TY - JOUR A1 - Bessaies-Bey, H. A1 - Khayat, K. H. A1 - Palacios, M. A1 - Schmidt, Wolfram A1 - Roussel, N. T1 - Viscosity modifying agents: Key components of advanced cement-based materials with adapted rheology N2 - Viscosity modifying agents (VMAs) are essential ingredients for the production of flowable cement-based materials. This paper presents an overview of commonly used VMAs and attempts to shed some light on the underlying physics at the origin of their mechanisms of action. The main molecular parameters of VMA controlling the rheological properties of the cement pore solution are highlighted. As the mechanisms of action of VMAs in cement-based materials are closely related to their affinity with the surface of cement particles, the adsorption of the main VMA types is discussed. The effect of VMAs on flow properties and stability of cement-based materials is presented for VMAs added without any superplasticizer, and then in systems incorporating both VMAs and superplasticizers. Finally, the effect of VMAs in enhancing concrete properties to secure adequate performance of different construction applications, and perspectives for future developments of novel cement-based materials made with VMAs are showcased. KW - Viscosity modifying agents KW - Cement KW - Stability KW - Rheology KW - Working mechanism KW - Compatibility PY - 2022 DO - https://doi.org/10.1016/j.cemconres.2021.106646 VL - 152 SP - 1 EP - 20 PB - Elsevier AN - OPUS4-58396 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, K. A1 - Mezhov, Alexander A1 - Schmidt, Wolfram T1 - Effect of Polycarboxylate Superplasticizer in Ordinary Portland Cement and Sulfate Resistant Cement N2 - Polycarboxylate superplasticizers (PCE) are the most widely used admixtures in today’s cementitious construction materials. The molecular structure has a decisive influence on the effectiveness of PCE, which also can be tailored to serve in a different cementitious system. The current study investigates the influence of the backbone charge density of PCE on the rheology, hydration kinetics, and adsorption behavior of ordinary Portland cement (OPC) and sulfate-resistant cement (SRC). The results indicate that regardless of the PCE type, OPC requires a higher amount of PCE to be adsorbed to induce changing of rheological parameters and hydration kinetics. Regardless of the cement type, the PCE with a higher charge density exhibits higher adsorption behavior, corresponding to lower viscosity measurement. Compared to OPC, SRC is more sensitive to the introduction of both PCEs and has a lower saturation dosage, indicating that SRC generally provides better workability properties regardless of the PCE. KW - Polycarboxylate superplasticizers (PCE) KW - Sulfate resistant cement (SRC) KW - Rheological KW - Adsorption KW - Cement hydration PY - 2023 DO - https://doi.org/10.1061/JMCEE7.MTENG-15033 SN - 0899-1561 VL - 35 IS - 6 SP - 1 EP - 12 PB - ASCE Libary AN - OPUS4-58244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Wolfram A1 - Cunnigham, P. R. A1 - Shaba, A. F. A1 - Olonade, K. A. A1 - Ndawula, J. A1 - Tawiah, A. T. A1 - Marangu, J. M. A1 - Tlhatlha, Pheladi A1 - Obeng, E. ED - Banhia, N. T1 - Informal Sector Inclusion in Sustainable Concrete Construction in Africa N2 - Concrete used as a construction material is inevitable in Africa’s rapid urban growth, despite its significant contribution to carbon emissions. Hence, best practice concrete with reduced Portland cement clinker needs to be applied. The highly informal nature ofAfrica’s construction sector could impede the implementation of sustainable concrete construction. Although urgent need for economisation unintentionally often leads informal actors to operate according to circularity principles, the sector lacks awareness of climate challenges and incentives for adopting climate-friendly materials and technologies. In addition, the informal sector is prone to fraudulent adulterated materials and components causing challenges for safe and durable construction. The authors elaborate on the crucial role of the informal sector in driving sustainable construction forward, despite the lack of policies and disinterest from regulatory bodies. Solutions through education, communication, and quality control are proposed and discussed. T2 - 77th RILEM Annual Week and the 1st Interdisciplinary Symposium on Smart & Sustainable Infrastructures (ISSSI 2023) CY - Vancouver, Canada DA - 04.09.2023 KW - Cement testing KW - Hydration KW - Economic development KW - Informal sector KW - Cement chemistry PY - 2024 SN - 978-3-031-53391-4 DO - https://doi.org/10.1007/978-3-031-53389-1_47 VL - 48 SP - 506 EP - 520 PB - Springer Nature Switzerland AG CY - Schweiz AN - OPUS4-61586 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmidt, Wolfram A1 - Kanjee, J. A1 - Motukwa, G. A1 - Olonade, K. A1 - Dodoo, A. T1 - A snapshot review of future‑oriented standards for cement, admixtures, and concrete: How Africa can spearhead the implementation of green urban construction materials N2 - The existing cement and concrete standards are not capable of making full use of the current technology capacity due to strong focus on conventional concrete and thus they are not fit for the current and future challenges of construction industry. The paper highlights shortcomings with regard to the implementation of the existing standards. It can be seen that future-oriented standards are generally required to contribute to a lower-carbon footprint of the industry. These changes are significantly more relevant in sub-Saharan Africa, due to the rapidly increasing urbanisation challenge and the enormous potentials to develop lower-carbon technologies than elsewhere in the world. KW - Future‑oriented standards KW - Green urban construction KW - Cement PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-582563 DO - https://doi.org/10.1557/s43580-023-00563-9 SN - 2731-5894 VL - 4 IS - 8 SP - 557 EP - 565 PB - Springer International Publishing CY - Springer Nature Switzerland, Cham AN - OPUS4-58256 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, K. A1 - Mezhov, Alexander A1 - Schmidt, Wolfram T1 - Chemical and thixotropic contribution to the structural build-up of cementitious materials N2 - The structural build-up of fresh cement paste is often considered as a purely thixotropic phenomenon in literature even though cementitious materials undergo a non-reversible hydration process that can have an influence on the structuration process. In the current paper a method is proposed to validate the impact of the non-reversible structural build-up. It is shown that fresh cement paste samples lose their structural gain almost completely due to thixotropy while the structural build-up due to hydration can be observed but occurs in a significantly lower order of magnitude over the course of the first hours of hydration. In addition, it is shown, that the chemical component of the structural build-up accelerates with the onset of the acceleration period of hydration, while its contribution in the entire structural build-up remains constant. KW - Thixotropy KW - Structural build-up KW - Penetration test KW - Rheological properties PY - 2022 DO - https://doi.org/10.1016/j.conbuildmat.2022.128307 SN - 0950-0618 VL - 345 IS - 128307 SP - 1 EP - 10 PB - Elsevier Ltd. AN - OPUS4-58248 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zhang, K. A1 - Mezhov, Alexander A1 - Schmidt, Wolfram T1 - Thixotropic and chemical structural build-up of cement pastes with superplasticizer under different storage conditions N2 - Synopsis: The paper presents the results of a study on the influence of agitation on the structural build-up of fresh cement pastes using a penetration test. It first presents results about the influence of the penetrating shape’s geometry on the influence on the cement paste specimen. Then, results are shown for the load-deflection curves depending upon time and agitation before testing. Based on the observation of the force required to penetrate the sample, conclusions on the structural build-up can be made. The observations were made over the course of time with samples that were left at rest and partly agitated before testing at different time steps. The setup allows to identify the contribution of the chemical reaction to the structural build-up process. The presence of superplasticizer obviously reduces the load that cement paste can withstand, while the loss of thixotropy is found notably lower than that of neat cement pates T2 - 13th International Conference on Superplasticizers and Other Chemical Admixtures in Concrete CY - Milan, Italy DA - 10.07.2022 KW - Thixotropy KW - Superplasticizer KW - Structural build-up KW - Texture analyzer KW - Penetration test PY - 2022 DO - https://doi.org/10.14359/51736058 VL - 354 SP - 13 EP - 24 PB - ACI Special Publications AN - OPUS4-58324 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zhang, K. A1 - Schmidt, Wolfram A1 - Mezhov, Alexander T1 - Influence of the hydroxypropylation of starch on its performance as viscosity modifying agent N2 - Synopsis: Starch is a commonly used viscosity modifying agent (VMA). The performance of starch as VMA depends on its origin (e.g. potato, corn, cassava, etc.) and corresponding molecular properties, such as molecular weight, ratio between amylose and amylopectin etc. Depending upon the application, the efficiency of starch can be enhanced by hydroxypropylation. The maximum degree of substitution (DoS) cannot be greater than 3.0, which is the number of hydroxy groups per glucose monomer in the polymer. In the current research three potato starches exhibiting the DoS of 0.4, 0.6 and 0.8 were utilised. The influence of the modified starch on the rheological properties and hydration of cement paste, as well as the viscosity of the pore solution were investigated. Our findings show that the starch with the highest DoS increases the dynamic yield stress the most, while the plastic viscosity is less dependent on the DoS. Additionally, starch with the highest DoS retards hydration to lower degree than other starches. T2 - 13th International Conference on Superplasticizers and Other Chemical Admixtures in Concrete CY - Milan, Italy DA - 10.07.2022 KW - Potato starch KW - Rheological KW - Cement hydration KW - Pore solutions PY - 2022 DO - https://doi.org/10.14359/51736074 VL - 354 SP - 209 EP - 218 PB - ACI Special Publications AN - OPUS4-58320 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mezhov, Alexander A1 - Zhang, K. A1 - Schmidt, Wolfram T1 - Interactions of Biobased Rheology Modifying Agents with Superplasticizer in Cement Paste N2 - Organic admixtures are an indispensable component of modern concrete. Thus, their purposeful application is not only technically and economically viable but in addition an inevitable tool to make concrete more environmentally friendly. In this context, the use of polysaccharides has increasingly gained interest in the built environment as sustainable resource for performance enhancement. However, due to its origin, biopolymers possess a vast variety of molecular structures which can result in incompatibilities with other polymers present in concrete, such as superplasticizers. The present study highlights effects of the joint application of different types of starches and polycarboxylates with respect to their influence on cement hydration and structural build-up of cement pastes. KW - Polysaccharides KW - Superplasticizers KW - Hydration KW - Cement PY - 2022 DO - https://doi.org/10.4028/www.scientific.net/CTA.1.563 SN - 2674-1237 SP - 563 EP - 568 PB - Trans Tech Publications Ltd, Switzerland CY - Basel, Switzerland. AN - OPUS4-58325 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Wolfram A1 - Olonade, K. A. A1 - Mbugua, R. N. A1 - Lenz, F. J. A1 - Tchetgnia Ngassam, I. T1 - Bio-Based Rheology Modifiers for High Performance Concrete – Possible Modes of Actions and Case Study for Cassava Starch in West Africa N2 - Polymers that help tailoring rheological properties during the casting process have become inevitable constituents for all kinds of high-performance concrete technologies. Due to lacking industries, these typically crude-oil based admixtures are not readily available in many parts of the world, which limits the implementation of more sustainable high-performance construction technologies in these regions. Alternative polymers, which often demand for less processing, can be derived from local plant-based resources. The paper provides experimental data of flow tests of cement pastes with polysaccharides from Triumfetta pendrata A. Rich, acacia gum and cassava without and in the presence of polycarboxylate ether superplasticizer. The flow tests are amended by observations of the zeta potentials and the hydrodynamic diameters in the presence of and without calcium ions in the dispersion medium. The results show that in the presence of and without calcium ions all polysaccharides provide negative zeta potentials, yet, they affect flowability and thixotropy in different ways. Cassava starch, acacia gum, and the gum of Triumfetta pendrata A. Rich qualified well for robustness improvement, strong stiffening, and additive manufacturing, respectively. The reason for the different effects can be found in their average sizes and size distribution. Due to the promising results, a flow chart for local value chains is derived on the example of yet unused cassava wastes, which can be converted in parallel. T2 - 3rd International Conference on the Application of Superabsorbent Polymers CY - Skukuza, South Africa KW - Admixtures KW - Polysaccharides KW - Rheology KW - Thixotropy KW - Concrete PY - 2020 SN - 978-3-030-33341-6 SN - 978-3-030-33342-3 DO - https://doi.org/10.1007/978-3-030-33342-3_17 SP - 158 EP - 166 PB - Springer AN - OPUS4-58404 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmidt, Wolfram A1 - Tchetgnia Ngassam, Ines Leana A1 - Olonade, K. A. A1 - Mbugua, R. A1 - Kühne, Hans-Carsten T1 - Plant based chemical admixtures – potentials and effects on the performance of cementitious materials N2 - While today, engineers can choose from a wide range of rheology modifying admixtures, in some parts of the world, these are difficult to access, due to their complex processing. However, alternatives can be bio‐based polymers such as polysaccharides from various sources. These are easily accessible all over the world, do not demand for complicated processing, and typically they are more sustainable than many established materials, which are crude oil‐based. The paper presents the effects of acacia gum, cassava starch and the gum of triumfetta pendrata A. Rich on the rheological performance of cementitious systems. It is shown that acacia gum can be as efficient as polycarboxylate based superplasticisers, cassava starch can reduce the yield stress slightly with little effect on the plastic viscosity, and the gum of triumfet ta pendrata A. Rich increases the thixotropy of cement pastes with plasticizing polymers significantly. KW - Polysaccharides KW - Rheology KW - Cement KW - Chemical admixtures KW - Bio-based concrete PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-476748 DO - https://doi.org/10.21809/rilemtechlett.2018.83 VL - 3 SP - 124 EP - 128 PB - RILEM S.A.R.L. CY - Paris AN - OPUS4-47674 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Wolfram A1 - Tchetgnia Ngassam, I. L. A1 - Mbugua, R. A1 - Olonade, K. A. ED - Greim, M. ED - Kusterle, W. ED - Teubert, O. T1 - Natural rheology modifying admixtures for concrete N2 - The possibility to tailor the rheology of concrete eventually opened up the path to new technologies, where design criteria are no longer limited to the compressive strength. Thus, it can be concluded that the capability to control the rheology of concrete can be considered as catalyst for many of today’s concrete innovations. In the same way rheology modifying admixtures will be key to mastering the challenges of the next decades. In many regions of the Southern hemisphere, the effective use of chemical admixtures would significantly contribute to solve problems induced by the challenging climate, but particularly in Africa there is often a lack of local supply and supply infrastructure. In Africa, concrete admixtures are largely shipped or transported from outside the continent. The long distance transportation of chemicals is not very environmentally friendly and the economic consequences are dramatic: the agents are difficult to purchase, expensive, and there is no large variety of products available in the market. Due to the enormous relevance of rheology modifying admixtures, it is worthwhile to recollect that nature provides an enormous variety of chemicals that can be used readily or with low processing and without enormous transportation distances, since these plants are typically regionally abundantly available, cheap, and they are environmental friendly. The paper presents an overview of various options for rheology modifying admixtures, that can be found in Africa, and that may become a real alternative, once their interaction within the complex cementitious system is well understood. T2 - 26. Workshop und Kolloquium "Rheologische Messungen an Baustoffen" CY - Regensburg, Germany DA - 21.02.2017 KW - Concrete KW - Rheology PY - 2017 SN - 978-3-7439-0171-1 SP - 75 EP - 87 PB - tredition GmbH CY - Hamburg AN - OPUS4-40599 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bresch, Harald A1 - Hodoroaba, Vasile-Dan A1 - Schmidt, Alexandra A1 - Rasmussen, K. A1 - Rauscher, H. T1 - Counting Small Particles in Electron Microscopy Images — Proposal for Rules and Their Application in Practice N2 - Electron microscopy (EM) is the gold standard for the characterisation of the morphology (size and shape) of nanoparticles. Visual observation of objects under examination is always a necessary first step in the characterisation process. Several questions arise when undertaking to identify and count particles to measure their size and shape distribution. In addition to challenges with the dispersion and identification of the particles, more than one protocol for counting particles is in use. This paper focuses on precise rules for the counting of particles in EM micrographs, as this influences the measurement accuracy of the number of particles, thus implicitly affecting the size values of the counted particles. We review and compare four different, commonly used methods for counting, which we then apply in case studies. The impact of the selected counting rule on the obtained final particle size distribution is highlighted. One main aim of this analysis is to support the application of a specific, well-defined counting approach in accordance with regulatory requirements to contribute to achieving more reliable and reproducible results. It is also useful for the new harmonised measurement procedures for determining the particle size and particle size distribution of nanomaterials. KW - Nano KW - Particle size distribution KW - Nanoparticle KW - Nanomaterial KW - OECD PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551891 DO - https://doi.org/10.3390/nano12132238 SN - 2079-4991 VL - 12 IS - 13 SP - 2238 PB - MDPI CY - Basel AN - OPUS4-55189 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lüth, Peter A1 - Frost, K. A1 - Kurth, Lutz A1 - Malow, Marcus A1 - Schmidt, Martin A1 - Michael-Schulz, Heike A1 - Uhlig, S. A1 - Zakel, S. T1 - CEQAT-DGHS Ringversuchsprogramm für die Chemikaliensicherheit - Schlussfolgerungen N2 - Die Ursachen für Chemikalienunfälle können vielfältig sein. Prävention beginnt bereits im Prüflabor, wenn Chemikalien auf ihre gefährlichen Eigenschaften getestet werden. Dazu sind Prüfmethoden entwickelt und veröffentlicht worden, die heute weltweit Anwendung finden. Auf die Validität der Prüfmethode und richtige Durchführung der Prüfung im Laboratorium müssen sich Sicherheitsfachkräfte, Transporteure oder Händler verlassen können. Anhand der in den letzten 10 Jahren im Rahmen des CEQAT-DGHS von BAM und PTB durchgeführten Ringversuche (RV) wird gezeigt, dass bei allen bisher untersuchten Prüfmethoden ein Verbesserungsbedarf besteht. Die RV müssen daher zunächst auf die Methodenverbesserung und -validierung abzielen und nicht auf Leistungstests. Das Labormanagement und die praktische Durchführung der Prüfung sind in vielen Laboratorien verbesserungsbedürftig. Der Begriff „Erfahrung der Prüfer“ ist kritisch zu sehen: Eine „lange Erfahrung mit vielen Prüfungen“ ist nicht unbedingt ein Garant für richtige Ergebnisse. T2 - 15. BAM-PTB-Kolloquium zur chemischen und physikalischen Sicherheitstechnik CY - Braunschweig, Germany DA - 21.05.2019 KW - Gefahrgut KW - Gefahrstoff KW - Ringversuch KW - Prüfmethode KW - Validierung KW - Qualitätssicherung PY - 2019 UR - https://www.ptb.de/cms/index.php?id=18763 DO - https://doi.org/10.7795/210.20190521M SP - 1 EP - 8 PB - Physikalisch-Technische Bundesanstalt (PTB) CY - Braunschweig AN - OPUS4-49489 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lüth, Peter A1 - Frost, K. A1 - Kurth, Lutz A1 - Malow, Marcus A1 - Schmidt, Martin A1 - Michael-Schulz, Heike A1 - Uhlig, S. A1 - Zakel, S. T1 - CEQAT-DGHS Ringversuchsprogramm für die Chemikaliensicherheit – Entwicklung von Verfahren zur Verifizierung der Prüfapparatur am Beispiel der Prüfmethode UN Test N.5 N2 - Prävention beginnt im Prüflabor, wenn Chemikalien auf ihre gefährlichen Eigenschaften getestet werden. Dazu sind Prüfmethoden entwickelt und veröffentlicht worden, die heute weltweit Anwendung finden. Auf die Validität der Prüfmethode und richtige Durchführung der Prüfung im Laboratorium müssen sich Sicherheitsfachkräfte, Transporteure oder Händler verlassen können. Anhand der in den letzten 10 Jahren im Rahmen des CEQAT-DGHS von BAM und PTB durchgeführten Ringversuche (RV) wird gezeigt, dass bei allen bisher untersuchten Prüfmethoden ein Verbesserungsbedarf besteht. Die RV müssen daher zunächst auf die Methodenverbesserung und -validierung abzielen und nicht auf Leistungstests. Das Labormanagement und die praktische Durchführung der Prüfung sind in vielen Laboratorien verbesserungsbedürftig. Der Begriff „Erfahrung der Prüfer“ ist kritisch zu sehen: Eine „lange Erfahrung mit vielen Prüfungen“ ist nicht unbedingt ein Garant für richtige Ergebnisse. Bei der Prüfung der gefährlichen Eigenschaften von Chemikalien sind Referenzmaterialen auf Grund der Instabilität in der Regel nicht verfügbar. Für Prüflaboratorien sind RV daher eine Alternative bei der Qualitätssicherung. RV sind jedoch aufwendig und können nur in relativ großen Zeitabständen durchgeführt werden. Es sind deshalb Verfahren zur Verifizierung z. B. der in den Laboratorien verwendeten Prüfapparaturen zu entwickeln. Die Entwicklung von Verifizierungsverfahren wird am Bespiel der Prüfmethode UN Test N.5 demonstriert. T2 - 15. BAM-PTB-Kolloquium zur chemischen und physikalischen Sicherheitstechnik CY - Braunschweig, Germany DA - 21.05.2019 KW - Gefahrgut KW - Gefahrstoff KW - Ringversuch KW - Prüfmethode KW - Validierung KW - Qualitätssicherung KW - Verifizierung PY - 2019 UR - https://www.ptb.de/cms/index.php?id=18763 DO - https://doi.org/10.7795/210.20190521E SP - 1 EP - 10 CY - Braunschweig AN - OPUS4-49495 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lüth, Peter A1 - Frost, K. A1 - Kurth, Lutz A1 - Malow, Marcus A1 - Michael-Schulz, Heike A1 - Schmidt, Martin A1 - Schulte, Petra A1 - Uhlig, S. A1 - Zakel, S. T1 - CEQAT-DGHS Interlaboratory Test Programme for Chemical Safety - Need of Test Methods Validation N2 - Safety experts, manufacturers, suppliers, importers, employers or consumers must be able to rely on the validity of safety-related test methods and on correct test results and assessments in the laboratory. Via the eChemPortal lots of data from the REACH registration dossiers are available. However, the quality and correctness of the information remains in the responsibility of the data submitter. Unfortunately, we found more or less appropriate information on physicochemical properties and concluded that more quality or adequacy of any data submitted will be needed. Interlaboratory tests play a decisive role in assessing the reliability of test results. Interlaboratory tests on different test methods have been performed by Bundesanstalt für Materialforschung und –prüfung (BAM) and Physikalisch-Technische Bundesanstalt (PTB) in collaboration with the QuoData GmbH during the last 10 years. Significant differences between the results of the participating laboratories were observed in all interlaboratory tests. The deviations of the test results were not caused only by laboratory faults but also by deficiencies of the test method. In view of the interlaboratory test results the following conclusions can be drawn: • To avoid any discrepancy on classification and labelling of chemicals it should become state of the art to use validated test methods and the results accompanied by the measurement uncertainty. • A need for improvement is demonstrated for all examined test methods. Thus, interlaboratory tests shall initially aim at the development, improvement and validation of the test methods and not on proficiency tests. • The laboratory management and the practical execution of the tests need to be improved in many laboratories. • The term "experience of the examiner" must be seen critically: A "long experience with many tests" is not necessarily a guarantee for correct results. T2 - 16th International Symposium on Loss Prevention and Safety Promotion in the Process Industries and accompanying exhibition. Loss prevention 2019 CY - Delft, The Netherlands DA - 16.06.2019 KW - Dangerous goods KW - Hazardous substances KW - Round robin test KW - Interlaboratory comparison KW - Test method KW - Validation KW - Quality assurance PY - 2019 UR - https://www.aidic.it/cet/19/77/001.pdf SN - 978-88-95608-74-7 DO - https://doi.org/10.3303/CET1977001 SN - 2283-9216 VL - 77 SP - 1 EP - 6 PB - Italian Association of Chemical Engineering AN - OPUS4-49496 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wiedensohler, A. A1 - Wiesner, A. A1 - Weinhold, K. A1 - Birmili, W. A1 - Herrmann, M. A1 - Merkel, M. A1 - Müller, T. A1 - Pfeifer, S. A1 - Schmidt, A. A1 - Tuch, T. A1 - Velarde, F. A1 - Quincey, P. A1 - Seeger, Stefan A1 - Nowak, A. T1 - Mobility particle size spectrometers: Calibration procedures and measurement uncertainties N2 - Mobility particle size spectrometers (MPSS) belong to the essential instruments in aerosol science that determine the particle number size distribution (PNSD)in the submicrometer size range. Following calibration procedures and target uncertainties against standards and reference instruments are suggested for a complete MPSS quality assurance program: a) calibration of the CPC counting efficiency curve (within 5% for the plateau counting efficiency; within 1 nm for the 50% detection efficiency diameter), b) sizing calibration of the MPSS, using a certified polystyrene latex (PSL) particle size standard at 203 nm (within 3%), c) intercomparison of the PNSD of the MPSS (within 10% and 20% of the dN/dlogDP concentration for the particle size range 20 – 200 nm and 200 to 800 nm, respectively), and d) intercomparison of the integral PNC of the MPSS (within 10%). Furthermore, following measurement uncertainties have been investigated: a) PSL particle size standards in the range from 100-500nm match within 1% after sizing calibration at 203 nm. b) Bipolar diffusion chargers based on the radioactive nuclides Kr85, Am241 and Ni63 and a new ionizer based on corona discharge follow the recommended bipolar charge distribution, while soft X-ray-based charges may alter faster than expected. c) The use of a positive high voltage supply show a 10% better performance than a negative one. d) The intercomparison of the integral PNC of an MPSS against the total number concentration is still within the target uncertainty at an ambient pressure of approximately 500 hPa. KW - Measurement uncertainties KW - Mobility particle size spectrometer (MPPS) KW - Condensation particle counter (CPC) KW - Calibration PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-425060 DO - https://doi.org/10.1080/02786826.2017.1387229 SN - 1521-7388 VL - 52 IS - 2 SP - 146 EP - 164 PB - Tailor & Francis CY - USA AN - OPUS4-42506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Poyraz, Ö. A1 - Schmidt, H. A1 - Seidel, K. A1 - Delißen, Friedmar A1 - Ader, C. A1 - Tenenboim, H. A1 - Goosmann, C. A1 - Laube, B. A1 - Thünemann, Andreas A1 - Zychlinsky, A. A1 - Baldus, M. A1 - Lange, A. A1 - Griesinger, C. A1 - Kolbe, M. T1 - Protein refolding is required for assembly of the type three secretion needle N2 - Pathogenic Gram-negative bacteria use a type three secretion system (TTSS) to deliver virulence factors into host cells. Although the order in which proteins incorporate into the growing TTSS is well described, the underlying assembly mechanisms are still unclear. Here we show that the TTSS needle protomer refolds spontaneously to extend the needle from the distal end. We developed a functional mutant of the needle protomer from Shigella flexneri and Salmonella typhimurium to study its assembly in vitro. We show that the protomer partially refolds from α-helix into β-strand conformation to form the TTSS needle. Reconstitution experiments show that needle growth does not require ATP. Thus, like the structurally related flagellar systems, the needle elongates by subunit polymerization at the distal end but requires protomer refolding. Our studies provide a starting point to understand the molecular assembly mechanisms and the structure of the TTSS at atomic level. PY - 2010 DO - https://doi.org/10.1038/nsmb.1822 SN - 1545-9993 SN - 1545-9985 VL - 17 SP - 788 EP - 792 PB - Nature Publ. Comp. CY - New York, NY, USA AN - OPUS4-21726 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chowdhary, S. A1 - Schmidt, R. F. A1 - Sahoo, A. K. A1 - tom Dieck, T. A1 - Hohmann, T. A1 - Schade, B. A1 - Brademann-Jock, Kerstin A1 - Thünemann, Andreas A1 - Netz, R. R. A1 - Gradzielski, M. A1 - Koksch, B. T1 - Rational design of amphiphilic fluorinated peptides: Evaluation of self-assembly properties and hydrogel formation N2 - Advanced peptide-based nanomaterials composed of self-assembling peptides (SAPs) are of emerging interest in pharmaceutical and biomedical applications. The introduction of fluorine into peptides, in fact, offers unique opportunities to tune their biophysical properties and intermolecular interactions. In particular, the degree of fluorination plays a crucial role in peptide engineering as it can be used to control the characteristics of fluorine-specific interactions and, thus, peptide conformation and self-assembly. Here, we designed and explored a series of amphipathic peptides by incorporating the fluorinated amino acids (2S)-4-monofluoroethylglycine (MfeGly), (2S)-4,4-difluoroethylglycine (DfeGly) and (2S)-4,4,4-trifluoroethylglycine (TfeGly) as hydrophobic components. This approach enabled studying the impact of fluorination on secondary structure formation and peptide self-assembly on a systematic basis. We show that the interplay between polarity and hydrophobicity, both induced differentially by varying degrees of side chain fluorination, does affect peptide folding significantly. A greater degree of fluorination promotes peptide fibrillation and subsequent formation of physical hydrogels in physiological conditions. Molecular simulations revealed the key role played by electrostatically driven intra-chain and inter-chain contact pairs that are modulated by side chain fluorination and give insights into the different self-organization behaviour of selected peptides. Our study provides a systematic report about the distinct features of fluorinated oligomeric peptides with potential applications as peptide-based biomaterials. KW - Small-angle X-ray scattering KW - SAXS KW - Amyloid PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-553504 DO - https://doi.org/10.1039/D2NR01648F SN - 2040-3364 VL - 14 IS - 28 SP - 10176 EP - 10189 PB - Royal Society of Chemistry AN - OPUS4-55350 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schulz, K. A1 - Schmack, R. A1 - Klemm, H. W. A1 - Kabelitz, Anke A1 - Schmidt, T. A1 - Emmerling, Franziska A1 - Kraehnert, R. T1 - Mechanism and kinetics of hematite crystallization in air: Linking bulk and surface models via mesoporous films with defined nanostructure N2 - Iron can form numerous oxides, hydroxides, and oxide−hydroxides. Despite their relevance, many of the transformation processes between these phases are still poorly understood. In particular the crystallization of quasi-amorphous hydroxides and oxide−hydroxides is difficult to assess, since typical diffraction and scattering methods provide only sampleaveraged information about the crystallized phases. We report a new approach for the investigation of the crystallization of oxide−hydroxides. The approach relies on model-type films that comprise a defined homogeneous nanostructure. The nanostructure allows quantitative linking of Information obtained by bulk-averaging diffraction techniques (XRD, SAXS) with locally resolved information, i.e., Domain sizes (SEM, TEM, LEEM) and phase composition (SAED). Using time-resolved imaging and diffraction we deduce mechanism and kinetics for the crystallization of ferrihydrite into hematite. Hematite forms via nucleation of hematite domains and subsequent Domain growth that terminates only upon complete transformation. A Johnson−Mehl−Avrami−Kolmogorov model describes the kinetics over a wide temperature range. The derived understanding enables the first synthesis of ferrihydrite films with ordered mesoporosity and quantitative control over the films’ hematite and ferrihydrite content. KW - Iron oxide KW - Crystallization KW - Mesoporous films KW - Nanostructure PY - 2017 DO - https://doi.org/10.1021/acs.chemmater.6b05185 SN - 0897-4756 SN - 1520-5002 VL - 29 IS - 4 SP - 1724 EP - 1734 AN - OPUS4-39690 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Wilrich, Cordula A1 - Schröder, Volkmar A1 - Brandes, E. A1 - Schmidt, Martin A1 - Wandrey, Peter-Andreas A1 - Mix, K.-H. A1 - Wehrstedt, Klaus-Dieter A1 - Bender, H. A1 - Stephan, U. A1 - Eberz, A. A1 - Steinbach, J. A1 - Stoessel, F. T1 - Plant and process safety - 2. Hazardous materials and process conditions N2 - "Ullmann's Encyclopedia of Industrial Chemistry" is the benchmark reference in chemistry and chemical and life science engineering, covering inorganic and organic chemicals, advanced materials, pharmaceuticals, polymers and plastics, metals and alloys, biotechnology and biotechnological products, food chemistry, process engineering and unit operations, analytical methods, environmental protection, and much more. The present article is part of the topic collection "Environmental Protection and Industrial Safety". It covers plant and process safety, focusing on hazardous materials and process conditions. KW - Flammable gases and vapors KW - Combustibility of liquids KW - Dust explosions KW - Explosive condensed substances KW - Harmful effects of substances KW - Exothermic and pressure-inducing chemical reactions PY - 2012 SN - 978-3-527-30673-2 DO - https://doi.org/10.1002/14356007.q20_q01 SP - 1 EP - 50 PB - Wiley-VCH CY - Weinheim AN - OPUS4-58108 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Everard, C.D. A1 - Schmidt, Martin A1 - McDonnell, K.P. A1 - Finnan, J. T1 - Heating processes during storage of Miscanthus chip piles and numerical simulations to predict self-ignition N2 - Miscanthus x Giganteus (Miscanthus) energy crop was examined at laboratory scale to assess its self-heating and self-ignition risks during storage. Chipped Miscanthus (18 mm) from February and March harvests, in 2012, were assessed as well as ground Miscanthus (3 mm) from the March harvest. February and March crops had moisture contents of 41.6 and 20.2%, respectively. Self-ignition temperatures were independent of moisture although moisture did affect the time from the beginning of storage until storage temperature was reached. Ground Miscanthus had lower self-ignition temperatures than chipped Miscanthus. Isothermal respirometric tests carried out showed increase risk of self-heating in the February crop compared to the March crop due to increased microbial activity. Numerical simulations were used to determine critical enhanced start temperatures, e.g. caused by microbial decomposition, of the stored Miscanthus. Safe storage conditions have been derived from the investigations. The numerical simulations demonstrated that self-ignition was possible in Miscanthus chip piles with a height greater than 6 m if there was significant heat release from microbiological activity. Reliable assessment of self-heating and self-ignition risks in large scale Miscanthus energy crop clamps or piles are required to prevent losses due to decomposition and fire damage. KW - Miscanthus x Giganteus KW - Hot storage test KW - Respirometric rates KW - Self-heating KW - Self-ignition KW - Numerical simulations KW - Biomass storage PY - 2014 DO - https://doi.org/10.1016/j.jlp.2014.06.003 SN - 0950-4230 SN - 1873-3352 VL - 30 SP - 188 EP - 196 PB - Butterworth CY - Guildford, Surrey AN - OPUS4-31149 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bier, A.K. A1 - Bognitzki, M. A1 - Schmidt, A. A1 - Greiner, A. A1 - Gallo, Emanuela A1 - Klack, Patrick A1 - Schartel, Bernhard T1 - Synthesis, properties, and processing of new siloxane-substituted poly(p-xylylene) via CVD N2 - The synthesis of a disiloxane-functionalized [2.2]paracyclophane and its polymerization to the corresponding siloxane-substituted poly(p-xylylene) via chemical vapor deposition (CVD) has been described. Because of the enhanced solubility of the siloxane substituted poly(p-xylylene) analysis of the molecular structure by NMR, molecular weight, and polydispersity by gel permeation chromatography (GPC), and processing by film casting as well as nanofiber formation by electrospinning was possible. Structural isomers were found by NMR which was expected due to the isomeric mixture of the precursor. High molecular weights at moderate polydispersities were found by GPC which was unexpected for a vapor phase deposition polymerization. The amorphous morphology in combination with a low glass transition temperature led to high elongation at break for the siloxane substituted poly(p-xylylene). Significant difference for the wetting versus water was found for as-deposited films, solution cast films, and nanofibers obtained by electrospinning with contact angles up to 135° close to superhydrophobic behavior. KW - Poly(p-xylylene) KW - Siloxane functionalized PPX KW - Chemical vapor deposition KW - Difunctionalized [2.2]paracyclophanes KW - Gorham process PY - 2012 DO - https://doi.org/10.1021/ma2021369 SN - 0024-9297 SN - 1520-5835 VL - 45 IS - 2 SP - 633 EP - 639 PB - American Chemical Society CY - Washington, DC AN - OPUS4-25466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Everard, C.D. A1 - Finnan, J. A1 - McDonnell, K.P. A1 - Schmidt, Martin T1 - Evaluation of self-heating in Miscanthus x giganteus energy crop clamps and the implications for harvesting time N2 - Miscanthus x giganteus energy crop grown in Ireland was harvested on 21st of February and 28th of March 2012 to examine the effects of harvesting time on self-heating during storage of Miscanthus chips in clamps (98 m³) under weather sheltered conditions. There was a relatively large difference in moisture content, of 21.4%, between Miscanthus crop harvested in February and March (41.6 and 20.2%, respectively). Temperature evolution over a storage period of up to 125 days was monitored at different heights and distances from the centre within the clamps. Maximum temperature in the February constructed clamp reached 69 °C compared to 28 °C in the March constructed clamp. Microbial activity was monitored via carbon dioxide and oxygen gas measurements. The high moisture clamp showed higher microbial activity and a volume yield loss of 4.3% due to decomposition in the top section of the clamp. Quality indices post-storage were also assessed. Calorific values from Miscanthus sampled 1 m below the top surface were similar after storage for both February and March constructed clamps, i.e. 18.52 and 18.70 MJ kg-1, respectively. A reliable assessment of self-heating in Miscanthus chip clamps has important consequences for both self-ignition risk and biomass quality. KW - Self-heating KW - Miscanthus x giganteus KW - Biomass storage KW - Self-ignition KW - Biomass quality PY - 2013 DO - https://doi.org/10.1016/j.energy.2013.06.022 SN - 0360-5442 VL - 58 SP - 350 EP - 356 PB - Elsevier CY - Amsterdam [u.a.] AN - OPUS4-29054 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Franco de Carvalho, J. M. A1 - Defàveri, K- A1 - Castro Mendes, J. A1 - Schmidt, Wolfram A1 - Kühne, Hans-Carsten A1 - Fiorotti Peixoto, R. A. T1 - Influence of particle size-designed recycled mineral admixtures on the properties of cement-based composites N2 - In this work, engineered recycled mineral admixtures were obtained from four different industrial residues: basic oxygen furnace slag, iron ore tailings, quartz mining tailings and quartzite mining tailings. The grinding performance was evaluated in two different programs and the characterization included chemical and mineralogical composition, particle morphology, and physical properties. Performance evaluations were carried out in blended pastes and mortars, including flow properties, hydration kinetics, soundness, pozzolanic activity, and compressive strength. Coarser-than-cement admixtures allowed better flow performance, greater dimensional stability and more economical production, while finer-thancementn admixtures improved mechanical performance by both filler effect and cementing activity. KW - Engineered recycled mineral admixtures KW - Rheology KW - Hydration kinetics KW - Basic oxygen furnace slag KW - Iron ore tailings KW - Mining tailings PY - 2021 DO - https://doi.org/10.1016/j.conbuildmat.2020.121640 SN - 0950-0618 VL - 272 SP - 1 EP - 13 PB - Elsevier Ltd. AN - OPUS4-58255 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kim, K.J. A1 - Unger, Wolfgang A1 - Kim, J.W. A1 - Moon, D.W. A1 - Gross, Thomas A1 - Hodoroaba, Vasile-Dan A1 - Schmidt, Dieter A1 - Wirth, Thomas A1 - Jordaan, W. A1 - van Staden, M. A1 - Prins, S. A1 - Zhang, L. A1 - Fujimoto, T. A1 - Song, X.P. A1 - Wang, H. T1 - Inter-laboratory comparison: quantitative surface analysis of thin Fe-Ni alloy films N2 - An international interlaboratory comparison of the measurement capabilities of four National Metrology Institutes (NMIs) and one Designated Institute (DI) in the determination of the chemical composition of thin Fe-Ni alloy films was conducted via a key comparison (K-67) of the Surface Analysis Working Group of the Consultative Committee for Amount of Substance. This comparison was made using XPS (four laboratories) and AES (one laboratory) measurements. The uncertainty budget of the measured chemical composition of a thin alloy film was dominated by the uncertainty of the certified composition of a reference specimen which had been determined by inductively coupled plasma mass spectrometry using the isotope dilution method. Pilot study P-98 showed that the quantification using relative sensitivity factors (RSFs) of Fe and Ni derived from an alloy reference sample results in much more accurate result in comparison to an approach using RSFs derived from pure Fe and Ni films. The individual expanded uncertainties of the participants in the K-67 comparison were found to be between 2.88 and 3.40 atomic %. The uncertainty of the key comparison reference value (KCRV) calculated from individual standard deviations and a coverage factor (k) of 2 was 1.23 atomic %. KW - Quantification KW - Fe-Ni alloy KW - Uncertainty KW - Key comparison KW - Traceability PY - 2012 DO - https://doi.org/10.1002/sia.3795 SN - 0142-2421 SN - 1096-9918 VL - 44 IS - 2 SP - 192 EP - 199 PB - Wiley CY - Chichester AN - OPUS4-24505 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmidt, B.V.K.J. A1 - Fechler, N. A1 - Falkenhagen, Jana A1 - Lutz, J.-F. T1 - Controlled folding of synthetic polymer chains through the formation of positionable covalent bridges N2 - Covalent bridges play a crucial role in the folding process of sequence-defined biopolymers. This feature, however, has not been recreated in synthetic polymers because, apart from some simple regular arrangements (such as block co-polymers), these macromolecules generally do not exhibit a controlled primary structure—that is, it is difficult to predetermine precisely the sequence of their monomers. Herein, we introduce a versatile strategy for preparing foldable linear polymer chains. Well-defined polymers were synthesized by the atom transfer radical polymerization of styrene. The controlled addition of discrete amounts of protected maleimide at precise times during the synthesis enabled the formation of polystyrene chains that contained positionable reactive alkyne functions. Intramolecular reactions between these functions subsequently led to the formation of different types of covalently folded polymer chains. For example, tadpole (P-shaped), pseudocyclic (Q-shaped), bicyclic (8-shaped) and knotted (α-shaped) macromolecular origamis were prepared in a relatively straightforward manner. KW - Copolymerization KW - Chain folding KW - SEC KW - NMR KW - FT-IR KW - LAC KW - MALDI PY - 2011 DO - https://doi.org/10.1038/NCHEM.964 SN - 1755-4330 SN - 1755-4349 VL - 3 SP - 234 EP - 238 PB - Nature Publishing Group CY - London, UK AN - OPUS4-23888 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -