TY - CONF A1 - Wilke, Olaf A1 - Poelke, Birte A1 - Klein, Luise A1 - Rohloff, Alexander A1 - Hoffmann, Holger T1 - Initial VOC Emissions from Consumer Products Determined in Micro-Scale Test Chambers: Results of a Round Robin Test N2 - Emissions of volatile organic compounds (VOCs) from consumer products may have a negative impact on indoor air quality, potentially also affecting human wellbeing. Since consumers may be exposed to these VOCs immediately after e.g. unwrapping of newly purchased products, reliable analytical methods are needed to determine air concentration profiles in the early phase of VOC emissions. Concerning typical sample sizes of consumer products, micro-scale test chambers (μ-chambers) were considered suitable for this purpose. In addition, compared to medium- or large-scale test chambers, μ-chambers require lower initial investment and operational costs, and offer options for emissions screenings where higher sample throughput is essential. For these reasons, a μ-chamber-based method to determine initial concentrations of VOCs emitting within the first hours of simulated product use was developed. The chamber air was frequently sampled on desorption tubes loaded with Tenax® TA, followed by quantification of emitted VOCs via thermal desorption gas chromatography mass spectrometry (TD-GC-MS). The method was assessed in a round robin test involving eight participating laboratories from 2 countries. Pieces of a rain poncho (sample area A: 2.01·10-4 m2) emitting cyclohexanone, phenol, 2-ethylhexanol, naphthalene and isophorone in significant concentrations were distributed as sample material. Each laboratory conducted triplicate emission tests over a period of 48 h in μ-chambers with volumes of 44 or 114 mL. The loading factors L of 4.57 m2·m-3 (44 mL) or 1.76 m2·m-3 (114 mL) and air flow rates of 24 mL·min-1 resulted in area-specific air flow rates q of 7.17 m3·m-2·h-1 in both chamber types. The temperature was set to 23°C and, if possible, relative humidity was set to approx. 50%. The chamber air was sampled after 0.5, 1, 2, 4, 24 and 48 hours. In addition, to assess the analytical performance, each participating laboratory received two analyte-spiked Tenax® TA-loaded desorption tubes for quality control (QC). Very low relative standard deviations (11–17%) were obtained for the QC test. The results of the emissions tests in the early phase (0.5–4 h) were also adequate, with acceptable z scores (|z|≤2.00) received by six to seven participating laboratories. All eight laboratories obtained acceptable z scores after the longer sampling periods (24 and 48 h). Hence, the inter-laboratory comparability of the results obtained with the developed μ-chamber method was successfully confirmed. T2 - Healthy Buildings Europe 2025 CY - Reykjavik, Iceland DA - 08.06.2025 KW - VOC Emissions KW - Consumer Product KW - Test Chamber KW - Round Robin Test PY - 2025 AN - OPUS4-63706 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Khanipour, Peyman T1 - Real time mass spectrometry - From Unravelling Electrochemical Reaction Mechanism to Trace Analysis of Impurities in Hydrogen Gas N2 - Climate change and related energy policies, exacerbated by unforeseen geopolitical developments, pose new challenges for gas analytics, such as the use of hydrogen, hydrogen-containing alternative gaseous fuels (NH3, etc.), the use of alternative methane-based energy gases (LNG, LPG, etc.) or decarbonisation via CCSU. In all topics, the quality, i.e. the actual chemical composition of the gases, naturally plays a decisive role. BAM is meeting this strategic importance with the further development of hydrogen analytics and is continuing to develop the methods used in order to support the German economy and research landscape with traceability, reference materials and analytical procedures as quickly as possible. Mass spectrometry plays an important role for trace analysis in hydrogen matrix. The presentation shows first experimental results from the application of PTR-TOF-MS (Proton Transfer Reaction Time-of-Flight Mass Spectrometry). T2 - 11th International GAS Analysis Symosium & Exhibition CY - Paris, France DA - 17.05.2022 KW - Gas Analysis KW - Hydrogen KW - Metrology KW - Mass Spectrometry KW - Trace Analysis PY - 2022 AN - OPUS4-56589 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tuma, Dirk T1 - High-pressure density data of hydrogen-containing natural gases for the extension of equation-of-state models N2 - This presentation reports new density data of hydrogen-containing natural gas mixtures between 250 and 350 K and up to pressures of 20 MPa. T2 - 11th International GAS Analysis Symposium & Exhibition CY - Paris, France DA - 17.05.2022 KW - Hydrogen-containing natural gas KW - Density data KW - Equation of state PY - 2022 AN - OPUS4-56433 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Messverfahren für Wasserstoff: Qualität durch Zertifizierung – Standortvorteile in Deutschland N2 - Die Veranstaltungsreihe "Neue Märkte erschließen – mit Normen und Standards hoch hinaus", die vom DIN gemeinsam mit der NOW GmbH organisiert wird, richtets sich vorwiegend an KMUs. Fokus der Veranstaltung sind Messverfahren für Wasserstoff. Der Beitrag der BAM führt sehr kurz die Rolle nationaler und internationaler Normung sowie weltweiter Metrologie im Rahmen der Meterkonvention bezüglich analytischer Qualitätssicherung und Zertifizierung von Gasen und Referenzmaterialien ein. Es werden aktuelle Beispiele für die Qualitätssicherung von Wasserstoff, mögliche dazu notwendige Ausrüstung und weiterführende Literaturquellen vorgestellt. T2 - Neue Märkte erschließen – mit Normen und Standards hoch hinaus CY - Online meeting DA - 18.03.2021 KW - Wasserstoff KW - Normung KW - Standortvorteil KW - Analytik KW - Wasserstoffanalytik KW - Wasserstoff Referenzmaterial KW - Gasanalytik PY - 2021 AN - OPUS4-52296 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Soruco Aloisio, Ricardo A1 - Klaus, Christian T1 - Auf dem Weg zu einer digitalen Qualitätsinfrastruktur - Use Case Wasserstofftankstelle 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. T2 - Hannover Messe 2024 - Speakers Corners CY - Hannover, Germany DA - 23.04.2024 KW - IT KW - OT KW - Infrastruktur KW - Datenintregration KW - VPN KW - Verwaltungsschale KW - Open Source KW - Software PY - 2024 AN - OPUS4-59930 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Grimmer, Christoph T1 - Development, application and measurement uncertainty of emission reference materials N2 - Volatile organic compounds (VOCs) emitted by furniture and building materials can cause health issues. For an improvement of indoor air quality low emitting materials should be used. Quality assurance and –control (QA/QC) measures require an emission reference material (ERM) with a predictable emission rate of VOCs. The idea is to use porous materials as ERM, which store the VOCs inside their pores and emit them constantly. T2 - Webinar Metrology for Indoor Air Quality Reference materials for QA/QC of the emission test chamber procedure CY - Online meeting DA - 11.04.2024 KW - Emission reference materials KW - Indoor air quality KW - Materials emissions test KW - VOC PY - 2024 AN - OPUS4-59963 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Matthias T1 - Metrological sound reference products for quality assurance and quality control measures in material emissions testing N2 - In industrialised countries more than 80% of the time is spent indoors. Products, such as building materials and furniture, emit volatile organic compounds (VOCs), which are therefore ubiquitous in indoor air. Different VOC combinations may, under certain environmental and occupational conditions, result in reported sensory irritation and health complaints. A healthy indoor environment can be achieved by controlling the sources and by eliminating or limiting the release of harmful substances into the air. One way is to use materials proven to be low emitting. Meanwhile, a worldwide network of professional commercial and non-commercial laboratories performing emission tests for the evaluation of products for interior use has been established. Therefore, comparability and metrological traceability of test results must be ensured. A laboratory’s proficiency can be proven by internal and external validation measures that both include the application of suitable reference materials. The emission test chamber procedure according to EN 16516 comprises several steps from sample preparation to sampling of test chamber air and chromatographic analysis. Quality assurance and quality control (QA/QC) must therefore be ensured. Currently, there is a lack of suitable reference products containing components relevant for the health-related evaluation of building products. The EU-funded EMPIR project 20NRM04 MetrIAQ (Metrology for the determination of emissions of dangerous substances from building materials into indoor air) aims to develop 1) gaseous primary reference materials (gPRM), which are used for the certification of gaseous (certified) reference materials (gCRM) and 2) emission reference materials (ERM). Most commercial gas standards of indoor-relevant compounds are not certified due to the lack of primary reference materials to which the project aims to contribute. The gPRM under development is a gas-phase standard containing trace levels of VOCs in nitrogen or air from the check standard according to EN 16516 (n-hexane, methyl isobutyl ketone, toluene, butyl acetate, cyclohexanone, o-xylene, phenol, 1,3,5-trimethylbenzene) with a target uncertainty of 5 %. The gPRM can be sampled into sorbent tubes to obtain transfer standards in the form of gCRM. The well characterised ERM represents a sample of a test specimen, e.g. building material, that is loaded into the emission test chamber for a period of several days and is used to evaluate the whole emission test chamber procedure. It shall have a reproducible and temporally constant compound release of less than 10 % variability over 14 days. Different approaches for retarded VOC release, such as the encapsulation of pure compounds and the impregnation of porous materials, are being tested to reach this aim. Furthermore, the design of the ERM is accompanied by the development of a numerical model for the prediction of the emissions for each of the target VOCs. The current progress of the work on both materials will be presented. T2 - CIM 2023 - 21st International Metrology Congress CY - Lyon, France DA - 07.03.2023 KW - Indoor air quality KW - VOC KW - Materials emissions testing KW - Emission reference material KW - Quality assurance/quality control PY - 2023 AN - OPUS4-57142 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Grimmer, Christoph T1 - Preparation of novel emission reference materials: μ-capsules & impregnated porous materials N2 - Volatile organic compounds (VOCs) emitted by furniture and building materials can cause health issues. For an improvement of indoor air quality low emitting materials should be used. Quality assurance and –control (QA/QC) measures require an emission reference material (ERM) with a predictable emission rate of VOCs. The idea is to use porous materials as ERM, which store the VOCs inside their pores and emit them constantly. T2 - WORKSHOP: METROLOGY FOR INDOOR AIR QUALITY CY - Mol, Belgium DA - 18.10.2023 KW - Emission reference materials KW - Indoor air quality KW - Materials emissions test KW - VOC PY - 2023 AN - OPUS4-59961 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Matthias T1 - Emission reference materials for indoor air measurements N2 - In industrialised countries more than 80% of the time is spent indoors. Products, such as building materials and furniture, emit volatile organic compounds (VOCs), which are therefore ubiquitous in indoor air. VOC in combination may, under certain environmental and occupational conditions, result in reported sensory irritation and health complaints. Emission concentrations can become further elevated in new or refurbished buildings where the rate of air exchange with fresh ambient air may be limited due to improved energy saving aspects. A healthy indoor environment can be achieved by controlling the sources and by eliminating or limiting the release of harmful substances into the air. One way is to use (building) materials proved to be low emitting. Meanwhile, a worldwide network of professional commercial and non-commercial laboratories performing emission tests for the evaluation of products for interior use has been established. Therefore, comparability of test results must be ensured. A laboratory’s proficiency can be proven by internal and external validation measures that both include the application of suitable emission reference materials (ERM). For the emission test chamber procedure according to EN 16516, no artificial ERM is commercially available. The EU-funded EMPIR project MetrIAQ aims to fill this gap by developing new and improved ERMs. The goal is to obtain a material with a reproducible and temporally constant compound release (less than 10 % variability over 14 days). Two approaches were tested: the impregnation of porous materials with VOC, and the encapsulation of VOC in polymer microcapsules. Impregnation is performed with help of an autoclave and supercritical CO2. The encapsulation is done by interfacial polymerisation on VOC droplets. For both approaches, synthesis and/or material parameters were varied to obtain an optimal ERM. Findings about the optimisation of ERM generation, as well as performance of the best emission reference materials, will be presented. T2 - GAS Analysis 2024 CY - Paris, France DA - 30.01.2024 KW - Emission reference materials KW - Materials emissions test KW - VOC KW - Indoor air quality PY - 2024 AN - OPUS4-59506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Klaus, Christian T1 - Verwaltungsschale Industrie 4.0 N2 - Die Veranstaltung richtet sich an alle Mitarbeiter der BAM. Ziel ist es, allen eine Idee zu vermitteln, was die Verwaltungsschale ist und wie sie angewendet werden kann. Die Zuhörer sollen hinterher eine Idee haben, ob bei ihrer eigenen Arbeit potenzielle Anknüpfungspunkte bestehen. Inhalt: • Beispiel aus QI Digital als Motivation (Problemstellung) • Beschreibung der VWS als Lösungsansatz für einheitliche Datenstrukturierung (mit verschiedenen Nutzern) • Fokus liegt nicht auf Neuentwicklung, sondern auf der Nutzung vorgeschlagener Werkzeuge und Standards der Industrie 4.0 • Struktur der Verwaltungsschale T2 - BAM Kolloquium CY - Berlin, Germany DA - 29.05.2024 KW - Verwaltungsschale KW - Digitaler Zwilling KW - Interoperabilität PY - 2024 AN - OPUS4-63498 LA - deu 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 in (Bio) Process Engineering N2 - The competitiveness of the process industry is based on ensuring the required product quality while making optimum use of equipment, raw materials and energy. Chemical 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. One way is knowledge-based production, taking into account all essential equipment, process and regulatory data of plants and laboratories. Today, the potential of this data is often not yet consistently used for a comprehensive understanding of production. Another approach uses flexible and modular chemical plants, 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. Digital transformation is enabling completely new production concepts that are being used increasingly. Intensified continuous production plants also allow for difficult to produce compounds. This contribution aims to encourage a more holistic approach to the digitalization and use of machine-assisted methods in (bio) process engineering by introduction of integrated and networked systems and processes, which have the potential to speed up the high-quality production of specialty chemicals and pharmaceuticals. T2 - 6th BioProScale Symposium - industrial scale bioprocess intensification from process development to large-scale understanding CY - Online meeting DA - 29.03.2021 KW - Industry 4.0 KW - Biotechnology KW - Bio engineering KW - Process Analytical Technology KW - BioProScale KW - Artificial Neural Networks PY - 2021 UR - https://biotechnologie.ifgb.de/node/648 AN - OPUS4-52371 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Fully integrated and intelligently networked systems and processes - Perspective: Smart sensors, actuators and communication N2 - Companies in the chemical industry have to tread new paths in order to survive successfully in a changed environment. This includes, in particular, the potential of digital technologies. The full integration and intelligent networking of systems and processes is making slow progress. This talk is a tribute to the field level. It wants to encourage a more holistic approach to the digitalisation of the process industry based on smart sensors, actuators and communication and provides information on current technical perspectives, such as the "one-network paradigm", ad-hoc networking, edge computing, FPGAs, virtual machines or blockchain. These give smart sensors, actuators and communication a completely new perspective. T2 - 5th European Conference on Process Analytics and Control Technology - EuroPACT 2021 CY - Online meeting DA - 15.11.2021 KW - Process Analytical Technology KW - Smart Sensors KW - Digital transformation KW - Industry 4.0 KW - EuroPact KW - Distributed Networks PY - 2021 UR - https://dechema.de/europact2021.html AN - OPUS4-53754 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - Raman spectroscopy for online monitoring of a homogeneous hydroformylation process in microemulsion N2 - An important industrial reaction is hydro¬formylation for the production of aldehydes from alkenes and syngas on the basis of homogeneous catalysis. The main cost factors of the processes currently used are product selectivity and the loss of the catalysts used. Therefore, various concepts for the hydroformylation of long-chain olefins have been developed, including hydroformylation in microemulsions, which is being investigated on a mini-plant scale at the Technical University of Berlin [1]. In this study, online Raman spectroscopy of the reaction of 1-dodecene to 1-tri¬decanal in a microemulsion was performed [2]. First, an experimental design was used to obtain a good representation of the operating range in the mini plant with respect to the concentrations of five reactants in a laboratory setup [3]. Based on the Raman spectra, Partial Least Squares (PLS) models for the prediction of 1-dodecene and 1-tride-decanal were calibrated and with these the reactions were predicted on a laboratory scale. In the next step, the PLS models were applied to online spectra from a mini-plant. This resulted in promising estimates of 1-tridecanal and acceptable predictions of 1-dodecene mass fractions. The predictive power of PLS models in this particular case was limited by unexpected by-product formation which, however, can easily be compensated by an extended calibration. Hence, Raman spectroscopy is a promising technique for process analysis in microemulsions. T2 - EuroPACT2021 CY - Online meeting DA - 15.11.2021 KW - Raman KW - Process analytics KW - Inline measurement PY - 2021 AN - OPUS4-53767 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Klinge, A. T1 - upMIN 100 – upcycling of mineral construction and demolition waste to substitute natural aggregates in earthen building materials N2 - The construction sector is one of the most resource-intensive sectors in Germany and is responsible for 40 % of CO2 emissions. emissions. Around 517 million tons of mineral raw materials are required annually for the construction of buildings in Germany. At the same time, mineral construction waste was the largest material flow at 229.3 million tons (2020). The rates of building material recycling have increased since 2000, especially for mineral waste. Nevertheless, the majority of recycled aggregates are used in technically largely unregulated applications (e.g. road construction). This downcycling leads to a loss of valuable resources for technically and economically valuable uses. The upMIN100 research project is investigating the question of whether and to what extent recycled mineral construction and demolition waste is suitable as an additive in earthen building materials such as earth plasters and earth blocks. The focus is placed on grain sizes < 2 mm, which are currently predominantly landfilled, as there are currently no regulations for their use in building products. In order to enable the use of construction and demolition waste, the technical feasibility must be ensured, quality requirements for source materials (e.g. limit values for pollutants in terms of health and environmental environmental compatibility and hazardous substances) and permissible proportions of recycled aggregates must be defined. To avoid negative impact on building occupants, the developed building materials have been tested in terms of harmful substances included in the mineral waste as well as emissions into the ambient air. Furthermore, the earthen building products, manufactured from mineral waste, should be free from pollutants to enable a return into the environment. According to the Substitute Building Materials Ordinance (EBV) this corresponds to criterion BM-0. Two different building material developments were used to test the technical feasibility and the pollutant content of the recycled aggregate. T2 - Sustainable Built Environment Conference 2025 CY - Zurich, Switzerland DA - 25.06.2025 KW - Mineral waste KW - Upcycling KW - Earthen building product KW - Circular construction PY - 2025 AN - OPUS4-63552 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kipphardt, Heinrich T1 - Introduction to Metrology in Chemistry N2 - Measurements are an important fundament of natural science in general and of chemical analysis in particular. Metrology is the science (and art) of performing measurements. The basic concepts and terms of metrology and their practical implementation are introduced. The very special peculiarities of chemical measurements that are absent in physical measurements are discussed. T2 - 7th PhD Seminar of the German Working Group for Analytical Spectroscopy (DAAS) in the GDCh Division of Analytical Chemistry CY - Berlin, Germany DA - 15.11.2023 KW - Metrology KW - Chemical Analysis PY - 2023 AN - OPUS4-58868 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Online-NMR Spektroskopie in der PAT - Entwicklungen zwischen Labor- und Feldeinsatz N2 - Die NMR-Spektroskopie ist eine der zentralen nicht-invasiven Analysenmethoden in der organischen Chemie und aus dem Laboralltag nicht mehr wegzudenken. Die direkte Proportionalität zwischen der Anzahl der Atomkerne im Messvolumen und der Signalfläche im Spektrum ist vergleichbar mit einem „Zählen der Kernspins“. Der Kalibrieraufwand für die Quantifizierung ist minimal und aus dem NMR-Spektrum sind Informationen zu Struktur und Identität zugänglich. Online-NMR-Spektroskopie wird unter Zuhilfenahme von speziellen Durchflussproben-köpfen und Messzellen bereits seit Jahrzehnten erforscht und eingesetzt. Durch die hohen Anforderungen an die Aufstellung und den Betrieb von klassischen Hochfeld-NMR-Spektrometern konnte sie allerdings nie den Sprung vom Labor in den Prozess schaffen. Dies hat sich durch die Entwicklungen im Bereich mobil einsetzbarer Benchtop-NMR-Spektrometer grundlegend verändert. Geringere Investitions- und Betriebskosten, sowie die Robustheit und einfache Bedienbarkeit dieser Systeme sind entscheidende Faktoren. Damit rückt eine Anwendung als Online-PAT-Methode technisch in greifbare Nähe. Designierte Prozess-NMR-Spektrometer sucht man heutzutage allerdings auf dem Markt meist noch vergebens. Die Reaktionsverfolgung im Labormaßstab konnte an unterschiedlichen Systemen erfolgreich demonstriert werden. Dabei zeigten sich allerdings Limitierungen in Hinblick auf einen möglichen Prozesseinsatz. Insbesondere die Temperaturempfindlichkeit der Magnetsysteme ist hier zu nennen. Anhand eines Prototyps wurde eine aktive Temperaturisolation mittels temperierter Luftströmungen entwickelt und erprobt. Eine Feldintegration von Laborsystemen geht sowohl technisch als auch regulatorisch mit zahlreichen Herausforderungen einher. Das raue Umfeld von Produktionsanlagen, sowie die Anforderungen an Explosionsschutz erfordern eine zugelassene Einhausung. Auf Basis von Erfahrungen mit einem ersten Prototyp erfolgte die gemeinsame Entwicklung eines möglichst flexibel einsetzbaren Analysenschranks. Neben der Hardware-Integration sind die automatisierte modellbasierte Auswertung der NMR-Spektren, sowie die Einbindung in die Prozessleittechnik essenziell für einen zuverlässigen Betrieb als PAT-Analysengerät. T2 - 18. Kolloquium AK Prozessanalytik CY - Krefeld, Germany DA - 27.11.2023 KW - Prozessanalytik KW - Online-NMR-Spektroskopie KW - NMR-Spektroskopie KW - Benchtop-NMR KW - Feldintegration PY - 2023 AN - OPUS4-58969 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fricke, F. A1 - Meyer, Klas T1 - Artificial Intelligence for Mass Spectrometry and Nuclear Magnetic Resonance Spectroscopy N2 - Mass Spectrometry (MS) and Nuclear Magnetic Resonance Spectroscopy (NMR) are critical components of every industrial chemical process as they provide information on the concentrations of individual compounds and by-products. These processes are carried out manually and by a specialist, which takes a substantial amount of time and prevents their utilization for real-time closed-loop process control. This paper presents recent advances from two projects that use Artificial Neural Networks (ANNs) to address the challenges of automation and performance-efficient realizations of MS and NMR. In the first part, a complete toolchain has been developed to develop simulated spectra and train ANNs to identify compounds in MS. In the second part, a limited number of experimental NMR spectra have been augmented by simulated spectra to train an ANN with better prediction performance and speed than state-of-theart analysis. These results suggest that, in the context of the digital transformation of the process industry, we are now on the threshold of a possible strongly simplified use of MS and MRS and the accompanying data evaluation by machine-supported procedures, and can utilize both methods much wider for reaction and process monitoring or quality control. T2 - 2021 Design, Automation & Test in Europe Conference & Exhibition (DATE) CY - Online meeting DA - 01.02.2021 KW - Industry 4.0 KW - Cyber-Physical Systems KW - Artificial Neural Networks KW - Mass Spectrometry KW - Nuclear Magnetic Resonance Spectroscopy PY - 2021 UR - www.date-conference.com AN - OPUS4-52181 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Industrielle Anwendungen der Niederfeld-NMR-Spektroskopie für die Qualitätskontrolle von Silanen N2 - Aus der Kombination verschiedener Silane als Ausgangsstoffe und als Produkt der Hydrolyse durch eine Reihe von Alkoholen oder Wasser ergibt sich eine Palette von hunderten technischen Produkten für verschiedenste Anwendungen. Funktionelle Trialkoxysilane haben sich in den vergangenen Jahren als vielseitig einsetzbare Organosilane erwiesen. Die Einsatzgebiete erstrecken sich vom Witterungsschutz von Bauwerken über haftvermittelnde Eigenschaften in der Glasfaserindustrie, bei Dicht- und Klebstoffen, in Farben und Lacken bis hin zur Modifizierung von polymeren Werkstoffen. Kommerzielle Benchtop-NMR-Spektrometer haben das Potential auch im Bereich der Silanchemie als Online-Methode zur Reaktionsüberwachung und für die Qualitätskontrolle eingesetzt zu werden. Interessante NMR-Kerne für die oben genanntem Produkte sind 1H und 29Si. In einer gemeinsamen Forschungskooperation zwischen EVONIK und BAM wurde anhand verschiedener Fallstudien die Anwendbarkeit der Niederfeld-NMR-Spektroskopie zur chemischen Analyse von Silanen evaluiert. Die Möglichkeiten der Konzentrationsbestimmung erweitern die Anwendungsgebiete, in denen bestehende Technologien wie z. B. NIR, Raman, UV/VIS, etc. mangels Referenzdaten nicht quantitativ eingesetzt werden können. Eine Fallstudie setzte dazu an, den Hydrolyse- und Kondensationsverlauf mit geeigneter Online-NMR-Analytik zu beobachten, den Reaktionsfortschritt der Hydrolyse und Kondensation auf dieser Basis besser zu verstehen und zu optimieren. Zu diesem Zweck werden durch Zugabe von Wasser zunächst die Alkoxysubstituenten eines Trialkoxysilans hydrolysiert und entsprechende Silanole gebildet. Diese können dann über eine SiOH-Funktion an den zu modifizierenden Werkstoff anbinden und über weitere Silanolgruppen unter Ausbildung von Siloxaneinheiten vernetzen. In einer weiteren Fallstudie wurde die Kinetik der Aufspaltungen einer cyclischen Silanverbindung untersucht. Die Online-NMR-Analytik kam hierbei sowohl im Labor als auch in der industriellen Produktionsanlage zum Einsatz. Hierfür wurde eine automatisierte Einhausung verwendet, welche den Einsatz eines kommerziellen NMR-Spektrometers in explosionsgeschützten Bereichen ermöglicht. T2 - Praktische Probleme der Kernresonanzspektroskopie CY - Online meeting DA - 16.03.2021 KW - NMR-Spektroskopie KW - Benchtop-NMR KW - Silane KW - Prozessanalytik PY - 2021 AN - OPUS4-52298 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Industrial Applications of benchtop NMR Spectroscopy for Quality Control of Silanes N2 - The combination of different silanes as starting materials and as a product of hydrolysis by several alcohols or water creates a range of hundreds of technical products for a wide range of applications. In recent years, functional trialkoxysilanes have proven to be multi-purpose organosilanes. Applications range from weather protection of buildings to additives for glass fiber industry, sealants, adhesives, coatings and paints to the modification of polymers. Commercial benchtop NMR spectrometers have the potential to be used in silane chemistry as an online method for reaction monitoring and quality control. NMR nuclei of interest for silane products are 1H and 29Si. In a joint research cooperation between EVONIK and BAM, the applicability of low-field NMR spectroscopy for the chemical analysis of silanes was evaluated. It was shown how it can extend the application range where existing technologies like NIR, Raman, UV/VIS, etc. cannot be used quantitatively due to a lack of reference data. In a first case study the process of hydrolysis and condensation was observed using online NMR analysis. For this purpose, the substituents of a trialkoxysilane are first hydrolyzed by adding water and corresponding silanols are formed, which can then bind to materials via SiOH functions and crosslink to form siloxane units. Another case study was dealing with the kinetics of the cleavage of a cyclic silane compound. Online NMR analysis was used both in the laboratory and in the manufacturing plant. For this purpose, a fully automated containment system was used, which enables the use of a commercial NMR spectrometer in ATEX-environments. In the third case study presented, quantitative 1H-NMR spectra were acquired on product mixtures of a trialkoxysilane and other components such as organic stabilizers, organotin compounds, an aromatic amine and organic peroxides. An automatic evaluation method based on Indirect Hard Modeling (IHM) was developed. T2 - Magritek's Spinsolve NMR Users Meeting 2021 CY - Online meeting DA - 20.04.2021 KW - NMR spectroscopy KW - Silanes KW - Process Analytical Technology KW - Quality Control PY - 2021 AN - OPUS4-52557 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 - 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 - 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 - CONF A1 - Tang, Chi-Long T1 - Minimizing the FFF-3D printer hardware bias on particle emission by adjustment of the set extruder temperature N2 - Fused filament fabrication (FFF) on desktop 3D printers is a material extrusion-based technique often used by educational institutions, small enterprises and private households. Polymeric filaments are melted and extruded through a heated nozzle to form a 3D object in layers. The extrusion temperature is therefore a key parameter for a successful print job, but also one of the main driving factors for the emission of harmful air pollutants, namely ultrafine particles and volatile organic gases, which are formed by thermal stress on the polymeric feedstock. The awareness of potential health risks has increased the number of emission studies in the past years. However, the multiplicity of study designs makes an objective comparison of emission data challenging because printer hardware factors such as the actual extruder temperature (TE) and also feedstockspecific emissions are not considered. We assume that across the market of commercial low- and mid-price FFF printers substantial deviations between actual and set extruder temperatures exist, which have a strong effect on the emissions and hence may bias the findings of exposure studies. In our last publication, we presented a standardized feedstock-specific emission test method and showed that for each investigated feedstock an increase in actual extruder temperature was accompanied by an increase in particle emissions (Tang and Seeger, 2022). Therefore, any systematic discrepancy between set and actual extruder temperature matters. In this study, we used a thermocouple and an infrared camera to measure the actual extruder temperatures at different heights. We found significant under- and overestimation of the actual extruder temperatures by the respective set temperatures in three commercial printers. This caused a broad variation of the measured total numbers of emitted particles (TP), even when the same feedstock was operated. For the determination of TP, we followed the DE-UZ 219 test guideline. In a second round we repeated the tests with all printers adjusted to exactly the same extruder temperatures, i.e., to TE=230°C for ABS and TE=210°C for PLA. All measurements were conducted in a 1 m³ emission test chamber. Particle emissions in the size range between 4 nm and 20 μm were detected. Printing on three different printer models without temperature adjustment resulted for each of the investigated feedstocks in a variation in TP of around two orders of magnitude. After temperature adjustment, this was substantially reduced to approx. one order of magnitude and hence minimizes the bias of printer hardware on the emissions. Our findings suggest that adjustment of the extruder temperature should be mandatory in emission testing standards. It also poses a more accurate benchmark and provides more reliable emission data for evaluation of indoor air quality or for health risk assessments. In addition, a proper temperature setting is in the interest of the user. Some commercial FFF printers may have a higher actual extruder temperature than displayed and unintended overheating may not only impair the print quality but may cause unnecessarily increased exposure to particle emissions. T2 - European Aerosol Conference 2023 CY - Málaga, Spain DA - 03.09.2023 KW - Ultrafine particles KW - Thermal imaging KW - 3D printing KW - Indoor air quality KW - Emission testing PY - 2023 AN - OPUS4-58258 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -