TY - CONF A1 - Maiwald, Michael T1 - Modular process control with compact NMR spectroscopy: From field integration to fully automated data analysis 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 - Benchtop NMR: From Academia to Industry CY - Online meeting DA - 28.09.2022 KW - Digital Transformatioin KW - Process Industry KW - Benchtop NMR Spectroscopy KW - Procee Analytical Technology KW - Modular Production KW - Specialty Chemicals KW - Industry 4.0 PY - 2022 UR - https://eventos.fct.unl.pt/benchtop_nmr_workshop2022/pages/welcome AN - OPUS4-55850 LA - eng 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 - ProcessNET Jahrestagung 2022 Aachen CY - Aachen, Germany DA - 12.09.2022 KW - Process analytical technology KW - NMR spectroscopy KW - Digitization KW - Additive manufacturing PY - 2022 AN - OPUS4-55975 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Benchtop NMR spectroscopy in chemical manufacturing: From hardware field integration to data modeling N2 - The use of benchtop-NMR instruments is constantly increasing during the recent years. Advantages of being affordable, portable and easy-to-operate without the need for trained staff make them especially interesting for industrial applications in quality control. However, applications of NMR spectroscopy as an online PAT tool are still very rare but offer a huge potential for process optimization and control. A key task to exploit this potential is hardware field integration of the lab-instruments in a rough environment of a chemical plant. Additionally, developments in automation and data evaluation are mandatory to ensure a robust unattended operation with low maintenance requirements. Here, we show an approach of a fully automated analyzer enclosure considering explosion safety, field communication, as well as environmental conditions in the field. Temperature sensitivity is still a limitation of benchtop-NMR instruments in flow applications. Recent developments of manufacturers allow for limited operation at static temperature levels, however, a dynamic system for continuous operation is still not available. Using a prototype system offering a larger bore, active temperature shielding studies with thermostated air were performed evaluating the performance. Automated data evaluation of NMR spectra using a modular indirect hard modeling (IHM) approach showed good results and flexibility. 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, offering new ways to simultaneously evaluating large numbers of different models. T2 - Quantitative NMR Methods for Reaction and Process Monitoring (NMRPM) CY - Kaiserslautern, Germany DA - 24.05.2023 KW - Field integration KW - Benchtop-NMR KW - Process Analytical Technology PY - 2023 AN - OPUS4-57560 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Sicherheit und Prozesskontrolle in der Wasserstoff-Wirtschaft: Anforderungen an Sensoren und Prozessanalytik N2 - Der Vortrag ist ein Impulsvortrag, der kurz in die Prozessketten der potentiellen Wasserstoffwirtschaft einführt. An vielen Stellen werden spezifische Sensoren benötigt, die die Prozess-Sicherheit und die Zuverlässigkeit von Qualitätsparametern gewährleisten. Es wird auch kurz auf die Forschungsföerderungslandschaft zu diesem Thema eingegangen. T2 - Sensorik für die Digitalisierung Chemische Produktionsanlagen – Wir bringen neue Projektideen auf dem Weg! CY - Frankfurt am Main, Germany DA - 13.06.2022 KW - Sensoren KW - Wasserstoff-Wirtschaft KW - Forschungslandschaft Wasserstoff KW - ProcessNet KW - Digitale Transformation PY - 2022 AN - OPUS4-55110 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 - Achema 2022 CY - Frankfurt a.M., Germany DA - 22.08.2022 KW - Process analytical technology KW - NMR spectroscopy KW - Digitization PY - 2022 AN - OPUS4-55974 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bernstein, Michael A1 - Diehl, Bernd W. K. A1 - Holzgrabe, Ulrike A1 - Maiwald, Michael A1 - Meyer, Klas A1 - Monakhova, Yulia A1 - Schönberger, Torsten T1 - qNMR - The handbook N2 - Quantitative NMR (qNMR) has been around for a long time, but also has great potential to solve future problems in any quantitative analysis. As a primary method, it differs fundamentally from chromatographic methods: it is better described as a quantum mechanical balance. Succesful implementation of qNMR requires certain attention to detail. "qNMR - the handbook" is intended to be a guide for analysts to help understand the fundamental principles of NMR and the significant points relating to its implementation for quantitation. Regulatory considerations of qNMR adoption are explained. NMR fundamentals are explained to provide understanding. Together with many useful examples, the book is a compelling addition to the laboratory's reference library, providing all the tools that any practitioner should know to successfully implement qNMR. The authors are qNMR pioneers and come from a variety of backgrounds including business, government and academia. KW - Quantitative NMR spectroscopy KW - NMR spectroscopy KW - Handbook KW - qNMR PY - 2023 SN - 978-3-7568-7891-8 SN - 978-3-7583-8050-1 SP - 1 EP - 302 PB - BoD – Books on Demand CY - Norderstedt AN - OPUS4-59839 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lozano-Martín, D. A1 - Martín, M. C. A1 - Chamorro, C. R. A1 - Tuma, Dirk A1 - Segovia, J. J. T1 - Speed of sound for three binary (CH4 + H2) mixtures from p = (0.5 up to 20) MPa at T = (273.16 to 375) K N2 - Speed of sound is one of the thermodynamic properties that can be measured with least uncertainty and is of great interest in developing equations of state. Moreover, accurate models are needed by the H2 industry to design the transport and storage stages of hydrogen blends in the natural gas network. This research aims to provide accurate data for (CH4 + H2) mixtures of nominal (5, 10, and 50) mol-% of hydrogen, in the p = (0.5 up to 20) MPa pressure range and with temperatures T = (273.16, 300, 325, 350, and 375) K. Using an acoustic spherical resonator, speed of sound was determined with an overall relative expanded (k = 2) uncertainty of 220 parts in 10^6 (0.022%). Data were compared to reference equations of state for natural gas-like mixtures, such as AGA8-DC92 and GERG-2008. Average absolute deviations below 0.095% and percentage deviations between 0.029% and up to 0.30%, respectively, were obtained. Additionally, results were fitted to the acoustic virial equation of state and adiabatic coefficients, molar isochoric heat capacities and molar isobaric heat capacities as perfect-gas, together with second and third acoustic virial coefficients were estimated. Density second virial coefficients were also obtained. KW - Speed of sound KW - Acoustic resonator KW - Heat capacity PY - 2020 DO - https://doi.org/10.1016/j.ijhydene.2019.12.012 SN - 0360-3199 VL - 45 IS - 7 SP - 4765 EP - 4783 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-50454 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lozano-Martín, D. A1 - Akubue, G. U. A1 - Moreau, A. A1 - Tuma, Dirk A1 - Chamorro, C. R. T1 - Accurate experimental (p, rho, T) data of the (CO2 + O2) binary system for the development of models for CCS processes N2 - The limited availability of accurate experimental data in wide ranges of pressure, temperature, and composition is the main constraining factor for the proper development and assessment of thermodynamic models and equations of state. In the particular case of carbon capture and storage (CCS) processes, there is a clear need for data sets related to the (carbon dioxide + oxygen) mixtures that this work aims to address. This work provides new experimental (p, rho, T) data for three binary (CO2 + O2) mixtures with mole fractions of oxygen x(O2) = (0.05, 0.10, and 0.20) mol/mol, in the temperature range T = (250 to 375) K and pressure range p = (0.5 to 13) MPa. The measurements were performed with a high-precision single-sinker densimeter with magnetic suspension coupling. The density data were obtained with estimated expanded relative uncertainties of 0.02 % for the highest densities and up to 0.3 % for the lowest ones.The results were compared to the corresponding results calculated by the current reference equations of state for this kind of mixtures, namely the EOS-CG (combustion gases) and the GERG-2008 equation of state, respectively. The EOS-CG yields better estimations in density than the GERG-2008 equation of state. The results from the EOS-GC model show no systematic temperature dependence. For the GERG-2008 model, however, this criterion is significantly less fulfilled. KW - carbon capture and storage KW - single-sinker densimeter KW - equation of state PY - 2020 DO - https://doi.org/10.1016/j.jct.2020.106210 SN - 0021-9614 VL - 150 SP - 106210 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-50925 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tuma, Dirk A1 - Lozano-Martín, D. A1 - Vega-Maza, D. A1 - Moreau, A. A1 - Martín, M. C. A1 - Segovia, J. J. T1 - Speed of sound data, derived perfect-gas heat capacities, and acoustic virial coefficients of a calibration standard natural gas mixture and a low-calorific H2-enriched mixture N2 - This work aims to address the technical aspects related to the thermodynamic characterization of natural gas mixtures blended with hydrogen for the introduction of alternative energy sources within the Power-to-Gas framework. For that purpose, new experimental speed of sound data are presented in the pressure range between (0.1 up to 13) MPa and at temperatures of (260, 273.16, 300, 325, and 350) K for two mixtures qualified as primary calibration standards: a 11 component synthetic natural gas mixture (11 M), and another low-calorific H2-enriched natural gas mixture with a nominal molar percentage x(H2) = 3 %. Measurements have been gathered using a spherical acoustic resonator with an experimental expanded (k = 2) uncertainty better than 200 parts in 106 (0.02 %) in the speed of sound. The heat capacity ratio as perfect-gas gammapg, the molar heat capacity as perfect-gas Cp,m pg, and the second betaa and third gammaa acoustic virial coefficients are derived from the speed of sound values. All the results are compared with the reference mixture models for natural gas-like mixtures, the AGA8-DC92 EoS and the GERG-2008 EoS, with Special attention to the impact of hydrogen on those properties. Data are found to be mostly consistent within the model uncertainty in the 11 M synthetic mixture as expected, but for the hydrogen-enriched mixture in the limit of the model uncertainty at the highest measuring pressures. KW - Natural gas mixtures KW - Speed-of-sound measurements KW - Equations of state KW - Acoustic virial coefficients PY - 2021 DO - https://doi.org/10.1016/j.jct.2021.106434 SN - 0021-9614 VL - 158 SP - 106434 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-52292 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tuma, Dirk T1 - Thermophysical properties of hydrogen-containing mixtures for the extension of equation-of-state models for natural gas N2 - The decarbonization of the energy sector is driving the interest in hydrogen as an energy-storage medium. A practical alternative to transport and distribute H2 is using the existing infrastructure for natural gas. The GERG-2008 equation of state currently serves as the ISO standard (ISO 20765-2) for the calculation of thermodynamic properties of natural gas, but H2 appears only as a secondary component. The availability of consolidated data for mixtures with H2 available at the time of its constitution was very limited. The experimental characterization of the thermodynamic behavior of mixtures of H2 with the main components of natural gas is thus of great relevance to validate and improve the GERG-2008 equation of state for its use with H2-enriched natural gas. T2 - Thermodynamik-Kolloquium 2021 CY - Online meeting DA - 27.09.2021 KW - Hydrogen-containing mixtures KW - Density measurements KW - Equations of state PY - 2021 AN - OPUS4-53991 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Chamorro, C. R. T1 - Thermodynamic (p, ρ, T) characterization of H2-enriched natural gases N2 - Hydrogen-enriched natural gas, H2NG is a mixture of natural gas and H2 that can be used on existing natural gas infrastructure with little or even no modification to be applied H2NG is thus an option in the transition from fossil fuels to a hydrogen economy, as it can reduce greenhouse gas emissions and can accelerate the adoption of H2 from renewable sources. Theoretically, H2 can be mixed with NG in any ratio, but H2NG mixtures with up to 20 vol-% of H2 represent the most realistic near term option due to technical and economic reasons. The addition of H2 to natural gas alters the thermodynamic properties of the mixture, which affects its transport, storage, and combustion characteristics. In this work, we present experimental density measurements for different H2NG mixtures, performed with a high-precision single sinker densimeter from 250 to 350 K and up to 20 MPa. The mixtures were prepared gravimetrically according to ISO 6142-1 for maximum precision in their composition. T2 - The 22nd European Conference on Thermophysical Properties ECTP 2023 CY - Venice, Italy DA - 10.09.2023 KW - Hydrogen-enriched natural gas KW - Single-sinker densimeter KW - High-pressure density KW - Equations of state PY - 2023 AN - OPUS4-60473 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Matthias T1 - Primary References for the Determination of Sulphur Impurities in Hydrogen N2 - Fuel cell electric vehicles are expanding quickly from light-duty to heavy-duty applications, such as buses or trucks. Hydrogen fuel quality needs to comply with ISO 14687:2025 to avoid any harmful impact on the vehicles. Total sulphur is one of the most impactful contaminants to a fuel cell system and has a threshold of 4 nmol/mol. In the European Partnership for Metrology (EPM) project Met4H2, BAM together with VSL, the National Metrology Institute of the Netherlands, developed novel gaseous primary reference materials (PRM) to improve the accuracy of the analysis of 7 sulphur compounds (hydrogen sulphide, carbonyl sulphide, methyl mercaptan, ethyl mercaptan, dimethyl sulphide, diethyl sulphide, and tetrahydrothiophene) for the quality control of hydrogen as fuel gas at this challenging amount fraction. These PRM were cross-validated using thermal desorption gas chromatography with a sulphur chemiluminescence detector (TD-GC/SCD). The results are presented and limits discussed. T2 - Joint workshop EMN for Energy Gases CY - Delft, Netherlands DA - 26.03.2025 KW - Sulphur impurities KW - Hydrogen KW - GC/SCD KW - Reference gas standards PY - 2025 AN - OPUS4-62818 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Klinge, Andrea A1 - Mönig, Julian A1 - Kalbe, Ute A1 - Richter, Matthias A1 - Horn, Wolfgang A1 - Ziegert, Christof A1 - Röhlen, Ulrich A1 - Roswag-Klinge, Eike T1 - upMIN 100 – upcycling MINeralischer Bau- und Abbruchabfälle zur Substitution natürlicher Gesteinskörnungen in Lehmbaustoffen T1 - upMIN 100 – Upcycling mineral construction and demolition debris as a substitute for natural aggregates in earth building materials N2 - Um zukünftig die Entnahme von Primärrohstoffen und die Deponierung von geeignetem Bodenaushub zu vermeiden, wurde im Forschungsvorhaben «upMIN100» der Einsatz von rezyklierten Gesteinskörnungen < 2 mm in Lehmbaustoffen untersucht. Diese Korngrößen aus Rezyklaten, die je nach Ausgangsstoffen und Produkt 5 – 70 % des fertigen Baustoffs ausmachen, waren zum Zeitpunkt des Projektstarts in den gültigen Lehmbaustoff-Normen DIN 18945 – 18948 nicht zugelassen, da diese als Zusatzstoffe nur natürliche Gesteinskörnungen nach DIN EN 12620, Mehl aus mörtelfreien Ziegeln sowie Blähperlit etc. nach DIN EN 13055-1 und als Bindemittel nur Baulehm aus natürlichen Vorkommen vorsahen. Um den Einsatz von rezyklierten Bau- und Abbruchabfällen für Lehmbaustoffe in der Norm zu ermöglichen, mussten daher die technische Durchführbarkeit, Qualitätsanforderungen an Ausgangsstoffe (z.B. Schadstoffgrenzwerte in Bezug auf Gesundheits- und Umweltverträglichkeit) sowie zulässige Anteile der Rezyklate geregelt werden. Aktuelle Sortier- und Aufbereitungsmethoden wurden im Hinblick auf die technische sowie die wirtschaftliche Machbarkeit überprüft und auf eine mögliche Optimierung untersucht. Um Fragen zur technischen Machbarkeit beantworten zu können, wurde im Vorhaben die exemplarische Entwicklung von zwei wiederverwendbaren Lehmbaustoffen (Lehmstein, Lehmputzmörtel) angestrebt, um zukünftig sowohl das Abfallaufkommen als auch die Rohstoffinanspruchnahme zu reduzieren. Zum einen sollten die Zuschläge bis zu 100% aber auch das natürliche Bindemittel Ton zu 80% – 100% substituiert werden. Der Machbarkeitsnachweis für beide Entwicklungen wurde in Form eines Prototyps mit einem Technologie-Reifegrad 4–5 (TRL 4–5) erbracht. N2 - To avoid the extraction of primary raw materials and the landfilling of suitable excavated soil in the future, the use of recycled aggregates < 2 mm in earth building materials was investigated in the “upMIN 100” research project. These grain sizes from recycled materials, which make up 5–70 % of the finished building material depending on the source materials and product, were not permitted in the applicable earth building material standards DIN 18945–18948 at the time the project started, as these only allow natural aggregates in accordance with DIN EN 12620, flour from mortarfree bricks and expanded perlite etc. as additives in accordance with DIN EN 13055-1 and only building clay from natural sources as a binder. For the use of recycled construction and demolition waste for earth building materials in the standard, the technical feasibility, quality requirements for source (e. g. limit values for harmful substances in terms of health and environmental compatibility) and permissible proportions of recyclates had to be regulated. Current sorting and processing methods were reviewed in terms of technical and economic feasibility and examined for possible optimisation. To ascertain the technical feasibility of the use of recycled construction demolition waste for earth building materials, the project developed two reusable earth building materials (earth blocks, clay plaster mortar) as examples of both waste reduction and of the use of raw materials in the future. On the one hand, up to 100 % of the aggregates and 80–100 % of the natural binder clay should be substituted. The proof of concept for both developments was provided in the form of a prototype with a technology readiness level 4–5 (TRL 4–5). T2 - Lehm 2024 Fachtagung CY - Weimar, Germany DA - 27.09.2024 KW - Recycled aggregates KW - Earthen building materials KW - Contaminants KW - Reuse KW - Resources PY - 2024 SP - 1 EP - 10 CY - Weimar AN - OPUS4-62612 LA - deu 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 - Soruco Aloisio, Ricardo T1 - Digitale Abbildung von Assets - Dateninfrastruktur für Industrie 4.0 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 aufgebaut. Zudem wurde der von der Plattform Industrie 4.0 empfohlene standardisierte Zwilling „Verwaltungsschale“ für einige Assets der Wasserstofftankstelle implementiert. T2 - QI-Forum 2024 CY - Berlin, Germany DA - 09.10.2024 KW - Datenintregration KW - IT KW - Infrastruktur KW - OT KW - Open Source KW - Software KW - VPN KW - Verwaltungsschale PY - 2024 AN - OPUS4-63493 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Adame, Andressa T1 - Development of an automatic system for in situ analysis of soil using a handheld Energy Dispersive X-Ray Fluorescence (EDXRF) N2 - The project “Intelligence for Soil” (I4S) aims at the design of an integrated system for improvement of soil functions and fertilizer recommendations. This system is composed by different sensors that will provide a detailed assessment of soil properties and processes, which are prerequisites for a site-specific, resource-saving and ecofriendly soil management, considering the soil as a sustainable resource for the bioeconomy. One of these sensors will be an energy-dispersive X-Ray Fluorescence spectrometer. It is a non-destructive technique suitable for in-situ measurements due to a minimum sample preparation and it allows fast multielement analyses. In this work, an automatic system has been developed using a handheld equipment from Olympus (Vanta C series). A polypropylene (PP) film was used to protect the measuring window of the device from dust and possible cross-contamination. To control the stepper motor that unrolls the PP film, a microcontroller was used to ensure that a piece of clean PP is in front of the measuring window for each new analysis. Preliminary calibration studies using pre-defined methods, Geochem and Soil Methods, were performed with the following Certified Reference Materials (CRMs): NRC Till 1-3, NIST 2710, BAM U110, ERM CC141, BCR 142R, IAEA Soil 7. The CRMs were measured 10 times at different spots. The spot size was 10 mm in diameter, irradiation time was 60 ? s. The averaged data from X ray characteristic emission line intensities for Al, P, Si, Ca, Fe, Mn, Zn, Cu and Ni Kα were in close agreement with certified mass fraction data. The linear correlation coefficients (r) ranged from 0.852 for P to 0.999 for Mn. A second round of calibration studies were performed with the following CRMs: GBW07402, GBW 07405, NCS DC 73023, NCS DC 73030, NCS DC 85109, NCS DC 87104, NIST 1646a, NIST 2704, NIST 2710, NRC Till 1-3, VS 2498-83, and the same pre-defined methods and experimental parameters were employed. The results of the 13 CRMs were now compared with the values obtained by a validated WDXRF method. The linear correlation coefficients (r) ranged from 0.998 for Ca to 0.999 for Zn. Other elements such as S, K and Ti can also be properly determined, but validation still requires more robust calibration models. Further calibration studies will be performed in order to circumvent matrix effects and to guarantee reliable results. Besides that, the automatic system will be placed on a mobile sensor platform and the system will be tested in the field. A guidance for on site-specific fertilization integrating the results obtained from different sensors placed on the platform is expected. T2 - 16. Kolloquium Prozessanalytik CY - Online Meeting DA - 23.11.2020 KW - Röntgenfluoreszenz KW - Boden KW - XRF KW - Soil PY - 2020 AN - OPUS4-51776 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - Schnelle Identifizierung von Mineralwolle mittels Nah-Infrarot-Spektroskopie N2 - Künstliche Mineralfasern (KMF) werden weltweit in vielfältiger Weise als Dämmstoffe verwendet. Jährlich fallen in Deutschland ungefähr 20 Millionen Tonnen KMF an, die nach dem Abriss auf Deponien entsorgt werden müssen. Grundsätzlich besteht jedoch die Möglichkeit der Rückführung dieser Materialien in den Produktionsprozess. Dafür ist es notwendig, anfallende KMF sowohl nach Material (Glaswolle, Steinwolle) als auch nach Alter zu sortieren. Auf der Suche nach einer Methode, die es grundsätzlich gestattet eine schnelle Untersuchung vor Ort auf einer Baustelle durchzuführen, wurde die Nah-Infrarot (NIR) Spektroskopie unter Verwendung eines Prozessspektrometers mit Reflexionssonde getestet. Anhand von Laboruntersuchungen an 70 KMF Proben, die entweder betriebsneu waren oder bundesweit auf Baustellen gesammelt wurden, konnte eine NIR-basierte Methode zur Unterscheidung in Glas- und Steinwolle entwickelt werden. Mittels Partial Least Square Diskriminanzanalyse (PLS-DA) der NIR Spektren wurde basierend auf 40 zufällig ausgewählten Proben ein chemometrisches Modell kalibriert, das erfolgreich zur Klassifizierung der verbleibenden 30 Proben eingesetzt werden konnte. Unabhängig von Farbe, Dichte oder Alter der untersuchten KMF Proben war es möglich, eine 100% korrekte Zuordnung des Materials zu erzielen. Die nötigen Referenzwerte wurden unter Nutzung eines Röntgenfluoreszenzspektroskopischen Verfahrens über den Elementgehalt nach VDI 3492 ermittelt. Insgesamt ist der experimentelle Aufwand für die Durchführung und Auswertung der NIR Messungen gering und manifestiert sich vor allem in der Kalibrierphase, die in diesem Fall die Untersuchung von 8-fach aliquotierten Probestücken der 70 KMF umfasste. Nur bei deutlich feuchtem Material muss ein zusätzlicher Trocknungs-schritt berücksichtigt werden. Das vorgestellte Verfahren wurde nachfolgend zu einem Patent angemeldet. Untersuchungen zu einer weiteren Unterscheidung der KMF nach Alter sind geplant. T2 - 16. Kolloquium Prozessanalytik der GDCh & Dechema CY - Online meeting DA - 23.11.2020 KW - Mineralwolle KW - NIR KW - Chemometrie PY - 2020 AN - OPUS4-51731 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Industrielle Anwendungen der Niederfeld-NMR-Spektroskopie für die Prozess- und 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 Forschungs-kooperation 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 - 10. ProcessNet-Jahrestagung CY - Online meeting DA - 21.09.2020 KW - NMR-Spektroskopie KW - Benchtop-NMR KW - Silane PY - 2020 AN - OPUS4-51350 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Industrial applications of low-field NMR spectroscopy for process and 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 - Practical Applications of NMR in Industry Conference (PANIC) CY - Online meeting DA - 19.10.2020 KW - Process Analytical Technology KW - NMR spectroscopy KW - Benchtop-NMR KW - Process-NMR PY - 2020 AN - OPUS4-51465 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Westwood, S. A1 - Martos, G. A1 - Josephs, R. A1 - Choteau, T. A1 - Wielgosz, R. A1 - Davies, S. A1 - Moawad, M. A1 - Tarrant, G. A1 - Chan, B. A1 - Alamgir, M. A1 - de Rego, E. A1 - Wollinger, W. A1 - Garrido, B. A1 - Fernandes, J. A1 - de Sena, R. A1 - Oliveira, R. A1 - Melanson, J. A1 - Bates, J. A1 - Mai Le, P. A1 - Meija, J. A1 - Quan, C. A1 - Huang, T. A1 - Zhang, W. A1 - Ma, R. A1 - Zhang, S. A1 - Hao, Y. A1 - He, Y. A1 - Song, S. A1 - Wang, H. A1 - Su, F. A1 - Zhang, T. A1 - Li, H. A1 - Lam, W. A1 - Wong, W. A1 - Fung, W. A1 - Philipp, Rosemarie A1 - Dorgerloh, Ute A1 - Meyer, Klas A1 - Piechotta, Christian A1 - Riedel, Juliane A1 - Westphalen, Tanja A1 - Giannikopoulou, P. A1 - Alexopoulos, Ch. A1 - Kakoulides, E. A1 - Kitamaki, Y. A1 - Yamazaki, T. A1 - Shimizu, Y. A1 - Kuroe, M. A1 - Numata, M. A1 - Pérez-Castorena, A. A1 - Balderas-Escamilla, M. A1 - Garcia-Escalante, J. A1 - Krylov, A. A1 - Mikheeva, A. A1 - Beliakov, M. A1 - Palagina, M. A1 - Tkachenko, I. A1 - Spirin, S. A1 - Smirnov, V. A1 - Tang Lin, T. A1 - Pui Sze, C. A1 - Juan, W. A1 - Lingkai, W. A1 - Ting, L. A1 - Quinde, L. A1 - Yizhao, C. A1 - Lay Peng, S. A1 - Fernandes-Whaley, M. A1 - Prevoo-Franzsen, D. A1 - Quinn, L. A1 - Nhlapo, N. A1 - Mkhize, D. A1 - Marajh, D. A1 - Chamane, S. A1 - Ahn, S. A1 - Choi, K. A1 - Lee, S. A1 - Han, J. A1 - Baek, S. A1 - Kim, B. A1 - Marbumrung, S. A1 - Jongmesuk, P. A1 - Shearman, K. A1 - Boonyakong, C. A1 - Bilsel, M. A1 - Gündüz, S. A1 - Ün, I. A1 - Yilmaz, H. A1 - Bilsel, G. A1 - Gökçen, T. A1 - Clarkson, C. A1 - Warren, J. A1 - Achtar, E. T1 - Mass fraction assignment of Bisphenol-A high purity material N2 - The CCQM-K148.a comparison was coordinated by the BIPM on behalf of the CCQM Organic Analysis Working Group for NMIs and DIs which provide measurement services in organic analysis under the CIPM MRA. It was undertaken as a "Track A" comparison within the OAWG strategic plan. CCQM-K148.a demonstrates capabilities for assigning the mass fraction content of a solid organic compound having moderate molecular complexity, where the compound has a molar mass in the range (75 - 500) g/mol and is non-polar (pKow < −2), when present as the primary organic component in a neat organic solid and where the mass fraction content of the primary component in the material is in excess of 950 mg/g. Participants were required to report the mass fraction of Bisphenol A present in one supplied unit of the comparison material. Participants using a mass balance method for the assignment were also required to report their assignments of the impurity components present in the material. Methods used by the seventeen participating NMIs or DIs were predominantly based on either stand-alone mass balance (summation of impurities) or qNMR approaches, or the combination of data obtained using both methods. The results obtained using thermal methods based on freezing-point depression methods were also reported by a limited number of participants. There was excellent agreement between assignments obtained using all three approaches to assign the BPA content. The assignment of the values for the mass fraction content of BPA consistent with the KCRV was achieved by most of the comparison participants with an associated relative standard uncertainty in the assigned value in the range (0.1 - 0.5)%. KW - Bisphenol-A KW - Purity assessment KW - Interlaboratory key comparison KW - Metrology PY - 2021 DO - https://doi.org/10.1088/0026-1394/58/1A/08015 VL - 58 IS - 1A SP - 08015 PB - IOP Publishing AN - OPUS4-54188 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -