso wird ein Technologiewechsel in der Produktion der Prozessindustrie (wahrscheinlich modulbasiert) postuliert. Ziel des AK 3.7 wird es in Zukunft sein, diese Anforderungen an smarte Feldgeräte aufzugreifen und gemeinsam mit den thematisch überlappenden Interessenskreisen in Standards zu übersetzen. KW - Prozessindustrie KW - Automation KW - NAMUR KW - Sensorik KW - Aktorik KW - Kommunikation PY - 2021 SN - 2190-4111 SN - 2364-3137 IS - 9 SP - 73 PB - Vulkan Verlag CY - Essen AN - OPUS4-54336 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cairns, Warren R. L. A1 - Butler, Owen T. A1 - Cavoura, Olga A1 - Davidson, Christine M. A1 - Todolí-Torró, José-Luis A1 - von der Au, Marcus T1 - Atomic spectrometry update – a review of advances in environmental analysis N2 - Highlights in the field of air analysis included: a new focus on measuring micro- and nanoplastic particles in air, the development of hyphenated ICP-MS systems for in situ sampling and measurement of airborne metallic particles and the reported use of wearable black carbon sensors for measuring exposure to diesel fumes within the workplace. Significant advancements in the analysis of waters have been made in developing novel resin materials and new protocols for existing commercially available resins, aimed at the determination and speciation of trace levels of metals and metalloids in water matrices. These developments have been validated for sample purification and pre-concentration. In addition to traditional column chemistry, on-line hyphenated techniques were employed to enhance speciation analysis, with optimized methods enabling faster analysis and facilitating a more holistic approach by allowing the simultaneous detection of multiple species or elements in a single run. Efforts have also been directed towards detecting particles in the micro- and nanometer range, broadening the analytical scope beyond the ionic fraction. This year, the focus shifted from natural and engineered nanoparticles towards the critical field of plastic pollution, with several innovative methodologies introduced. Furthermore, to achieve better precision and lower detection limits in the field of MS/MS, numerous studies explored the behaviour of gases and reactions within reaction cells, contributing to the refinement of these techniques. In the analysis of soils and plants, methods aimed at improving the efficiency of green solvents were again prominent. Developments in AES were largely driven by the desire to create small, low-cost, low-power-consumption instrumentation suitable for field deployment. The study of NPs in soil and plant systems continued to be a focus for sp-ICP-MS. The past year has again seen a large volume of publications featuring LIBS, with particular interest in methods to enhance signal intensity and thereby improve limits of detection. Of interest in XRF was the development of in-house spectrometers for underwater mercury screening and in vivo plant analysis. Developments in geological analysis include new homogeneous natural and synthetic materials that have been developed as reference materials (RMs) in the analysis of geological samples by microanalytical techniques, such as LA-ICP-MS, LIBS and SIMS. Additional information on already existing RMs has been obtained for in situ isotope ratio determinations. Attention has been paid to sample preparation and purification methods able to shorten the analysis time and to improve the accuracy. Much attention has been paid to the use of LA-ICP-MS/MS as a means for removing spectral interferences in the case of in situ localized isotopic analysis and dating of geological materials. The development of new chemometric models as well as software has continued to improve data quality. The use of artificial intelligence is growing and techniques such as machine learning have led to significant improvements in the quality of geochemical results. KW - Review KW - Water KW - Environment PY - 2025 DO - https://doi.org/10.1039/D4JA90056A SN - 0267-9477 VL - 40 IS - 1 SP - 11 EP - 69 PB - Royal Society of Chemistry CY - London AN - OPUS4-62283 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - Potential of multivariate data analysis (MVA) in X-ray fluorescence analysis N2 - X-ray fluorescence spectrometry (XRF) is used, for example, in geochemistry, archaeology, materials science and agriculture to analyze the elemental composition of various samples [1]. Quantitative spectrum analysis typically applies methods such as fundamental parameters or intensity correction [1, 2]. However, there are also approaches to analyze XRF spectra using data-driven MVA approaches that are not based on a physical model. Principal component analysis (PCA) enables the visualization of data and the discovery of hidden relationships between analytical signals and sample parameters [1, 3]. Classification methods, e.g. PCA, cluster or discriminant analysis, can help to distinguish samples based on various complex integral features such as authenticity or origin of the sample [3]. MVA can also be used to correlate various external factors with elemental composition. In addition to classifying mineral wool into different material types based on characteristic oxides, PCA also enables the visualization of problem cases and supports the detection of possible outliers [4]. Multivariate regression methods such as partial least squares regression (PLSR) are a powerful tool for the quantitative analysis of spectra. In contrast to univariate analysis, in which only one characteristic is used as the basis for the regression, entire spectra or spectral ranges are analyzed here. It has been shown that the quantitative determination of C, H, N and O in polymers based on WDXRF spectra can be achieved by PLSR [5]. However, in the presence of complex matrix effects, the limitations of PLSR become clear, as was shown in a reference case (EDXRF spectra of steel and ore samples) [2]. Here, PLSR still outperformed the fundamental parameter approach, but proved to be less accurate than an intensity correction approach. Neural networks, which are better able to deal with nonlinear effects, are only an alternative if both a large number of calibration samples are available for adequate network training and a lot of time is available for network optimization. Despite limitations, it can be summarized that MVA, if used correctly, can contribute to increasing the informative value of XRF and to opening up new fields of application in areas of growing economic importance [1-5]. T2 - 12. PRORA Fachtagung Prozessnahe Röntgenanalytik CY - Berlin, Germany DA - 28.11.2024 KW - Chemometrics KW - Mineral wool KW - Data analysis KW - X-ray fluorescence PY - 2024 AN - OPUS4-62032 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Deconvolution in High-Field- and Benchtop-NMR applications N2 - Numerical "sum integration" is the typical way to extract signal area from NMR spectra for quantitative evaluation, however, in complex situations of peak overlaps or crowded spectra this can be impractical. Deconvolution methods based on linefitting and optimization allow for a more accurate extraction of signal features from the spectrum in these cases. The increasing number of benchtop NMR applications showing lower signal dispersion and therefore more often complex spectral patterns foster the development and application of model-based spectra evaluation methods. This includes techniques like Indirect Hard Modeling (IHM), Quantum-Mechanical Spectra Analysis (QMSA), Chemometric modeling like PLS-R or MCR, as well as Machine-learning approaches using Neural Networks. This presentation gives an overview and introduction into deconvolution methods in the context of high-field and benchtop-NMR applications in complex spectra and process monitoring. T2 - CCQM OAWG/PAWG Advances in qNMR Workshop CY - Sèvres, France DA - 08.04.2025 KW - NMR Spectroscopy KW - Process Analytical Technology KW - Deconvolution KW - Benchtop-NMR PY - 2025 AN - OPUS4-62956 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Process Monitoring with Compact NMR spectroscopy: Applications from Lab to Field N2 - The use of compact NMR instruments based on permanent magnets has been increasing in recent years. Their affordability, portability, and ease of operation without the need for trained staff make them particularly interesting for quality control application in industrial production. Recent developments by instrument manufacturers, such as multi-nuclei options or extended interfacing, have made these systems even more versatile. However, the application of NMR spectroscopy as an online PAT tool remains rare, despite its significant potential for process optimization and control. A key challenge in exploiting this potential is the integration of lab instruments into the harsh environment of a chemical plant. Additionally, advancements in automation and data evaluation are key tasks to ensure robust, unattended operation with minimal maintenance requirements. In this presentation, we showcase examples of using NMR spectroscopy for process monitoring at the lab scale, the development of open-source software tools for NMR data evaluation (PyIHM, within the Python package KLASSEZ), and a successful example of field integration, running an automated laboratory instrument in the environment of a industrial production plant. T2 - Quantitative NMR Methods for Reaction and Process Monitoring (NMRPM) CY - Kaiserslautern, Germany DA - 31.03.2025 KW - Compact NMR spectroscopy KW - Process Monitoring KW - Downstream processing KW - Indirect Hard Modeling KW - Field integration PY - 2025 AN - OPUS4-62850 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - Kombinierte Bestimmung von Wasserstoff in Gasgemischen mittels Raman- und NMR-Spektroskopie N2 - Vorgestellt wird die Nutzung von Online tauglichen Raman- und NMR-Spektrometern zur Quantifizierung des Wasserstoffmolanteils in gravimetrisch hergestellten Primärgasstandards unter Labor-Bedingungen. Es zeigte sich, dass Matrixeffekte insbesondere bei der Raman-Spektroskopie vernachlässigbar sind für die Quantifizierung von H2. Aufgrund der leichten Handhabbarkeit und der geringen Messunsicherheiten ergibt sich eine potenzielle Anwendung von Raman- und NMR-Spektroskopie unter Feldbedingungen als Online-Messeinheit im Bereich 5-100 cmol/mol Wasserstoff. T2 - 19. PAT Erfahrungsaustauschtreffen CY - Basel, Switzerland DA - 17.09.2024 KW - Raman KW - NMR KW - Wasserstoff PY - 2024 AN - OPUS4-62035 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lozano-Martín, D. A1 - Tuma, Dirk A1 - Kipphardt, Heinrich A1 - Khanipour, Peyman A1 - Chamorro, C. R. T1 - Thermodynamic characterization of the (H2 + C3H8) system significant for the hydrogen economy: Experimental (p, rho, T) determination and equation-of-state modelling N2 - For the gradual introduction of hydrogen in the energy market, the study of the properties of mixtures of hydrogen with typical components of natural gas (NG) and liquefied petroleum gas (LPG) is of great importance. This work aims to provide accurate experimental (p, rho, T) data for three hydrogen-propane mixtures with nominal compositions (amount of substance, mol/mol) of (0.95 H2 + 0.05 C3H8), (0.90 H2 + 0.10 C3H8), and (0.83 H2 + 0.17 C3H8), at temperatures of 250, 275, 300, 325, 350, and 375 K, and pressures up to 20 MPa. A single-sinker densimeter was used to determine the density of the mixtures. Experimental density data were compared to the densities calculated from two reference equations of state: the GERG-2008 and the AGA8-DC92. Relative deviations from the GERG-2008 EoS are systematically larger than those from the AGA8-DC92. They are within the ±0.5% band for the mixture with 5% of propane, but deviations are higher than 0.5% for the mixtures with 10% and 17% of propane, especially at low temperatures and high pressures. Finally, the sets of new experimental data have been processed by the application of two different statistical equations of state: the virial equation of state, through the second and third virial coefficients, B(T, x) and C(T, x), and the PC-SAFT equation of state. KW - Hydrogen-containing gas mixture KW - Density data KW - Equation of state KW - Virial coefficients PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570056 DO - https://doi.org/10.1016/j.ijhydene.2022.11.170 SN - 0360-3199 VL - 48 IS - 23 SP - 8645 EP - 8667 PB - Elsevier B. V. CY - Amsterdam AN - OPUS4-57005 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -