TY - JOUR A1 - Brusamarello-Santos, L. C. C. A1 - Alberton, D. A1 - Valdameri, G. A1 - Camilios-Neto, D. A1 - Covre, R. A1 - Lopes, K. d. P. A1 - Zibetti Tadra-Sfeir, M. A1 - Faoro, H. A1 - Adele Monteiro, R. A1 - Barbosa-Silva, A. A1 - Broughton, William John A1 - Oliveira Pedrosa, F. A1 - Wassem, R. A1 - de Souza, E.M. T1 - Modulation of defence and iron homeostasis genes in rice roots by the diazotrophic endophyte Herbaspirillum seropedicae N2 - Rice is staple food of nearly half the world’s population. Rice yields must therefore increase to feed ever larger populations. By colonising rice and other plants, Herbaspirillum spp. stimulate plant growthand productivity. However the molecular factors involved are largely unknown. To further explore this interaction, the transcription profiles of Nipponbare rice roots inoculated with Herbaspirillum seropedicae were determined by RNA-seq. Mapping the 104 million reads against the Oryza sativa cv. Nipponbare genome produced 65 million unique mapped reads that represented 13,840 transcripts each with at least two-times coverage. About 7.4% (1,014) genes were differentially regulated and of these 255 changed expression levels more than two times. Several of the repressed genes encoded proteins related to plant defence (e.g. a putative probenazole inducible protein), plant disease resistance as well as enzymes involved in flavonoid and isoprenoid synthesis. Genes related to the synthesis and efflux of phytosiderophores (PS) and transport of PS-iron complexes were induced by the bacteria. These data suggest that the bacterium represses the rice defence system while concomitantly activating iron uptake. Transcripts of H. seropedicae were also detected amongst which transcripts of genes involved in nitrogen fixation, cell motility and cell wall synthesis were the most expressed. KW - Herbaspirillum seropedicae KW - Pathogen KW - Rice KW - qPCR KW - Genome PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-490122 DO - https://doi.org/10.1038/s41598-019-45866-w SN - 2045-2322 VL - 9 SP - 10573-1 EP - 10573-15 PB - Nature CY - London AN - OPUS4-49012 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zocca, Andrea A1 - Lüchtenborg, Jörg A1 - Mühler, T. A1 - Wilbig, Janka A1 - Mohr, Gunther A1 - Villatte, T. A1 - Léonard, Fabien A1 - Nolze, Gert A1 - Sparenberg, M. A1 - Melcher, J. A1 - Hilgenberg, Kai A1 - Günster, Jens T1 - Enabling the 3D Printing of Metal Components in μ-Gravity N2 - As humanity contemplates manned missions to Mars, strategies need to be developed for the design and operation of hospitable environments to safely work in space for years. The supply of spare parts for repair and replacement of lost equipment will be one key need, but in-space manufacturing remains the only option for a timely supply. With high flexibility in design and the ability to manufacture ready-to-use components directly from a computeraided model, additive manufacturing (AM) technologies appear extremely attractive. For the manufacturing of metal parts, laser-beam melting is the most widely used AM process. However, the handling of metal powders in the absence of gravity is one prerequisite for its successful application in space. A gas flow throughout the powder bed is successfully applied to compensate for missing gravitational forces in microgravity experiments. This so-called gas-flow-assisted powder deposition is based on a porous Building platform acting as a filter for the fixation of metal particles in a gas flow driven by a pressure difference maintained by a vacuum pump. KW - Additive manufacturing KW - µ-gravity KW - Laser beam melting KW - Parabolic flight KW - 3D printing PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-492190 DO - https://doi.org/10.1002/admt.201900506 SP - 1900506 PB - WILEY-VCH Verlag GmbH AN - OPUS4-49219 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Le, Quynh Hoa A1 - Bäßler, Ralph A1 - Bettge, Dirk T1 - On the corrosion mechanism of CO2 transport pipeline steel caused by condensate: Synergistic effects of NO2 and SO2 N2 - To study the effects of condensed acid liquid, hereafter referred to as condensate, on the CO2 transport pipeline steels, gas mixtures containing a varying concentration of H2O, O2, NO2, and SO2, were proposed and resulted in the condensate containing H2SO4 and HNO3 with the pH ranging from 0.5 to 2.5. By exposing the pipeline steel to the synthetic condensate with different concentration of acidic components, the corrosion kinetic is significantly changed. Reaction kinetic was studied using electrochemical methods coupled with water analysis and compared with surface analysis (scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), and X-ray diffractometry (XRD)) of corroded coupons. The results showed that, although the condensation of NO2 in the form of HNO3 causes faster general corrosion rate, it is the condensation of SO2 in the form of H2SO4 or the combination of SO2 and NO2 that may cause much more severe problems in the form of localized and pitting corrosions. The resulting corrosion forms were depended on the chemical nature of acids and their concentration at the same investigated pH. The effects of changing CO2 flow rate and renewing condensate on pitting corrosion were further studied. KW - Carbon capture, utilization and storage technology KW - CCUS KW - Corrosion KW - Condensate KW - Electrochemical characterisation KW - Pitting corrosion KW - Impurities KW - Carbon steel PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-473685 UR - https://www.mdpi.com/1996-1944/12/3/364 DO - https://doi.org/10.3390/ma12030364 SN - 1996-1944 VL - 12 IS - 3 SP - 364, 1 EP - 17 PB - MDPI CY - Basel AN - OPUS4-47368 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hampel, Marco A1 - Schenderlein, Matthias A1 - Schary, Christian A1 - Dimper, Matthias A1 - Özcan Sandikcioglu, Özlem T1 - Efficient detection of localized corrosion processes on stainless steel by means of scanning electrochemical microscopy (SECM) using a multi-electrode approach N2 - High resolution analysis of corrosion processes on stainless steels is a challenging task. The application of local electrochemical techniques such as scanning electrochemical microscopy (SECM) has opened new possibilities for the detection of corrosion products and activity on metallic surfaces. However, due to its stochastic nature, the analysis of pitting corrosion requires being at the right place at the right time. Scanning over large areas at a high resolution not only leads to long scan durations but also leaves many short-lived processes undetected. In this paper we present the combined automated operation of SECM and wire multi-electrodes connected to a multi-electrode analyzer (MMA). The inter-electrode currents between 25 wire electrodes connected via zero resistance ammeters (ZRA) are measured by the MMA at open circuit potential (OCP) and the electrodes reporting anodic currents are detected automatically to be analyzed by means of SECM. The results demonstrate the successful application of this methodology for the detection of unstable and stable pitting processes on 304 stainless steel in a corrosive aqueous environment. KW - Scanning electrochemical microscope (SECM) KW - Localised corrosion KW - Corrosion monitoring PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-478646 DO - https://doi.org/10.1016/j.elecom.2019.02.019 VL - 101 SP - 52 EP - 55 PB - Elsevier B.V. AN - OPUS4-47864 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Aristia, Gabriela A1 - Le, Quynh Hoa A1 - Bäßler, Ralph T1 - Corrosion of Carbon Steel in Artificial Geothermal Brine: Influence of Carbon Dioxide at 70 °C and 150 °C N2 - This study focuses on the corrosion mechanism of carbon steel exposed to an artificial geothermal brine influenced by carbon dioxide (CO2) gas. The tested brine simulates a geothermal source in Sibayak, Indonesia, containing 1500 mg/L of Cl-, 20 mg/L of SO4 2-, and 15 mg/L of HCO3-with pH 4. To reveal the temperature effect on the corrosion behavior of carbon steel, exposure and electrochemical tests were carried out at 70 °C and 150 °C. Surface analysis of corroded specimens showed localized corrosion at both temperatures, despite the formation of corrosion products on the surface. After 7 days at 150 °C, SEM images showed the formation of an adherent, dense, and crystalline FeCO3 layer. Whereas at 70 °C, the corrosion products consisted of chukanovite (Fe2(OH)2CO3) and siderite (FeCO3), which are less dense and less protective than that at 150 °C. Control experiments under Ar-environment were used to investigate the corrosive effect of CO2. Free corrosion potential (Ecorr) and electrochemical impedance spectroscopy (EIS) confirm that at both temperatures, the corrosive effect of CO2 was more significant compared to that measured in the Ar-containing solution. In terms of temperature effect, carbon steel remained active at 70 °C, while at 150 °C, it became passive due to the FeCO3 formation. These results suggest that carbon steel is more susceptible to corrosion at the near ground surface of a geothermal well, whereas at a deeper well with a higher temperature, there is a possible risk of scaling (FeCO3 layer). A longer exposure test at 150 °C with a stagnant solution for 28 days, however, showed the unstable FeCO3 layer and therefore a deeper localized corrosion compared to that of seven-day exposed specimens. KW - Carbon steel KW - CO2 KW - Corrosion KW - Electrochemical impedance spectroscopy KW - Geothermal PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-498168 DO - https://doi.org/10.3390/ma12223801 SN - 1996-1944 VL - 12 IS - 22 SP - 3801-1 EP - 20 PB - MDPI CY - Basel AN - OPUS4-49816 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lu, Z. A1 - Haist, M. A1 - Ivanov, D. A1 - Jakob, C. A1 - Jansen, D. A1 - Leinitz, Sarah A1 - Link, J. A1 - Mechtcherine, V. A1 - Neubauer, J. A1 - Plank, J. A1 - Schmidt, Wolfram A1 - Schilde, C. A1 - Schröfl, C. A1 - Sowoidnich, T. A1 - Stephan, D. T1 - Characterization data of reference cement CEM I 42.5 R used for Priority Program DFG SPP 2005 “Opus Fluidum Futurum - Rheology of reactive, multiscale, multiphase construction materials” N2 - A thorough characterization of starting materials is the precondition for further research, especially for cement, which contains various phases and presents quite a complex material for fundamental scientific investigation. In the paper at hand, the characterization data of the reference cement CEM I 42.5 R used within the priority program 2005 of the German Research Foundation (DFG SPP 2005) are presented from the aspects of chemical and mineralogical compositions as well as physical and chemical properties. The data were collected based on tests conducted by nine research groups involved in this cooperative program. For all data received, the mean values and the corresponding errors were calculated. The results shall be used for the ongoing research within the priority program. KW - Portland cement KW - Characterization KW - DFG SPP 2005 PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-500849 DO - https://doi.org/10.1016/j.dib.2019.104699 SN - 2352-3409 VL - 27 SP - 104699 PB - Elsevier Inc. AN - OPUS4-50084 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Topolniak, Ievgeniia A1 - Hodoroaba, Vasile-Dan A1 - Pfeifer, Dietmar A1 - Braun, Ulrike A1 - Sturm, Heinz T1 - Boehmite Nanofillers in Epoxy Oligosiloxane Resins: Influencing the Curing Process by Complex Physical and Chemical Interactions N2 - In this work, a novel boehmite (BA)-embedded organic/inorganic nanocomposite coating based on cycloaliphatic epoxy oligosiloxane (CEOS) resin was fabricated applying UV-induced cationic polymerization. The main changes of the material behavior caused by the nanofiller were investigated with regard to its photocuring kinetics, thermal stability, and glass transition. The role of the particle surface was of particular interest, thus, unmodified nanoparticles (HP14) and particles modified with p-toluenesulfonic acid (OS1) were incorporated into a CEOS matrix in the concentration range of 1–10 wt.%. Resulting nanocomposites exhibited improved thermal properties, with the glass transition temperature (Tg) being shifted from 30 °C for unfilled CEOS to 54 °C (2 wt.% HP14) and 73 °C (2 wt.% OS1) for filled CEOS. Additionally, TGA analysis showed increased thermal stability of samples filled with nanoparticles. An attractive interaction between boehmite and CEOS matrix influenced the curing. Real-time infrared spectroscopy (RT-IR) experiments demonstrated that the epoxide conversion rate of nanocomposites was slightly increased compared to neat resin. The beneficial role of the BA can be explained by the participation of hydroxyl groups at the particle surface in photopolymerization processes and by the complementary contribution of p-toluenesulfonic acid surface modifier and water molecules introduced into the system with nanoparticles. KW - Real-time infrared spectroscopy KW - Boehmite KW - Nanocomposite KW - Cationic photocuring KW - Cycloaliphatic epoxy oligosiloxane KW - Epoxy conversion degree PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-479628 DO - https://doi.org/10.3390/ma12091513 VL - 12 IS - 9 SP - 1513 PB - MDPI AN - OPUS4-47962 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ghasem Zadeh Khorasani, Media A1 - Silbernagl, Dorothee A1 - Szymoniak, Paulina A1 - Hodoroaba, Vasile-Dan A1 - Sturm, Heinz T1 - The effect of boehmite nanoparticles (gamma‐AlOOH) on nanomechanical and thermomechanical properties correlated to crosslinking density of epoxy N2 - We show that complex physical and chemical interactions between boehmite nanoparticles and epoxy drastically affect matrix properties, which in the future will provide tuning of material properties for further optimization in applications from automotive to aerospace. We utilize intermodulation atomic force microscopy (ImAFM) for probing local stiffness of both particles and polymer matrix. Stiff particles are expected to increase total stiffness of nanocomposites and the stiffness of polymer should remain unchanged. However, ImAFM revealed that stiffness of matrix in epoxy/boehmite nanocomposite is significantly higher than unfilled epoxy. The stiffening effect of the boehmite on epoxy also depends on the particle concentration. To understand the mechanism behind property alteration induced by boehmite nanoparticles, network architecture is investigated using dynamic mechanical thermal analysis (DMTA). It was revealed that although with 15 wt% boehmite nanoparticles the modulus at glassy state increases, crosslinking density of epoxy for this composition is drastically low. KW - Crosslinking density KW - Epoxy KW - Intermodulation KW - Atomic force microscopy KW - Nanomechanical properties KW - Boehmite nanoparticles PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-476050 DO - https://doi.org/10.1016/j.polymer.2018.12.054 SN - 0032-3861 SN - 1873-2291 VL - 164 SP - 174 EP - 182 PB - Elsevier AN - OPUS4-47605 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Vallée, A. A1 - Bally, P. A1 - Bruel, C. A1 - Chandat, L. A1 - Choquer, M. A1 - Dieryckx, C. A1 - Dupuy, J.W. A1 - Kaiser, S. A1 - Latorse, M.-P. A1 - Loisel, E. A1 - Mey, G. A1 - Morgant, G. A1 - Rascle, C. A1 - Schumacher, Julia A1 - Simon, A. A1 - Souibgui, E. A1 - Viaud, M. A1 - Villalba, F. A1 - Poussereau, N. T1 - A similar secretome disturbance as a hallmark of non-pathogenic Botrytis cinerea ATMT-mutants? N2 - The gray mold fungus Botrytis cinerea is a necrotrophic pathogen able to infect hundreds of host plants, including high-value crops such as grapevine, strawberry and tomato. In order to decipher its infectious strategy, a library of 2,144 mutants was generated by random insertional mutagenesis using Agrobacterium tumefaciensmediated transformation (ATMT). Twelve mutants exhibiting total loss of virulence toward different host plants were chosen for detailed analyses. Their molecular characterization revealed a single T-DNA insertion in different loci. Using a proteomics approach, the secretome of four of these strains was compared to that of the parental strain and a common profile of reduced lytic enzymes was recorded. Significant variations in this profile, notably deficiencies in the secretion of proteases and hemicellulases, were observed and validated by biochemical tests. They were also a hallmark of the remaining eight non-pathogenic strains, suggesting the importance of these secreted Proteins in the infection process. In the twelve non-pathogenic mutants, the Differentiation of infection cushions was also impaired, suggesting a link between the Penetration structures and the secretion of proteins involved in the virulence of the pathogen. KW - Fungus KW - Plant pathogen KW - Virulence PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-502710 DO - https://doi.org/10.3389/fmicb.2019.02829 SN - 1664-302X VL - 10 SP - Article 2829 PB - Frontiers Media CY - Lausanne AN - OPUS4-50271 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meyer, A. A1 - Weidner, Steffen A1 - Kricheldorf, H. T1 - Stereocomplexation of cyclic polylactides with each other and with linear poly(L-lactide)s N2 - Two kinds of cyclic poly(D- and L-lactide)s were synthesized, namely CI labeled samples mainly consisting of even-numbered cycles with low dispersity and CII, CIII or CIV-labeled ones consisting of equal amounts of even and odd-numbered cycles with high dispersity and igher molecular weights (Mw up to 300 000). Furthermore, linear poly L-lactide)s were prepared by initiation with ethanol and in both series the molecular weight was varied. The formation of stereocomplexes from cyclic poly(D-lactide)s and all kinds of poly L-lactide)s was performed in dichloromethane/toluene mixtures. The stereocomplexes crystallized from the reaction mixture were characterized in the virgin state and after annealing at 205 °C. Stereocomplexes free of stereohomopolymers with crystallinities up to 80% were obtained from all experiments in yields ranging from 60 to 80%. Despite the high annealing temperature (maintained for 1 h), little transesterification was observed and the crystallinity slightly increased. KW - Polylactide KW - MALDI-TOF MS KW - Stereocomplex KW - Cyclic PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-496693 DO - https://doi.org/10.1039/c9py01236b VL - 10 SP - 6191 EP - 6199 PB - Royal Society for Chemistry AN - OPUS4-49669 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. R. A1 - Weidner, Steffen A1 - Scheliga, F. T1 - Synthesis of cyclic poly(l-lactide) catalyzed by Bismuth salicylates-A combination of two drugs N2 - l‐lactide was polymerized in bulk at 160 or 180°C with mixtures of bismuth subsalicylate (BiSub) and salicylic (SA) as catalysts. The SA/Bi ratio and the monomer/Bi ratio were varied. The highest molecular weights (weight average, Mw) were achieved at a SA/Bi ratio of 1/1 (Mw up to 92 000 g mol−1). l‐Lactide was also polymerized with combinations of BiSub and silylated SA, and Mw values up to 120 000 g mol−1 were achieved at 180°C. MALDI‐TOF mass spectrometry and Mark‐Houwink‐Sakurada measurements proved that under optimized reaction conditions the resulting polylactides consist of cycles. KW - Polylactide KW - MALDI-TOF MS KW - Cyclization KW - Catalyst KW - Salicylate PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-488622 DO - https://doi.org/10.1002/pola.29473 SN - 0887-624X SN - 1099-0518 SP - 29473 PB - Wiley AN - OPUS4-48862 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Shamsuddoha, Md A1 - Hüsken, Götz A1 - Schmidt, Wolfram A1 - Kühne, Hans-Carsten A1 - Baeßler, Matthias T1 - Superplasticizer and Shrinkage Reducing Admixture Dosages for Microfine Cement in Grout Systems N2 - Grouts have numerous applications including crack repair as maintenance in construction industries. Microfine cements are intensively used for high strength mortar and grout products. They are ideal for injection grouting in structural repair. Such grouts should have suitable rheological properties to be injectable, especially those used in repair and rehabilitation. The use of superplasticizers (SP) in these products is thus becoming increasingly crucial to achieve favorable workability and viscosity properties. A difficulty in such grouts is the plastic shrinkage due to finer particles used. It is thus necessary to determine optimum SP and shrinkage reducing admixture (SRA) dosages for a microfine cement based grout. In this study, a saturation dosage was decided from two Polycarboxylate ether (PCE) based SPs in relation to neat cement using slump flow and rheological parameters. A range of grout mixtures was formulated containing micro silica (MS) and fly ash (FA), and tested for suitable rheological and mechanical parameters. Based on the results, a grout mixture with MS and FA was selected to determine optimum SRA content. According to the results, a SP dosage of 3% by weight of neat cement is sufficient to achieve saturation. The grout material including MS and FA can produce comparable properties to neat cement grout. MS is found to improve compressive strength within the range considered, whereas a higher FA content provides favourable rheological properties. Finally, a SRA dosage of 4%, which could reduce the shrinkage by about 43% after 28d days, is determined for the grout system. T2 - 2nd International Conference on Building Materials and Materials Engineering (ICBMM 2018) CY - University of Lisbon, Portugal DA - 26.09.2018 KW - Grout KW - Microfine Cement KW - Superplasticizer KW - Supplementary Cementitious Materials KW - Shrinkage Reducing Admixture PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-478319 DO - https://doi.org/10.1051/matecconf/201927801001 VL - 278 SP - Article Number 01001 PB - EDP Sciences AN - OPUS4-47831 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ghasem Zadeh Khorasani, Media A1 - Silbernagl, Dorothee A1 - Platz, D. A1 - Sturm, Heinz T1 - Insights into Nano-Scale Physical and Mechanical Properties of Epoxy/Boehmite Nanocomposite Using Different AFM Modes N2 - Understanding the interaction between nanoparticles and the matrix and the properties of interphase is crucial to predict the macroscopic properties of a nanocomposite system. Here, we investigate the interaction between boehmite nanoparticles (BNPs) and epoxy using different atomic force microscopy (AFM) approaches. We demonstrate benefits of using multifrequency intermodulation AFM (ImAFM) to obtain information about conservative, dissipative and van der Waals tip-surface forces and probing local properties of nanoparticles, matrix and the interphase. We utilize scanning kelvin probe microscopy (SKPM) to probe surface potential as a tool to visualize material contrast with a physical parameter, which is independent from the mechanics of the surface. Combining the information from ImAFM stiffness and SKPM surface potential results in a precise characterization of interfacial region, demonstrating that the interphase is softer than epoxy and boehmite nanoparticles. Further, we investigated the effect of boehmite nanoparticles on the bulk properties of epoxy matrix. ImAFM stiffness maps revealed the significant stiffening effect of boehmite nanoparticles on anhydride-cured epoxy matrix. The energy Dissipation of epoxy Matrix locally measured by ImAFM shows a considerable increase compared to that of neat epoxy. These measurements suggest a substantial alteration of epoxy structure induced by the presence of boehmite. KW - Nanomechanics KW - Intermodulation-AFM KW - Interphase KW - Boehmite KW - Epoxy PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-476040 DO - https://doi.org/10.3390/polym11020235 SN - 2073-4360 VL - 11 IS - 2 SP - 235, 1 EP - 19 PB - MDPI AN - OPUS4-47604 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Falk, Florian A1 - Menneken, M. A1 - Stephan-Scherb, Christiane T1 - Real-time observation of high- temperature gas corrosion in dry and wet SO2-containing atmosphere N2 - Sulfur and water have a fundamental impact on the corrosion rate and potential failure of materials. It is therefore necessary to understand the mechanisms, rates, and potential means of transport, as well as the reactions of these elements with an alloy. This paper investigates the effect of water vapor in the initial stages of SO2 corrosion of an Fe-9Cr-0.5Mn model alloy at 650°C in situ under laboratory conditions using energy-dispersive x-ray diffraction analysis. Two separate experiments were run, one with a 99.5% Ar + 0.5% SO2 atmosphere and one with a 69.5% Ar + 0.5% SO2 + 30% H2O atmosphere. With a wet atmosphere, the alloy formed a scale with decreasing oxygen content towards the scale–alloy interface. Sulfides were identified above and below a (Fe, Cr)3O4 layer in the inner corrosion zone. In contrast to this, the overall scale growth was slower in a dry SO2 atmosphere. KW - Early oxidation KW - Early sulfidation KW - Ferritic steels PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-472844 UR - https://link.springer.com/article/10.1007/s11837-019-03335-9#enumeration DO - https://doi.org/10.1007/s11837-019-03335-9 SN - 1047-4838 SN - 1543-1851 VL - 71 SP - 1 EP - 6 PB - Springer CY - New York AN - OPUS4-47284 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - An, Biwen Annie A1 - Shen, Y. A1 - Voordouw, J. A1 - Voordouw, G. T1 - Halophilic methylotrophic methanogens may contribute to the high ammonium concentrations found in shale oil and shale gas reservoirs N2 - Flow-back and produced waters from shale gas and shale oil fields contain high ammonium, which can be formed by methanogenic degradation of methylamines into methane and ammonium. Methylamines are added to fracturing fluid to prevent clay swelling or can originate from metabolism of the osmolyte triglycinebetaine (GB). We analyzed field samples from a shale gas reservoir in the Duvernay Formation and from a shale oil reservoir in the Bakken formation in Canada to determine the origin of high ammonium. Fresh waters used to make fracturing fluid, early flow-back waters, and late flow back waters from the shale gas reservoir had increasing salinity of 0.01, 0.58, and 2.66 Meq of NaCl, respectively. Microbial community analyses reflected this fresh water to saline transition with halophilic taxa including Halomonas, Halanaerobium, and Methanohalophilus being increasingly present. Early and late flow-back waters had high ammonium concentrations of 32 and 15 mM, respectively. Such high concentrations had also been found in the Bakken produced waters. Enrichment cultures of Bakken produced waters in medium containing mono, di-, or trimethylamine, or triglycinebetaine (GB) converted these substrates into ammonium (up to 20 mM) and methane. The methylotrophic methanogen Methanohalophilus, which uses methylamines for its energy metabolism and uses GB as an osmolyte, was a dominant community member in these enrichments. Halanaerobium was also a dominant community member that metabolizes GB into trimethylamine, which is then metabolized further by Methanohalophilus. However, the micromolar concentrations of GB measured in shale reservoirs make them an unlikely source for the 1,000-fold higher ammonium concentrations in flow-back waters. This ammonium either originates directly from the reservoir or is formed from methylamines, which originate from the reservoir, or are added during the hydraulic fracturing process. These methylamines are then converted into ammonium and methane by halophilic methylotrophic methanogens, such as Methanohalophilus, present in flow-back waters. KW - Methanogen KW - Oil and gas industry KW - Shale KW - Halophile KW - Corrosion PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-474982 DO - https://doi.org/10.3389/fenrg.2019.00023 SN - 2296-598X VL - 7 SP - 1 EP - 13 PB - Frontiers Media CY - Lausanne AN - OPUS4-47498 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liehr, Sascha A1 - Jäger, L. A. A1 - Karapanagiotis, Christos A1 - Münzenberger, Sven A1 - Kowarik, Stefan T1 - Real-time dynamic strain sensing in optical fibers using artificial neural networks N2 - We propose to use artificial neural networks (ANNs) for raw measurement data interpolation and signal shift computation and to demonstrate advantages for wavelength-scanning coherent optical time domain reflectometry (WS-COTDR) and dynamic strain distribution measurement along optical fibers. The ANNs are trained with synthetic data to predict signal shifts from wavelength scans. Domain adaptation to measurement data is achieved, and standard correlation algorithms are outperformed. First and foremost, the ANN reduces the data analysis time by more than two orders of magnitude, making it possible for the first time to predict strain in real-time applications using the WS-COTDR approach. Further, strain noise and linearity of the sensor response are improved, resulting in more accurate measurements. ANNs also perform better for low signal-to-noise measurement data, for a reduced length of correlation input (i.e., extended distance range), and for coarser sampling settings (i.e., extended strain scanning range). The general applicability is demonstrated for distributed measurement of ground movement along a dark fiber in a telecom cable. The presented ANN-based techniques can be employed to improve the performance of a wide range of correlation or interpolation problems in fiber sensing data analysis and beyond. KW - Distributed vibration sensing KW - Distributed acoustic sensing KW - Coherent optical time domain reflectometry KW - Optical fiber sensor KW - Artificial neural network KW - Real time measurement KW - Distributed strain sensing PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-474832 UR - https://www.osapublishing.org/oe/abstract.cfm?uri=oe-27-5-7405 DO - https://doi.org/10.1364/OE.27.007405 SN - 1094-4087 VL - 27 IS - 5 SP - 7405 EP - 7425 PB - Optical Society of America AN - OPUS4-47483 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Palkowski, Carsten A1 - Zottl, A. A1 - Malenkovic, I. A1 - Simo, Anne T1 - Fixing efficiency values by unfixing compressor speed: Dynamic test method for heat pumps N2 - The growing market penetration of heat pumps indicates the need for a performance test method that better reflects the dynamic behavior of heat pumps. In this contribution, we developed and implemented a dynamic test method for the evaluation of the seasonal performance of heat pumps by means of laboratory testing. Current standards force the heat pump control inactive by fixing the compressor speed. In contrast, during dynamic testing, the compressor runs unfixed while the heat pump is subjected to a temperature profile. The profile consists of the different outdoor temperatures of a typical heating season based on the average European climate and also includes temperature changes to reflect the dynamic behavior of the heat pump. The seasonal performance can be directly obtained from the measured heating energy and electricity consumption making subsequent data interpolation and recalculation with correction factors obsolete. The method delivers results with high precision and high reproducibility and could be an appropriate method for a fair rating of heat pumps. KW - Heat pump KW - Dynamic test method KW - Seasonal performance factor KW - Variable frequency drive KW - Energy label PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-476944 DO - https://doi.org/10.3390/en12061045 SN - 1996-1073 VL - 12 IS - 6 SP - 1045, 1 EP - 16 PB - MDPI CY - Basel, Switzerland AN - OPUS4-47694 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Palkowski, Carsten A1 - Schwarzenberg, S. A1 - Simo, Anne T1 - Seasonal cooling performance of air conditioners: The importance of independent test procedures used for MEPS and labels N2 - Minimum energy performance standards and labels are commonly used tools to reduce the household energy use thus mitigating greenhouse gas emissions. However, the technical foundation for minimum energy performance standards and labels are test procedures for rating and testing of appliances. To de- termine the seasonal cooling performance of air conditioners, the current test standards require fixing of the compressor speed of the units to achieve steady-state conditions; this way of operation, how- ever, differs from real-life use. To make the seasonal cooling performance testing better reflect the real use conditions, this study proposes a compensation method which can be conducted independently from manufacturer data and still allows modulation of the tested units. Our results show that the tested units behave differently under part-load conditions, which results in a lower energy efficiency rating for some of the tested devices. KW - Air conditioner KW - Independent test method KW - Real use behavior KW - Seasonal energy efficiency ratio KW - Minimum energy performance standards KW - Energy label PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-485813 DO - https://doi.org/10.1016/j.ijrefrig.2019.05.021 SN - 0140-7007 VL - 104 SP - 417 EP - 425 PB - Elsevier AN - OPUS4-48581 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Knieschewski, Arno A1 - Stamminger, R. A1 - Simo, Anne T1 - Cost analysis of screening methods to find non-compliant models using the example of tumble dryers N2 - The European energy label was established to reduce energy consumption in Europe. All classes and values on the energy label are stated by the supplier. The task of market surveillance is to ensure correct labels and to validate their values through compliance tests. However, this can only be done for a small fraction of all models on the market, since physical tests are expensive. Screening methods can be used to narrow down the number of critical products before compliance tests are done to decrease the costs of finding non-compliant models. This study shows a mathematical approach to analyze the cost benefits of screening methods to find non-compliant models. Furthermore, the analysis presented has been applied to 18 screening methods for tumble dryers. The performance test for tumble dryers consists of seven test runs. All screening methods evaluated are composed of a reduced number of test runs. The most efficient screening method reduces the surveillance costs by 40 %. KW - Screening method KW - Market surveillance KW - Tumble dryer KW - Energy label PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-486762 DO - https://doi.org/10.1007/s12053-019-09805-y SN - 1570-646X SN - 1570-6478 VL - 12 IS - 7 SP - 1707 EP - 1715 PB - Springer CY - Dordrecht AN - OPUS4-48676 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Haustein, T. A1 - Busweiler, Sabine A1 - Haustein, V. A1 - von Laar, C. A1 - Plarre, Rüdiger T1 - Laboratory breeding of Korynetes caeruleus (Coleoptera: Cleridae) for the biological of Anobium punctatum) (Coleoptera, Ptinidae) N2 - Larvae and adults of Korynetes caeruleus (de Geer 1775) (Coleoptera: Cleridae) were collected from old churches and reared in the laboratory on Anobium punctatum (de Geer 1774) (Coleoptera: Ptinidae). Breeding success of K. caeruleus was low, but basic parameters of this species’ developmental cycle were identifi ed. At 21°C and 75% relative humidity and a fourmonth cold period at 4°C, the development of K. caeruleus from egg to adult appearance lasted 2 years. The pupal stage may be reached and completed after one and a half years. Feeding on larvae of A. punctatum by larvae of K. caeruleus was observed and consisted of a combination of sucking haemolymph and consuming body parts. The sickle-like mandibles of larvae of K. caeruleus penetrate the cuticle of prey larvae; this is followed by pumping and sucking body movements. Adult beetles of A. punctatum were not attacked by K. caeruleus larvae. Feeding behaviour of adult K. caeruleus was not investigated. KW - Cultural heritage KW - Coleoptera KW - Korynetes caeruleus KW - Cleridae KW - Ptinidae KW - Anobium punctatum KW - Biological pest control KW - Life history data KW - Laboratory breeding KW - Wood protection PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-494999 DO - https://doi.org/10.14411/eje.2019.038 SN - 1802-8829 VL - 116 SP - 362 EP - 371 PB - České Budějovice AN - OPUS4-49499 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kindrachuk, Vitaliy A1 - Fedelich, Bernard A1 - Rehmer, Birgit A1 - Peter, Frauke T1 - Computational methods for lifetime prediction of metallic components under high-temperature fatigue N2 - The issue of service life prediction of hot metallic components subjected to cyclic loadings is addressed. Two classes of lifetime models are considered, namely, the incremental lifetime rules and the parametric models governed by the fracture mechanics concept. Examples of application to an austenitic cast iron are presented. In addition, computational techniques to accelerate the time integration of the incremental models throughout the fatigue loading history are discussed. They efficiently solve problems where a stabilized response of a component is not observed, for example due to the plastic strain which is no longer completely reversed and accumulates throughout the fatigue history. The performance of such an accelerated Integration technique is demonstrated for a finite element simulation of a viscoplastic solid under repeating loading–unloading cycles. KW - Fatigue KW - Incremental lifetime models KW - Finite element analysis PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-481215 UR - https://www.mdpi.com/2075-4701/9/4/390 DO - https://doi.org/10.3390/met9040390 SN - 2075-4701 VL - 9 IS - 4 SP - 390, 1 EP - 24 PB - mdpi CY - Basel, Switzerland AN - OPUS4-48121 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wegner, Karl David A1 - Dussert, F. A1 - Truffier-Boutry, D. A1 - Benayad, A. A1 - Beal, D. A1 - Mattera, L. A1 - Ling, W. L. A1 - Carrière, M. A1 - Reiss, P. T1 - Influence of the Core/Shell Structure of Indium Phosphide Based Quantum Dots on Their Photostability and Cytotoxicity N2 - With the goal to improve their photostability, InP-based QDs are passivated with three types of inorganic shells, namely (i) a gradient ZnSexS1−x shell, (ii) an additional ZnS shell on top of the gradient shell with two different thicknesses (core/shell/shell, CSS), (iii) an alumina coating on top of ZnS. All three systems have photoluminescence Quantum yields (PLQY) > 50%and similar PL decay times (64–67 ns). To assess their photostability they are incorporated into a transparent poly (methyl methacrylate) (PMMA) matrix and exposed to continuous irradiation with simulated sunlight in a climate chamber. The alumina coated core/shell system exhibits the highest stability in terms of PLQY Retention as well as the lowest shift of the PL maximum and lowest increase of the PL linewidth, followed by the CSS QDs and finally the gradient shell system. By means of XPS studies we identify the degradation of the ZnS outer layer and concomitant xidation of the emissive InZnP core as the main origins of degradation in the gradient structure. These modifications do not occur in the case of the alumina-capped sample, which exhibits excellent chemical stability. The gradient shell and CSS systems could be transferred to the aqueous phase using surface ligand exchange with penicillamine. Cytotoxicity studies on human primary keratinocytes revealed that exposure for 24 h to 6.25–100 nM of QDs did not affect cell viability. However, a trend toward reduced cell proliferation is observed for higher concentrations of gradient shell and CSS QDs with a thin ZnS shell, while CSS QDs with a thicker ZnS shell do not exhibit any impact. KW - Indium phosphide KW - Quantum dots KW - Cytotoxicity KW - Photostability PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-494249 DO - https://doi.org/10.3389/fchem.2019.00466 VL - 7 SP - Article Number: 466 PB - Frontiers Media SA AN - OPUS4-49424 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Otto, Peter A1 - de Lorenzis, L. A1 - Unger, Jörg F. T1 - Explicit dynamics in impact simulation using a NURBS contact interface N2 - In this paper, the impact problem and the subsequent wave Propagation are considered. For the contact discretization an intermediate non-uniform rational B-spline (NURBS) layer is added between the contacting finite element bodies, which allows a smooth contact formulation and efficient element-based integration. The impact event is ill-posed and requires a regularization to avoid propagating stress oscillations. A nonlinear mesh-dependent penalty regularization is used, where the stiffness of the penalty regularization increases upon mesh refinement. Explicit time integration methods are well suited for wave propagation problems, but are efficient only for diagonal mass matrices. Using a spectral element discretization in combination with a NURBS contact layer the bulk part of the mass matrix is diagonal. KW - Explicit dynamics KW - Impact simulation KW - Isogeometric analysis KW - mortar method KW - spectral elements PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506041 DO - https://doi.org/10.1002/nme.6264 VL - 121 IS - 6 SP - 1248 EP - 1267 PB - Wiley Online Libary AN - OPUS4-50604 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zinke, R. A1 - Virothi, N. A1 - Köhler, F. A1 - Klippel, A. A1 - Schalau, Sebastian A1 - Krause, U. T1 - Experimental measurement of initial evaporation mass flows from gasoline spills and comparison with empirical models N2 - In this paper, we investigate the evaporation mass flow originating from spills of gas-oline. Large spills of gasoline may form during partial or complete roof sinkings or inthe case of perforations at various deck fittings at external floating roof tanks usedfor the storage. Additionally, spills may form in the retention area in the case of leak-ages at pipes or at the hull. The aim is to predict the order of magnitude of real-scaleevaporation mass flow. The determined evaporation mass flows will be used in arelated project as input values for subsequent dispersion modeling in the vicinity ofthe tanks. This is relevant for questions of fire and explosion protection as well as forenvironmental protection aspects in tank farms or refineries, which use externalfloating roof tanks. The measurements presented in this paper were compared withpredictions by empirical models and investigations of evaporations from small floorspills, round-bottom flask, or from Petri dishes published in the literature. The maingoal of this paper is to test the applicability of empirical models to provide reasonableevaporation mass flows as input for CFD dispersion simulations. KW - Spill evaporation PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-504322 DO - https://doi.org/10.1002/prs.12128 VL - 39 IS - 3 SP - e12128 PB - Wiley Online Libary AN - OPUS4-50432 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kapa, Thomas A1 - Schreier, Andy A1 - Krebber, Katerina T1 - A 100-km BOFDA Assisted by First-Order Bi-Directional Raman Amplification N2 - We present, to our knowledge for the first time, a 100-km Brillouin Optical Frequency-Domain Analysis (BOFDA) employing a 200-km fiber loop. Compared to our previous publication, enhanced sensor length, sensor accuracy and spatial resolution are presented. The performance improvements are achieved by applying distributed Raman amplification (DRA) and a digital high-pass filter. We report on temperature measurements over sensing distances of 75 km and 100 km both with a 12.5-m spatial resolution. Temperature changes of 5 °C have been measured along 75 km sensing fiber. A temperature change of 30 °C has been detected at 99.5 km. KW - Distributed sensing KW - Fiber optics sensors KW - Stimulated Brillouin scattering PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-476577 DO - https://doi.org/10.3390/s19071527 SN - 1424-8220 VL - 19 IS - 7 SP - 1527, 1 EP - 9 PB - MDPI CY - Basel, Switzerland AN - OPUS4-47657 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Teng, Jun A1 - Tang, De-Hui A1 - Zhang, Xiao A1 - Hu, Wei-Hua A1 - Said, Samir A1 - Rohrmann, Rolf G. T1 - Automated modal analysis for tracking structural change during construction and operation phases N2 - The automated modal analysis (AMA) technique has attracted significant interest over the last few years, because it can track variations in modal parameters and has the potential to detect structural changes. In this paper, an improved density-based spatial clustering of applications with noise (DBSCAN) is introduced to clean the abnormal poles in a stabilization diagram. Moreover, the optimal system model order is also discussed to obtain more stable poles. A numerical Simulation and a full-scale experiment of an arch bridge are carried out to validate the effectiveness of the proposed algorithm. Subsequently, the continuous dynamic monitoring system of the bridge and the proposed algorithm are implemented to track the structural changes during the construction phase. Finally, the artificial neural network (ANN) is used to remove the temperature effect on modal frequencies so that a health index can be constructed under operational conditions. KW - Automated Modal Analysis for Tracking Structural Change during Construction and Operation Phases PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-475116 UR - https://www.mdpi.com/1424-8220/19/4/927/pdf DO - https://doi.org/10.3390/s19040927 SN - 1424-8220 VL - 19 IS - 4 SP - 927, 1 EP - 23 PB - MDPI AG CY - Basel, Switzerland AN - OPUS4-47511 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ren, J. A1 - Weigert, Florian A1 - Weber, F. A1 - Wang, Y. A1 - Choudhury, S. A1 - Xiao, J. A1 - Lauermann, I. A1 - Resch-Genger, Ute A1 - Bande, A. A1 - Petit, T. ED - Petit, Tristan T1 - Influence of surface chemistry on optical, chemical and electronic properties of blue luminescent carbon dots N2 - Carbon dots have attracted much attention due to their unique optical, chemical and electronic properties enabling a wide range of applications. The properties of carbon dots can be effectively adjusted through modifying their chemical composition. However, a major challenge remains in understanding the core and surface contributions to optical and electronic transitions. Here, three blue luminescent carbon dots with carboxyl, amino and hydroxyl groups were comprehensively characterized by UV-vis absorption and emission spectroscopy, synchrotron-based X-ray spectroscopy, and infrared spectroscopy. The influence of the surface functionality on their fluorescence was probed by pH-dependent photoluminescence measurements. Moreover, the hydrogen bonding interactions between water and the surface groups of carbon dots were characterized by infrared spectroscopy. Our results show that both core and surface electronic states of blue luminescent carbon dots contribute to electronic acceptor levels while the chemical nature of the surface groups determines the hydrogen bonding behavior of the carbon dots. This comprehensive spectroscopic study demonstrates that the surface chemistry has a profound influence on the electronic configuration and surface–water interaction of carbon dots, thus affecting their photoluminescence properties. KW - Quantum dots KW - Spectroscopy KW - UV Vis KW - Fluorescence KW - Surface chemistry PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-472325 DO - https://doi.org/10.1039/c8nr08595a SN - 2040-3372 VL - 11 IS - 4 SP - 2056 EP - 2064 PB - RSC AN - OPUS4-47232 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Priebe, Nsesheye Susan A1 - Gluth, Gregor A1 - Sturm, Patrick A1 - Vogler, Nico A1 - Kühne, Hans-Carsten T1 - Comparison of calcined illitic clays (brick clays) and low-grade kaolinitic clays as supplementary cementitious materials N2 - The use of calcined clays as supplementary cementitious materials (SCMs) has been identified as a viable option to decrease the CO2 emissions related to cement production. However, while extensive data is available about kaolinitic clays in this context, other clays such as illitic clays appear to be under-studied. Therefore, in the present study, two illitic clays were compared to two low-grade kaolinitic clays in terms of transformations in the calcination temperature range 650–900 °C, and performance of the calcined clays in blended cement pastes as measured by strength evolution, heat release, hydrated phase formation and portlandite consumption. The illitic clays required a higher calcination temperature for complete dehydroxylation of their illite than what is necessary for dehydroxylation of kaolinite. These higher calcination temperatures also led to particle sintering, significantly decreasing the specific surface area of the illitic clays, particularly for the clay with the higher Fe2O3 content. Nevertheless, while the kaolinitic clays generally exhibited the best performance as SCM, the illitic clay with lower Fe2O3 content performed similar to the kaolinitic clays when calcined at optimum temperature and applied at a moderate substitution rate. These findings demonstrate that several different clays have the potential to be used as SCM and indicate possible routes to identify suitable deposits for this purpose. KW - Blended cement KW - Calcined clay KW - Brick clay KW - Illite KW - Kaolinite PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-488195 DO - https://doi.org/10.1617/s11527-019-1393-2 SN - 1359-5997 SN - 1871-6873 N1 - Geburtsname von Priebe, Nsesheye Susan: Msinjili, N. S. - Birth name of Priebe, Nsesheye Susan: Msinjili, N. S. VL - 52 IS - 5 SP - Article Number 94 PB - Springer Nature AN - OPUS4-48819 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Otto, Peter A1 - Lorenzis, L. A1 - Unger, Jörg F. T1 - Explicit dynamics in impact simulation using a NURBS contact interface N2 - In this paper, the impact problem and the subsequent wave propagation are considered. For the contact discretization an intermediate NURBS layer is added between the contacting finite element bodies, which allows a smooth contact formulation and efficient element‐based integration. The impact event is ill‐posed and requires a regularization to avoid propagating stress oscillations. A nonlinear mesh dependent penalty regularization is used, where the stiffness of the penalty regularization increases upon mesh refinement. Explicit time integration methods are well suited for wave propagation problems, but are efficient only for diagonal mass matrices. Using a spectral element discretization and the coupled FE‐NURBS approach the bulk part of the mass matrix is diagonal. KW - Impact simulation KW - Explicit dynamics KW - Isogeometric analysis KW - Spectral elements KW - Mortar method PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-494947 DO - https://doi.org/10.1002/nme.6264 SP - 1 EP - 21 PB - Wiley Online Libary AN - OPUS4-49494 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zirnstein, Benjamin A1 - Schulze, Dietmar A1 - Schartel, Bernhard T1 - Mechanical and fire properties of multicomponent flame retardant EPDM rubbers using aluminum trihydroxide, ammonium polyphosphate, and polyaniline N2 - In this study, multicomponent flame retardant systems, consisting of Ammonium polyphosphate (APP), aluminum trihydroxide (ATH), and polyaniline (PANI), were used in ethylene propylene diene monomer (EPDM) rubber. The multicomponent system was designed to improve flame retardancy and the mechanical properties of the rubber compounds, while simultaneously reducing the amount of filler. PANI was applied at low loadings (7 phr) and combined with the phosphorous APP (21 phr) and the mineral flame retardant ATH (50 phr). A comprehensive study of six EPDM rubbers was carried out by systematically varying the fillers to explain the impact of multicomponent flame retardant systems on mechanical properties. The six EPDM materials were investigated via the UL 94, limiting oxygen index (LOI), FMVSS 302, glow wire tests, and the cone calorimeter, showing that multicomponent flame retardant systems led to improved fire performance. In cone calorimeter tests the EPDM/APP/ATH/PANI composite reduced the maximum average rate of heat emission (MARHE) to 142 kW·m-2, a value 50% lower than that for the unfilled EPDM rubber. Furthermore, the amount of phosphorus in the residues was quantified and the mode of action of the phosphorous flame retardant APP was explained. The data from the cone calorimeter were used to determine the protective layer effect of the multicomponent flame retardant systems in the EPDM compounds. KW - EPDM KW - Rubber KW - Flame retardant KW - Polyaniline KW - Aluminum trihydroxide (ATH) PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-482769 DO - https://doi.org/10.3390/ma12121932 SN - 1996-1944 VL - 12 IS - 12 SP - 1932, 1 EP - 22 PB - MDPI AN - OPUS4-48276 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hussels, Maria-Teresa A1 - Chruscicki, Sebastian A1 - Arndt, Detlef A1 - Scheider, Swen A1 - Prager, Jens A1 - Homann, Tobias A1 - Habib, Abdel Karim T1 - Localization of transient events threatening pipeline integrity by fiber-optic distributed acoustic sensing N2 - Pipe integrity is a central concern regarding technical safety, availability, and environmental compliance of industrial plants and pipelines. A condition monitoring system that detects and localizes threats in pipes prior to occurrence of actual structural failure, e.g., leakages, especially needs to target transient events such as impacts on the pipe wall or pressure waves travelling through the medium. In the present work, it is shown that fiber-optic distributed acoustic sensing (DAS) in conjunction with a suitable application geometry of the optical fiber sensor allows to track propagating acoustic waves in the pipeline wall on a fast time-scale. Therefore, short impacts on the pipe may be localized with high fidelity. Moreover, different acoustic modes are identified, and their respective group velocities are in good agreement with theoretical predications. In another set of experiments modeling realistic damage scenarios, we demonstrate that pressure waves following explosions of different gas mixtures in pipes can be observed. Velocities are verified by local piezoelectric pressure transducers. Due to the fully distributed nature of the fiber-optic sensing system, it is possible to record accelerated motions in detail. Therefore, in addition to detection and localization of threatening events for infrastructure monitoring, DAS may provide a powerful tool to study the development of gas explosions in pipes, e.g., investigation of deflagration-to-detonation-transitions (DDT). KW - Distributed acoustic sensing (DAS) KW - Distributed vibrations sensing (DVS) KW - Fiber-optic sensing KW - Condition monitoring KW - Pipeline integrity KW - Gas explosion PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-488555 DO - https://doi.org/10.3390/s19153322 SN - 1424-8220 VL - 19 IS - 15 SP - 3322, 1 EP - 20 PB - MDPI CY - Basel, CH AN - OPUS4-48855 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Provis, J. L. A1 - Arbi, K. A1 - Bernal, S. A. A1 - Bondar, D. A1 - Buchwald, A. A1 - Castel, A. A1 - Chithiraputhiran, S. A1 - Cyr, M. A1 - Dehghan, A. A1 - Dombrowski-Daube, K. A1 - Dubey, A. A1 - Ducman, V. A1 - Gluth, Gregor A1 - Nanukuttan, S. A1 - Peterson, K. A1 - Puertas, F. A1 - van Riessen, A. A1 - Torres-Carrasco, M. A1 - Ye, G. A1 - Zuo, Y. T1 - RILEM TC 247-DTA round robin test: mix design and reproducibility of compressive strength of alkali-activated concretes N2 - The aim of RILEM TC 247-DTA ‘Durability Testing of Alkali-Activated Materials’ is to identify and validate methodologies for testing the durability of alkali-activated concretes. To underpin the durability testing work of this committee, five alkali-activated concrete mixes were developed based on blast furnace slag, fly ash, and flash-calcined metakaolin. The concretes were designed with different intended performance levels, aiming to assess the capability of test methods to discriminate between concretes on this basis. A total of fifteen laboratories worldwide participated in this round robin test programme, where all concretes were produced with the same mix designs, from single-source aluminosilicate precursors and locally available aggregates. This paper reports the mix designs tested, and the compressive strength results obtained, including critical insight into reasons for the observed variability in strength within and between laboratories. KW - Alkali-activated materials KW - Alkali-activated slag KW - Compressive strength KW - Concrete KW - Mix-design PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-489131 DO - https://doi.org/10.1617/s11527-019-1396-z SN - 1359-5997 SN - 1871-6873 VL - 52 IS - 5 SP - Article Number 99 PB - Springer Nature AN - OPUS4-48913 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hoevelmann, J. A1 - Stawski, T. M. A1 - Besselink, R. A1 - Freeman, H. M. A1 - Dietmann, K. M. A1 - Mayanna, S. A1 - Pauw, Brian Richard A1 - Benning, L. G. T1 - A template-free and low temperature method for the synthesis of mesoporous magnesium phosphate with uniform pore structure and high surface area N2 - Mesoporous phosphates are a group of nanostructured materials with promising applications, particularly in biomedicine and catalysis. However, their controlled synthesis via conventional template-based routes presents a number of challenges and limitations. Here, we show how to synthesize a mesoporous Magnesium phosphate with a high surface area and a well-defined pore structure through thermal decomposition of a crystalline struvite (MgNH4PO4·6H2O) precursor. In a first step, struvite crystals with various morphologies and sizes, ranging from a few micrometers to several millimeters, had been synthesized from supersaturated aqueous solutions (saturation index (SI) between 0.5 and 4) at ambient pressure and temperature conditions. Afterwards, the crystals were thermally treated at 70–250 °C leading to the release of structurally bound water (H2O) and ammonia (NH3). By combining thermogravimetric analyses (TGA), scanning and transmission electron microscopy (SEM, TEM), N2 sorption analyses and small- and wide-angle X-ray scattering (SAXS/WAXS) we show that this decomposition process results in a pseudomorphic transformation of the original struvite into an amorphous Mg-phosphate. Of particular importance is the fact that the final material is characterized by a very uniform mesoporous structure with 2–5 nm wide pore channels, a large specific surface area of up to 300 m2 g−1 and a total pore volume of up to 0.28 cm3 g−1. Our struvite decomposition method is well controllable and reproducible and can be easily extended to the synthesis of other mesoporous phosphates. In addition, the so produced mesoporous material is a prime candidate for use in biomedical applications considering that Magnesium phosphate is a widely used, non-toxic substance that has already shown excellent biocompatibility and biodegradability. KW - Struvite KW - SAXS KW - Scattering KW - Nanoporous KW - Geology PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-477130 DO - https://doi.org/10.1039/c8nr09205b VL - 11 IS - 14 SP - 6939 EP - 6951 PB - Royal Society of Chemistry AN - OPUS4-47713 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Descalzo, Ana B. A1 - Ashokkumar, Pichandi A1 - Shen, Z. A1 - Rurack, Knut T1 - On the Aggregation Behaviour and Spectroscopic Properties of Alkylated and Annelated BoronDipyrromethene (BODIPY) Dyes in Aqueous Solution N2 - The tendency of boron-dipyrromethene (BODIPY) dyes to associate in water is well known, and usually a cause for inferior fluorescence properties. Synthetic efforts to chemically improve BODIPYs’ water solubility and minimize this problem have been numerous in the past. However, a deeper understanding of the phenomena responsible for fluorescence quenching is still required. Commonly, the spectroscopic behaviour in aqueous media has been attributed to aggregate or excimer formation, with such works often centring on a single BODIPY family. Herein, we provide an integrating discussion including very diverse types of BODIPY dyes. Our studies revealed that even subtle structural changes can distinctly affect the association behaviour of the fluorophores in water, involving different photophysical processes. The palette of behaviour found ranges from unperturbed emission, to the formation of H or J aggregates and excimers, to the involvement of tightly bound, preformed excimers. These results are a first step to a more generalized understanding of spectroscopic properties vs. structure, facilitating future molecular design of BODIPYs, especially as probes for biological applications. KW - Aggregates KW - BODIPY KW - Excimers KW - Fluorescence KW - Photophysics PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-497771 DO - https://doi.org/10.1002/cptc.201900235 SN - 2367-0932 VL - 4 IS - 2 SP - 120 EP - 131 PB - WILEY-VCH CY - Weinheim AN - OPUS4-49777 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liu, H. A1 - Song, W. A1 - Gröninger, Delia A1 - Zhang, L. A1 - Lu, Y. A1 - Chan, K. S. A1 - Zhou, Z. A1 - Rurack, Knut A1 - Shen, Z. T1 - Real-time monitoring of newly acidified organelles during autophagy enabled by reaction-based BODIPY dyes N2 - Real-time monitoring of newly acidified organelles during autophagy in living cells is highly desirable for a better understanding of intracellular degradative processes. Herein, we describe a reaction-based boron dipyrromethene (BODIPY) dye containing strongly electron-withdrawing diethyl 2-cyanoacrylate groups at the α-positions. The probe exhibits intense red fluorescence in acidic organelles or the acidified cytosol while negligible fluorescence in other regions of the cell. The underlying mechanism is a nucleophilic reaction at the central meso-carbon of the indacene core, resulting in the loss of π-conjugation entailed by dramatic spectroscopic changes of more than 200 nm between its colorless, non-fluorescent leuco-BODIPY form and its red and brightly emitting form. The reversible transformation between red fluorescent BODIPY and leuco-BODIPY along with negligible cytotoxicity qualifies such dyes for rapid and direct intracellular lysosome imaging and cytosolic acidosis detection simultaneously without any washing step, enabling the real-time monitoring of newly acidified organelles during autophagy. KW - Autophagy KW - BODIPY KW - Fluorescence KW - Lysosome KW - Real-time imaging PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-498358 UR - https://www.nature.com/articles/s42003-019-0682-1 DO - https://doi.org/10.1038/s42003-019-0682-1 SN - 23993642 VL - 2 SP - 442 PB - Nature Research CY - London AN - OPUS4-49835 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Büchele, Dominique A1 - Chao, Madlen A1 - Ostermann, Markus A1 - Leenen, M. A1 - Bald, Ilko T1 - Multivariate chemometrics as a key tool for prediction of K and Fe in a diverse German agricultural soil-set using EDXRF N2 - Within the framework of precision agriculture, the determination of various soil properties is moving into focus, especially the demand for sensors suitable for in-situ measurements. Energy-dispersive X-ray fluorescence (EDXRF) can be a powerful tool for this purpose. In this study a huge diverse soil set (n = 598) from 12 different study sites in Germany was analysed with EDXRF. First, a principal component analysis (PCA) was performed to identify possible similarities among the sample set. Clustering was observed within the four texture classes clay, loam, silt and sand, as clay samples contain high and sandy soils low iron mass fractions. Furthermore, the potential of uni- and multivariate data evaluation with partial least squares regression (PLSR) was assessed for accurate Determination of nutrients in German agricultural samples using two calibration sample sets. Potassium and iron were chosen for testing the performance of both models. Prediction of these nutrients in 598 German soil samples with EDXRF was more accurate using PLSR which is confirmed by a better overall averaged deviation and PLSR should therefore be preferred. KW - XRF KW - Chemometrics KW - Soil KW - Agriculture KW - Multivariate PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-498671 DO - https://doi.org/10.1038/s41598-019-53426-5 VL - 9 SP - 17588 PB - Nature AN - OPUS4-49867 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yildirim, Arda A1 - Sentker, K. A1 - Smales, Glen Jacob A1 - Pauw, Brian Richard A1 - Huber, P. A1 - Schönhals, Andreas T1 - Collective orientational order and phase behavior of a discotic liquid crystal under nanoscale confinement N2 - The phase behavior and molecular ordering of hexakishexyloxy triphenylene (HAT6) DLC under cylindrical nanoconfinement is studied utilizing differential scanning calorimetry (DSC) and dielectric spectroscopy (DS), where cylindrical nanoconfinement is established through embedding HAT6 into the nanopores of anodic aluminum oxide membranes (AAO), and a silica membrane with pore diameters ranging from 161 nm down to 12 nm. Both unmodified and modified pore walls were considered, and in the latter case the pore walls of AAO membranes were chemical treated with n octadecylphosphonic acid (ODPA) resulting in the formation of a 2.2 nm thick layer of grafted alkyl chains. Phase transition enthalpies decrease with decreasing pore size, indicating that a large proportion of the HAT6 molecules within the pores has a disordered structure, which increases with decreasing pore size for both pore walls. In the case of the ODPA modification the amount of ordered HAT6 is increased compared to the unmodified case. The pore size dependencies of the phase transition temperatures were approximated using the Gibbs Thomson equation, where the estimated surface tension is dependent on the molecular ordering of HAT6 molecules within the pores and upon their surface. DS was employed to investigate the molecular ordering of HAT6 within the nanopores. These investigations revealed that with a pore size of around 38 nm, for the samples with the unmodified pore walls, the molecular ordering changes from planar axial to homeotropic radial. However, the planar axial configuration, which is suitable for electronic applications, can be successfully preserved through ODPA modification for most of the pore sizes. KW - Discotic Liquid Crystals KW - Nanoconfinement PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-475222 DO - https://doi.org/10.1039/c8na00308d SN - 2516-0230 VL - 1 IS - 3 SP - 1104 EP - 1116 PB - RSC AN - OPUS4-47522 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gramse, G. A1 - Schönhals, Andreas A1 - Kienberger, F. T1 - Nanoscale dipole dynamics of protein membranes studied by broadband dielectric microscopy N2 - We investigate the nearfield dipole mobility of protein membranes in a wide frequency range from 3 kHz to 10 GHz. The results of our nanoscale dielectric images and spectra of bacteriorhodopsin (bR) reveal Debye relaxations with time constants of τ ∼ 2 ns and τ ∼ 100 ns being characteristic of the Dipole moments of the bR retinal and α-helices, respectively. However, the dipole mobility and therefore the protein biophysical function depend critically on the amount of surface water surrounding the protein, and the characteristic mobility in the secondary structure is only observed for humidity levels <30%. Our results have been achieved by adding the frequency as a second fundamental dimension to quantitative dielectric microscopy. The key elements for the success of this advanced technique are the employed heterodyne detection scheme, the broadband electrical signal source, a high frequency optimized cabling, development of calibration procedures and precise finite element modelling. Our study demonstrates the exciting possibilities of broadband dielectric microscopy for the investigation of dynamic processes in cell bioelectricity at the individual molecular level. Furthermore, the technique may shed light on local dynamic processes in related materials science applications like semiconductor Research or nano-electronics. KW - Broadband dielectric microscopy PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-475230 DO - https://doi.org/10.1039/c8nr05880f SN - 2040-3372 VL - 11 IS - 10 SP - 4303 EP - 4309 PB - RSC AN - OPUS4-47523 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Röhsler, Andreas A1 - Sobol, Oded A1 - Unger, Wolfgang A1 - Böllinghaus, Thomas T1 - Comprehensive study of deuterium-induced effects in in austenitic stainless steel AISI 304L N2 - The damaging impact of hydrogen on the austenitic stainless steel AISI 304 L was analysed. To this aim, samples were charged electrochemically with the hydrogen isotope deuterium (2H, D) and examined with time-of-flight secondary ion mass spectrometry (ToF-SIMS) and electron backscatter diffraction (EBSD). The fusion of the obtained chemical and structural information revealed local enrichment of deuterium in austenite, transformation into martensite, crack formation and severe roughening of the specimen surface. The results indicated that martensite was not only formed during charging but also during Desorption and ToF-SIMS examinations. Furthermore, cross-sections of deuterium-charged samples revealed that in preferred deformation bands a g/ε/a 0 evolution is taking place. By means of microscopic analyses and carrier gas hot extraction (CGHE), it was found that the use of NaAsO2 as recombination poison decreased the uptake of hydrogen significantly and resulted in severe precipitation on the specimen surfaces. This is in contrast to the popular presumption that NaAsO2 enhances the uptake of hydrogen (and deuterium) during electrochemical charging by hampering its recombination from Atoms to molecules. KW - AISI 304L KW - Hydrogen KW - ToF-SIMS KW - Deuterium KW - Martensite PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-477540 DO - https://doi.org/10.1016/j.ijhydene.2019.03.058 SN - 0360-3199 SN - 1879-3487 VL - 44 IS - 23 SP - 12228 EP - 12238 PB - Elsevier Ltd. AN - OPUS4-47754 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schwibbert, Karin A1 - Menzel, F. A1 - Epperlein, N. A1 - Bonse, Jörn A1 - Krüger, Jörg T1 - Bacterial adhesion on femtosecond laser-modified polyethylene N2 - In this study, femtosecond laser-induced sub-micrometer structures are generated to modify polyethylene (PE) surface topographies. These surfaces were subjected to bacterial colonization studies with Escherichia coli and Staphylococcus aureus as test strains. The results reveal that the nanostructures do not influence S. aureus coverage, while the adhesion of E. coli is reduced. KW - Bacterial adhesion KW - Laser-modified surface KW - Polyethylene KW - Laser-induced nanostructures KW - Biofilm PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-492280 DO - https://doi.org/10.3390/ma12193107 VL - 12 IS - 19 SP - 3107 PB - MDPI CY - Basel, Schweiz AN - OPUS4-49228 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gharaati, S. A1 - Wang, Cui A1 - Förster, C. A1 - Weigert, Florian A1 - Resch-Genger, Ute A1 - Heinze, K. T1 - Triplet–Triplet Annihilation Upconversion in a MOF with AcceptorFilled Channels N2 - In summary, we report a highly modular solid TTA-UC system comprising of a crystalline, thermally stable PCN222(Pd) MOF with CA-coated MOF channels and with a DPA annihilator embedded in a solution-like environment in the MOF channels. This solid material displays blue upconverted delayed emission with a luminescence lifetime of 373 us, a threshold value of 329 mW*cm-2 and a triplet–triplet energy transfer efficiency of 82%. This optical application adds another facet to the versatile chemistry of PCN-222 MOFs. The design concept is also applicable to other TTA-UC pairs and enables tuning of the UCL color, for example, by replacing DPA with other dyes as exemplarily shown for 2,5,8,11-tetra-tert-butyl-perylene, that yields UCL at 450 nm. Current work aims to reduce the oxygen sensitivity and to increase the retention of the trapped annihilators in organic environments, for example, by tuning the chain length of the carboxylic acid and by coating the MOF surface. In addition, the TTA-UC efficiency will be further enhanced by reducing the reabsorption of the UC emission caused by Pd(TCPP) and by optimizing the sensitizer/annihilator interface. KW - Porphyrin KW - Method KW - MOF KW - Fluorescence KW - Dye KW - Sensor KW - Oxygen sensitive KW - Single molecule KW - DPA KW - Lifetime KW - Upconverstion KW - Quantum yield KW - Triplet-triplet annihilation KW - Sensitization KW - Energy transfer KW - NMR PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-500580 DO - https://doi.org/10.1002/chem.201904945 VL - 26 IS - 5 SP - 1003 EP - 1007 PB - Wiley-VCH Verlag CY - Weinheim AN - OPUS4-50058 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kembuan, C. A1 - Saleh, Maysoon I. A1 - Rühle, Bastian A1 - Resch-Genger, Ute A1 - Graf, C. T1 - Coating of upconversion nanoparticles with silica nanoshells of 5–250 nm thickness N2 - A concept for the growth of silica shells with a thickness of 5–250 nm onto oleate-coated NaYF4:Yb3+/Er3+ upconversion nanoparticles (UCNP) is presented. The concept enables the precise adjustment of shell thicknesses for the preparation of thick-shelled nanoparticles for applications in plasmonics and sensing. First, an initial 5–11 nm thick shell is grown onto the UCNPs in a reverse microemulsion. This is followed by a stepwise growth of these particles without a purification step, where in each step equal volumes of tetraethyl orthosilicate and ammonia water are added, while the volumes of cyclohexane and the surfactant Igepal® CO-520 are increased so that the ammonia water and surfactant concentrations remain constant. Hence, the number of micelles stays constant, and their size is increased to accommodate the growing core–shell particles. Consequently, the formation of core-free silica particles is suppressed. When the negative zeta potential of the particles, which continuously decreased during the stepwise growth, falls below −40 mV, the particles can be dispersed in an ammoniacal ethanol solution and grown further by the continuous addition of tetraethyl orthosilicate to a diameter larger than 500 nm. Due to the high colloidal stability, a coalescence of the particles can be suppressed, and single-core particles are obtained. This strategy can be easily transferred to other nanomaterials for the design of plasmonic nanoconstructs and sensor systems. KW - Reverse microemulsion KW - Silica coating KW - Stepwise growth KW - Thick shells KW - Upconversion nanoparticles PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-502769 DO - https://doi.org/10.3762/bjnano.10.231 SN - 2190-4286 VL - 10 SP - 2410 EP - 2421 PB - Beilstein-Institut zur Förderung der Chemischen Wissenschaften CY - Frankfurt, M. AN - OPUS4-50276 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Javaheri, E. A1 - Lubritz, J. A1 - Graf, B. A1 - Rethmeier, Michael T1 - Mechanical Properties Characterization of Welded Automotive Steels N2 - Among the various welding technologies, resistance spot welding (RSW) and laser beam welding (LBW) play a significant role as joining methods for the automobile industry. The application of RSW and LBW for the automotive body alters the microstructure in the welded areas. It is necessary to identify the mechanical properties of the welded material to be able to make a reliable statement about the material behavior and the strength of welded components. This study develops a method by which to determine the mechanical properties for the weldment of RSW and LBW for two dual phase (DP) steels, DP600 and DP1000, which are commonly used for the automotive bodies. The mechanical properties of the resistance spot weldment were obtained by performing tensile tests on the notched tensile specimen to cause an elongation of the notched and welded area in order to investigate its properties. In order to determine the mechanical properties of the laser beam weldment, indentation tests were performed on the welded material to calculate its force-penetration depth-curve. Inverse numerical simulation was used to simulate the indentation tests to determine and verify the parameters of a nonlinear isotropic material model for the weldment of LBW. Furthermore, using this method, the parameters for the material model of RSW were verified. The material parameters and microstructure of the weldment of RSW and LBW are compared and discussed. The results show that the novel method introduced in this work is a valid approach to determine the mechanical properties of welded high-strength steel structures. In addition, it can be seen that LBW and RSW lead to a reduction in ductility and an increase in the amount of yield and tensile strength of both DP600 and DP1000. KW - Mechanical property KW - Laser beam welding KW - Dual phase steel KW - Resistance spot welding PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-502269 DO - https://doi.org/10.3390/met10010001 VL - 10 IS - 1 SP - 1 EP - 20 PB - MDPI AN - OPUS4-50226 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radnik, Jörg A1 - Dang, T. T. H. A1 - Gatla, S. A1 - Raghuwanshi, V. S. A1 - Tatchev, D. A1 - Hoell, A. T1 - Identifying the location of Cu ions in nanostructured SAPO-5 molecular sieves and its impact on the redox properties N2 - Combining X-ray Absorption Fine Spectroscopy (XAFS) with Anomalous Small-Angle X-ray Scattering (ASAXS) determines the location of Cu2+ ions in silicoaluminophosphate (SAPO-5) frameworks prepared by hydrothermal crystallization or impregnation. As expected, for the hydrothermally prepared sample, incorporation in the SAPO-5 framework was observed. For the first time preferential location of Cu2+ ions at the inner and outer surfaces of the framework is determined. Temperature-Programmed Reduction (TPR) and X-ray Photoelectron Spectroscopy (XPS) investigations demonstrated that such Cu2+ is stable in an argon (Ar) atmosphere up to 550 °C and can only be reduced under a hydrogen atmosphere. In contrast, Cu2+ deposited by impregnation on the pure SAPO-5 framework can be easily reduced to Cu+ in an Ar atmosphere. At lower Cu amounts, mononuclear tetrahedrally coordinated Cu species were formed which are relatively stable in the monovalent form. In contrast, at higher Cu amounts, CuO particles were found which change easily between the mono- and bivalent species. KW - Nanostructured material KW - Molecular sieves KW - X-ray absorption Fine Spectroscopy KW - Anomalous Small Angle X-ray Scattering KW - X-ray Photoelectron Spectroscopy PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-474793 DO - https://doi.org/10.1039/c8ra10417d SN - 2046-2069 VL - 9 IS - 12 SP - 6429 EP - 6437 PB - RSC AN - OPUS4-47479 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lisec, Jan A1 - Jaeger, Carsten A1 - Rashid, R. A1 - Munir, R. A1 - Zaidi, N. T1 - Cancer cell lipid class homeostasis is altered under nutrient-deprivation but stable under hypoxia N2 - Background: Cancer cells modify the balance between fatty acid (FA) synthesis and uptake under metabolic stress, induced by oxygen/nutrient deprivation. These modifications were shown to alter the levels of individual triglyceride (TG) or phospholipid sub-species. To attain a holistic overview of the lipidomic profiles of cancer cells under stress we performed a broad lipidomic assay, comprising 244 lipids from six major classes. This assay allowed us to perform robust analyses and assess the changes in averages of broader lipid-classes, stratified on the basis of saturation index of their fatty-acyl side chains. Methods: Global lipidomic profiling using Liquid Chromatography-Mass Spectrometry was performed to assess lipidomic profiles of biologically diverse cancer cell lines cultivated under metabolically stressed conditions. Results: Neutral lipid compositions were markedly modified under serum-deprived conditions and, strikingly, the cellular level of triglyceride subspecies decreased with increasing number of double bonds in their fatty acyl chains. In contrast and unexpectedly, no robust changes were observed in lipidomic profiles of hypoxic (2% O2) Cancer cells despite concurrent changes in proliferation rates and metabolic gene expression. Conclusions: Serum-deprivation significantly affects lipidomic profiles of cancer cells. Although, the levels of individual lipid moieties alter under hypoxia (2% O2), the robust averages of broader lipid classes remain unchanged. KW - Tumor metabolism KW - Fatty acid metabolism KW - Lipidomic profile KW - Metabolic stress PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-481061 DO - https://doi.org/10.1186/s12885-019-5733-y SN - 1471-2407 VL - 19 SP - 501, 1 EP - 11 PB - Springer Nature AN - OPUS4-48106 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Duewer, D. L. A1 - Murray, J. A. A1 - Wood, L. J. A1 - Wise, S. A. A1 - Hein, Sebastian A1 - Koch, Matthias A1 - Philipp, Rosemarie A1 - Werneburg, Martina A1 - Hackenberg, R. A1 - Polzer, J. A1 - Avila, M. A. A1 - Serrano, V. A1 - Kakoulides, E. A1 - Alexopoulos, C. A1 - Giannikopoulou, P. A1 - Gui, E. M. A1 - Lu, T. A1 - Teo, T. L. A1 - Hua, T. A1 - Dazhou, C. A1 - Chunxin, L. A1 - Changjun, Y. A1 - Hongmei, L. A1 - Nammoonnoy, J. A1 - Sander, L. C. A1 - Lippa, K. A1 - Quinn, L. A1 - Swiegelaar, C. A1 - Fernandes-Whaley, M. A1 - Gören, A. C. A1 - Gökcen, T. T1 - CCQM-K95.1 Low-polarity analytes in a botanical matrix: Polycyclic aromatic hydrocarbons (PAHs) in tea N2 - Extraction, chromatographic separation, and quantification of low-concentration organic compounds in complex matrices are core challenges for reference material producers and providers of calibration services. Evidence of successful participation in formal, relevant international comparisons is needed to document measurement capability claims made by national metrology institutes (NMIs) and designated institutes (DIs). To enable NMIs and DIs to update or establish their claims, in 2014 the Organic Analysis Working Group (OAWG) initiated CCQM-K95.1 "Low-Polarity Analytes in a Botanical Matrix: Polycyclic Aromatic Hydrocarbons (PAHs) in Tea". This was a follow-on comparison from CCQM-K95 which was completed in 2014. The polycyclic aromatic hydrocarbons (PAHs) benz[a]anthracene (BaA) and benzo[a]pyrene (BaP) are considered priority pollutants by U.S. Environmental Protection Agency and are regulated contaminants in food, pose chromatographic separation challenges, and for which exist well-characterized measurement procedures and standard materials. BaA and BaP in a smoked tea were therefore selected as representative target measurands for CCQM-K95.1. Ten NMIs participated in CCQM-K95.1. The consensus summary mass fractions for the two PAHs are in the range of (50 to 70) ng/g with relative standard deviations of (6 to 10) %. Successful participation in CCQM K95.1 demonstrates the following measurement capabilities in determining mass fraction of organic compounds, with molar mass of 100 g/mol to 500 g/mol and having polarity pKow −2, in a botanical matrix ranging in mass fraction from 10 ng/g to 1000 ng/g: (1) value assignment of primary reference standards (if in-house purity assessment carried out), (2) value assignment of single and/or multi-component organic solutions, (3) extraction of analytes of interest from the matrix, (4) cleanup and separation of analytes of interest from interfering matrix or extract components, and (5) separation and quantification using gas chromatography or liquid chromatography. KW - Benz[a]anthracene (BaA) KW - Benzo[a]pyrene (BaP) KW - Gas chromatography (GC) KW - Isotope dilution (ID) KW - Liquid chromatography (LC) KW - Mass spectrometry (MS) KW - Polycyclic aromatic hydrocarbon (PAH) KW - Yerba mate tea PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-471430 DO - https://doi.org/10.1088/0026-1394/56/1A/08002 SN - 0026-1394 SN - 1681-7575 VL - 56 IS - 1 A SP - 08002, 1 EP - 89 PB - IOP Science AN - OPUS4-47143 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brüngel, R. A1 - Rückert, J. A1 - Wohlleben, W. A1 - Babick, F. A1 - Ghanem, A. A1 - Gaillard, C. A1 - Mech, A. A1 - Rauscher, H. A1 - Hodoroaba, Vasile-Dan A1 - Weigel, S. A1 - Friedrich, C. M. T1 - NanoDefiner e-Tool: An Implemented Decision Support Framework for Nanomaterial Identification N2 - The European Commission’s recommendation on the definition of nanomaterial (2011/696/EU) established an applicable standard for material categorization. However, manufacturers face regulatory challenges during registration of their products. Reliable categorization is difficult and requires considerable expertise in existing measurement techniques (MTs). Additionally, organizational complexity is increased as different authorities’ registration processes require distinct reporting. The NanoDefine project tackled these obstacles by providing the NanoDefiner e-tool: A decision support expert system for nanomaterial identification in a regulatory context. It providesMT recommendations for categorization of specific materials using a tiered approach (screening/confirmatory), and was constructed with experts from academia and industry to be extensible, interoperable, and adaptable for forthcoming revisions of the nanomaterial definition. An implemented MT-driven material categorization scheme allows detailed description. Its guided workflow is suitable for a variety of user groups. Direct feedback and explanation enable transparent decisions. Expert knowledge is Held in a knowledge base for representation of MT performance criteria and physicochemical particle type properties. Continuous revision ensured data quality and validity. Recommendations were validated by independent case studies on industry-relevant particulate materials. Besides supporting material identification and registration, the free and open-source e-tool may serve as template for other expert systems within the nanoscience domain. KW - EC nanomaterial definition KW - Decision support KW - Expert system KW - Nanomaterial KW - Nanoparticles PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-492449 DO - https://doi.org/10.3390/ma12193247 VL - 12 IS - 19 SP - 3247 PB - MDPI CY - Basel, CH AN - OPUS4-49244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nöller, Renate A1 - Danielewski, A. A1 - Giel, R. A1 - Overgaauw, E. A1 - Hahn, Oliver T1 - Material analysis of Aztec codices in Berlin. Assignment of small fragments compiled as cutouts on one plate in Humboldt’s “Atlas pittoresque du voyage” N2 - The collection Manuscripta Americana in Berlin consists of fragmented codices acquired by Alexander von Humboldt in Mexico. Some of these Humboldt Codices are published as hieroglyphic writings of the Aztecs in “Vues des Cordilleres et Monuments des Peuples indigènes de l’Amerique”. Starting from a special compilation of seven fragments on plate 36 in the “Atlas”, we investigated the corresponding original fragments using material analysis in order to clarify their historical relations. The analyses were carried out with X-ray fluorescence analysis, VIS spectroscopy, and infrared spectroscopy in diffuse reflection and revealed typical indigenous colors like cochineal, indigo, and organic yellows (e.g. mangrove and zacatlaxcalli). Four fragments under investigation show exactly the same material and thus must once have belonged together in one compendium. An additional manuscript from Mizquiahuala also shown on plate 36 can be matched to another one that is not published in the “Atlas”. KW - Manuscripts KW - Alexander von Humboldt KW - Non-destructiv testing KW - Colourants KW - Writing materials PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-498971 DO - https://doi.org/10.1080/20548923.2019.1682816 SN - 2054-8923 SP - 1 EP - 14 PB - Routledge, Taylor & Francis Group CY - London AN - OPUS4-49897 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Greco, A. A1 - Starostin, V. A1 - Karapanagiotis, Christos A1 - Hinderhofer, A. A1 - Gerlach, A. A1 - Pithan, L. A1 - Liehr, Sascha A1 - Schreiber, Frank A1 - Kowarik, Stefan T1 - Fast fitting of reflectivity data of growing thin films using neural networks N2 - X-ray reflectivity (XRR) is a powerful and popular scattering technique that can give valuable insight into the growth behavior of thin films. This study Shows how a simple artificial neural network model can be used to determine the thickness, roughness and density of thin films of different organic semiconductors [diindenoperylene, copper(II) phthalocyanine and alpha-sexithiophene] on silica from their XRR data with millisecond computation time and with minimal user input or a priori knowledge. For a large experimental data set of 372 XRR curves, it is shown that a simple fully connected model can provide good results with a mean absolute percentage error of 8–18% when compared with the results obtained by a genetic least mean squares fit using the classical Parratt formalism. Furthermore, current drawbacks and prospects for improvement are discussed. KW - Artificial neural networks KW - X-ray reflectivity PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-498997 DO - https://doi.org/10.1107/S1600576719013311 SN - 1600-5767 VL - 52 SP - 1342 EP - 1347 PB - Wiley AN - OPUS4-49899 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Buljak, V. A1 - Oesch, Tyler A1 - Bruno, Giovanni T1 - Simulating fiber-reinforced concrete mechanical performance using CT-based fiber orientation data N2 - The main hindrance to realistic models of fiber-reinforced concrete (FRC) is the local materials property variation, which does not yet reliably allow simulations at the structural level. The idea presented in this paper makes use of an existing constitutive model, but resolves the problem of localized material variation through X-ray computed tomography (CT)-based pre-processing. First, a three-point bending test of a notched beam is considered, where pre-test fiber orientations are measured using CT. A numerical model is then built with the zone subjected to progressive damage, modeled using an orthotropic damage model. To each of the finite elements within this zone, a local coordinate system is assigned, with its longitudinal direction defined by local fiber orientations. Second, the parameters of the constitutive damage model are determined through inverse analysis using load-displacement data obtained from the test. These parameters are considered to clearly explain the material behavior for any arbitrary external action and fiber orientation, for the same geometrical properties and volumetric ratio of fibers. Third, the effectiveness of the resulting model is demonstrated using a second, “control” experiment. The results of the “control” experiment analyzed in this research compare well with the model results. The ultimate strength was predicted with an error of about 6%, while the work-of-load was predicted within 4%. It demonstrates the potential of this method for accurately predicting the mechanical performance of FRC components. KW - Fiber-reinforced concrete KW - X-ray computed tomography (CT) KW - Anisotropic fiber orientation KW - Inverse analysis PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-474728 DO - https://doi.org/10.3390/ma12050717 SN - 1996-1944 VL - 12 IS - 5 SP - 717, 1 EP - 16 PB - MDPI AN - OPUS4-47472 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mishurova, Tatiana A1 - Artzt, K. A1 - Haubrich, J. A1 - Requena, G. A1 - Bruno, Giovanni T1 - Exploring the correlation between subsurface residual stresses and manufacturing parameters in laser powder bed fused Ti-6Al-4V N2 - Subsurface residual stresses (RS) were investigated in Ti-6Al-4V cuboid samples by means of X-ray synchrotron diffraction. The samples were manufactured by laser powder bed fusion (LPBF) applying different processing parameters, not commonly considered in open literature, in order to assess their influence on RS state. While investigating the effect of process parameters used for the calculation of volumetric energy density (such as laser velocity, laser power and hatch distance), we observed that an increase of energy density led to a decrease of RS, although not to the same extent for every parameter variation. Additionally, the effect of support structure, sample roughness and LPBF machine effects potentially coming from Ar flow were studied. We observed no influence of support structure on subsurface RS while the orientation with respect to Ar flow showed to have an impact on RS.We conclude recommending monitoring such parameters to improve part reliability and reproducibility. KW - Additive manufacturing KW - Synchrotron X-ray diffraction KW - Residual stress KW - Ti-6Al-4V PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-474281 DO - https://doi.org/10.3390/met9020261 SN - 2075-4701 VL - 9 IS - 2 SP - 261, 1 EP - 13 PB - MDPI AN - OPUS4-47428 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Laquai, René A1 - Gouraud, F. A1 - Müller, Bernd R. A1 - Huger, M. A1 - Chotard, T. A1 - Antou, G. A1 - Bruno, Giovanni T1 - Evolution of Thermal Microcracking in Refractory ZrO2-SiO2 after Application of External Loads at High Temperatures N2 - Zirconia-based cast refractories are widely used for glass furnace applications. Since they have to withstand harsh chemical as well as thermo-mechanical environments, internal stresses and microcracking are often present in such materials under operating conditions (sometimes in excess of 1700 °C). We studied the evolution of thermal (CTE) and mechanical (Young’s modulus) properties as a function of temperature in a fused-cast refractory containing 94 wt.% of monoclinic ZrO2 and 6 wt.% of a silicate glassy phase. With the aid of X-ray refraction techniques (yielding the internal specific surface in materials), we also monitored the evolution of microcracking as a function of thermal cycles (crossing the martensitic phase transformation around 1000 °C) under externally applied stress. We found that external compressive stress leads to a strong decrease of the internal surface per unit volume, but a tensile load has a similar (though not so strong) effect. In agreement with existing literature on -eucryptite microcracked ceramics, we could explain These phenomena by microcrack closure in the load direction in the compression case, and by microcrack propagation (rather than microcrack nucleation) under tensile conditions. KW - Electro-fused zirconia KW - Microcracking KW - Synchrotron x-ray refraction radiography (SXRR) KW - Thermal expansion PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-477431 DO - https://doi.org/10.3390/ma12071017 VL - 12 IS - 7 SP - 1 EP - 15 PB - MDPI AN - OPUS4-47743 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mieller, Björn T1 - Influence of test procedure on dielectric breakdown strength of alumina N2 - Dielectric strength testing of ceramics can be performed with various setups and parameters. Comparisons of results from different sources are often not meaningful, because the results are strongly dependent on the actual testing procedure. The aim of this study is to quantify the influence of voltage ramp rate, electrode size, electrode conditioning, and sample thickness on the measured AC dielectric strength of a commercial alumina. Mean values, Weibull moduli, and failure probabilities determined in standardized short time tests are evaluated and related to withstand voltage tests. Dielectric strength values in the range from 21.6 to 33.2 kV/mm were obtained for the same material using different testing procedures. Short time tests resulted in small standard deviations (< 2 kV/mm) and high Weibull moduli around 30, while withstand tests at voltage levels with low and virtual zero failure probability in short time tests resulted in large scatter of withstand time and Weibull moduli < 1. The strong decrease in Weibull moduli is attributed to progressive damage from partial discharge and depolarization during AC testing. These findings emphasize the necessity of a thorough documentation of testing procedure and highlight the importance of withstand voltage tests for a comprehensive material characterization. KW - Ceramic KW - High-voltage testing KW - Dielectric breakdown KW - Alumina PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-483852 DO - https://doi.org/10.1007/s40145-018-0310-4 SN - 2226-4108 SN - 2227-8508 VL - 8 IS - 2 SP - 247 EP - 255 PB - Springer AN - OPUS4-48385 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strangfeld, Christoph A1 - Johann, Sergej A1 - Bartholmai, Matthias T1 - Smart RFID Sensors Embedded in Building Structures for Early Damage Detection and Long-Term Monitoring N2 - In civil engineering, many structures are made of reinforced concrete. Most Degradation processes relevant to this material, e.g., corrosion, are related to an increased level of material moisture. Therefore, moisture monitoring in reinforced concrete is regarded as a crucial method for structural health monitoring. In this study, passive radio frequency identification (RFID)-based sensors are embedded into the concrete. They are well suited for long-term operation over decades and are well protected against harsh environmental conditions. The energy supply and the data transfer of the humidity sensors are provided by RFID. The sensor casing materials are optimised to withstand the high alkaline environment in concrete, having pH values of more than 12. Membrane materials are also investigated to identify materials capable of enabling water vapour transport from the porous cement matrix to the embedded humidity sensor. By measuring the corresponding relative humidity with embedded passive RFID-based sensors, the cement hydration is monitored for 170 days. Moreover, long-term moisture monitoring is performed for more than 1000 days. The Experiments show that embedded passive RFID-based sensors are highly suitable for long-term structural health monitoring in civil engineering. KW - RFID based sensors KW - Embedded sensors KW - Corresponding relative humidity KW - Porous building materials KW - Reinforced concrete KW - Corrosion KW - Civil engineering PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-500831 DO - https://doi.org/10.3390/s19245514 VL - 19 IS - 24 SP - 1 EP - 18 PB - MDPI CY - Basel, Swiss AN - OPUS4-50083 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sebald, M.A. A1 - Gebauer, J. A1 - Sommerfeld, Thomas A1 - Koch, Matthias T1 - First Synthesis of (−)-Altenuene-D3 Suitable as Internal Standard for Isotope Dilution Mass Spectrometry N2 - Metabolites from Alternaria fungi exhibit a variety of biological properties such as phytotoxic, cytotoxic, or antimicrobial activity. Optimization of a literature procedure culminated in an efficient total synthesis of (−)-altenuene as well as a stable isotope-labeled derivative suitable for implementation in a LC-MS/MS method for mycotoxin analysis. KW - Altenuene KW - Alternaria mycotoxins KW - Food safety KW - Isotope-labeled KW - SIDA-LC-MS/MS KW - Suzuki coupling PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-500696 DO - https://doi.org/10.3390/molecules24244563 SN - 1420-3049 VL - 24 SP - 4563 PB - MDPI CY - Basel AN - OPUS4-50069 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kneipp, Janina A1 - Zancajo, Victor M.R. A1 - Diehn, S. A1 - Filiba, N. A1 - Elbaum, R. T1 - Spectroscopic Discrimination of Sorghum Silica Phytoliths N2 - Grasses accumulate silicon in the form of silicic acid, which is precipitated as amorphous silica in microscopic particles termed phytoliths. These particles comprise a variety of morphologies according to the cell type in which the silica was deposited. Despite the evident morphological differences, phytolith chemistry has mostly been analysed in bulk samples, neglecting differences between the varied types formed in the same species. In this work, we extracted leaf phytoliths from mature plants of Sorghum bicolor (L.) Moench. Using solid state NMR and thermogravimetric analysis, we show that the extraction methods alter greatly the silica molecular structure, its condensation degree and the trapped organic matter. Measurements of individual phytoliths by Raman and synchrotron FTIR microspectroscopies in combination with multivariate analysis separated bilobate silica cells from prickles and long cells, based on the silica molecular structures and the fraction and composition of occluded organic matter. The variations in structure and composition of sorghum phytoliths suggest that the biological pathways leading to silica deposition vary between these cell types. KW - Phytoliths KW - Biosilicification KW - Raman KW - Sorghum KW - Solid state NMR KW - Synchrotron FTIR PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-502672 DO - https://doi.org/10.3389/fpls.2019.01571 VL - 10 SP - 1571 PB - Frontiers Media CY - Lausanne AN - OPUS4-50267 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmidt, C. A1 - Hensen, C. A1 - Wallmann, K. A1 - Liebetrau, V. A1 - Tatzel, Michael A1 - Schurr, S. L. A1 - Kutterolf, S. A1 - Haffert, L. A1 - Geilert, Sonja A1 - Hübscher, C. A1 - Lebas, E. A1 - Heuser, A. A1 - Schmidt, M. A1 - Strauss, H. A1 - Vogl, Jochen A1 - Hansteen, T. T1 - Origin of High Mg and SO4 Fluids in Sediments of the Terceira Rift, Azores‐Indications for Caminite Dissolution in a Waning Hydrothermal System N2 - During R/V Meteor cruise 141/1, pore fluids of near surface sediments were investigated to find indications for hydrothermal activity in the Terceira Rift (TR), a hyperslow spreading center in the Central North Atlantic Ocean. To date, submarine hydrothermal fluid venting in the TR has only been reported for the D. João de Castro seamount, which presently seems to be inactive. Pore fluids sampled close to a volcanic cone at 2,800‐m water depth show an anomalous composition with Mg, SO4, and total alkalinity concentrations significantly higher than seawater and a nearby reference core. The most straightforward way of interpreting these deviations is the dissolution of the hydrothermally formed mineral caminite (MgSO4 0.25 Mg (OH)2 0.2H2O). This interpretation is corroborated by a thorough investigation of fluid isotope systems (δ26Mg, δ30Si, δ34S, δ44/42Ca, and 87Sr/86Sr). Caminite is known from mineral assemblages with anhydrite and forms in hydrothermal recharge zones only under specific conditions such as high fluid temperatures and in altered oceanic crust, which are conditions generally met at the TR. We hypothesize that caminite was formed during hydrothermal activity and is now dissolving during the waning state of the hydrothermal system, so that caminite mineralization is shifted out of its stability zone. Ongoing fluid circulation through the basement is transporting the geochemical signal via slow advection toward the seafloor. KW - Isotope ratio KW - Delta value KW - Pore fluids KW - Magnesium KW - Hydrothermal fluid PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-503430 DO - https://doi.org/10.1029/2019GC008525 VL - 20 IS - 12 SP - 6078 EP - 6094 PB - Wiley AN - OPUS4-50343 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sarhan, R. M. A1 - Koopman, W. A1 - Schuetz, R. A1 - Schmid, Thomas A1 - Liebig, F. A1 - Koetz, J. A1 - Bargheer, M. T1 - The importance of plasmonic heating for the plasmondriven photodimerization of 4-nitrothiophenol N2 - Metal nanoparticles form potent nanoreactors, driven by the optical generation of energetic electrons and nanoscale heat. The relative influence of these two factors on nanoscale chemistry is strongly debated. This article discusses the temperature dependence of the dimerization of 4-nitrothiophenol (4-NTP) into 4,4′-dimercaptoazobenzene (DMAB) adsorbed on gold nanoflowers by Surface-Enhanced Raman Scattering (SERS). Raman thermometry shows a significant optical heating of the particles. The ratio of the Stokes and the anti-Stokes Raman signal moreover demonstrates that the molecular temperature during the reaction rises beyond the average crystal lattice temperature of the plasmonic particles. The product bands have an even higher temperature than reactant bands, which suggests that the reaction proceeds preferentially at thermal hot spots. In addition, kinetic measurements of the reaction during external heating of the reaction environment yield a considerable rise of the reaction rate with temperature. Despite this significant heating effects, a comparison of SERS spectra recorded after heating the sample by an external heater to spectra recorded after prolonged illumination shows that the reaction is strictly photo-driven. While in both cases the temperature increase is comparable, the dimerization occurs only in the presence of light. Intensity dependent measurements at fixed temperatures confirm this finding. KW - Nanoparticles KW - Plasmonic heating KW - Raman spectroscopy PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-475140 DO - https://doi.org/10.1038/s41598-019-38627-2 SN - 2045-2322 VL - 9 IS - 1 SP - 3060, 1 EP - 8 PB - Nature Publishing Group AN - OPUS4-47514 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Domonov, D.P. A1 - Pechenyuk, S.I. A1 - Semushina, Y.P. A1 - Yusenko, Kirill T1 - Solid state transformation in inner coordination sphere of [Co(NH3)6][Fe(C2O4)3]·3H2O as a route to access catalytically active Co-Fe materials N2 - Thermal decomposition of [Co(NH₃)₆][Fe(C₂O₄)₃]∙3H₂O in argon atmosphere, at a low heating rate (3°/min), and in large amounts of the initial complex (~0.1 mole), has been studied. It was possible to distinguish four decomposition steps upon heating: In the temperature range of 50⁻100 °C-the loss of crystal water; 100⁻190 °C-stability region of dehydrated complex; 230⁻270 °C-the range of stability of intermediate phase with the formula CoFe(NH₃)₂(C₂O₄)₂; 270⁻350 °C-thermal decomposition of the intermediate with the formation of metallic products and further air oxidation with the formation of Co1.5Fe1.5O₄. Catalytic properties of thermolysis products were tested in the decomposition reaction of H₂O₂ (inactive), oxidation of acetone (average activity), and decomposition of ammonium perchlorate (highly active). KW - Double complex salts KW - Catalysts KW - Single-source precursors PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-474014 DO - https://doi.org/10.3390/ma12020221 SN - 1996-1944 VL - 12 IS - 2 SP - 221, 1 EP - 10 PB - mdpi CY - Zürich AN - OPUS4-47401 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mekonnen, Tessema Fenta A1 - Panne, Ulrich A1 - Koch, Matthias T1 - Glucosylation and Glutathione Conjugation of Chlorpyrifos and Fluopyram Metabolites Using Electrochemistry/Mass Spectrometry N2 - Xenobiotics and their reactive metabolites are conjugated with native biomolecules such as glutathione and glucoside during phase II metabolism. Toxic metabolites are usually detoxified during this step. On the other hand, these reactive species have a potential health impact by disrupting many enzymatic functions. Thus, it is crucial to understand phase II conjugation reactions of xenobiotics in order to address their fate and possible toxicity mechanisms. Additionally, conventional methods (in vivo and in vitro) have limitation due to matrix complexity and time-consuming. Hence, developing fast and matrix-free alternative method is highly demandable. In this work, oxidative phase I metabolites and reactive species of chlorpyrifos (insecticide) and fluopyram (fungicide) were electrochemically produced by using a boron-doped diamond electrode coupled online to electrospray mass spectrometry (ESI-MS). Reactive species of the substrates were trapped by biomolecules (glutathione and glucoside) and phase II conjugative metabolites were identified using liquid chromatography (LC)-MS/MS, and/or Triple time of flight (TripleTOF)-MS. Glutathione conjugates and glucosylation of chlorpyrifos, trichloropyridinol, oxon, and monohydroxyl fluopyram were identified successfully. Glutathione and glucoside were conjugated with chlorpyrifos, trichloropyridinol, and oxon by losing a neutral HCl. In the case of fluopyram, its monohydroxyl metabolite was actively conjugated with both glutathione and glucoside. In summary, seven bioconjugates of CPF and its metabolites and two bioconjugates of fluopyram metabolites were identified using electrochemistry (EC)/MS for the first time in this work. The work could be used as an alternative approach to identify glutathione and glucosylation conjugation reactions of other organic compounds too. It is important, especially to predict phase II conjugation within a short time and matrix-free environment. KW - Pesticide KW - Bioconjugation KW - Oxidative metabolism KW - EC/MS PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-475932 DO - https://doi.org/10.3390/molecules24050898 VL - 24 IS - 5 SP - 898 EP - 910 PB - MDPI AN - OPUS4-47593 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Choi, Youngeun A1 - Schmidt, Carsten A1 - Tinnefeld, Philip A1 - Bald, Ilko A1 - Roedinger, Stefan T1 - A new reporter design based on DNA origami nanostructures for quantification of short oligonucleotides using microbeads N2 - The DNA origami technique has great potential for the development of brighter and more sensitive reporters for fluorescence based detection schemes such as a microbead-based assay in diagnostic applications. The nanostructures can be programmed to include multiple dye molecules to enhance the measured signal as well as multiple probe strands to increase the binding strength of the target oligonucleotide to these nanostructures. Here we present a proof-of-concept study to quantify short oligonucleotides by developing a novel DNA origami based reporter system, combined with planar microbead assays. Analysis of the assays using the VideoScan digital imaging platform showed DNA origami to be a more suitable reporter candidate for quantification of the target oligonucleotides at lower concentrations than a conventional reporter that consists of one dye molecule attached to a single stranded DNA. Efforts have been made to conduct multiplexed analysis of different targets as well as to enhance fluorescence signals obtained from the reporters. We therefore believe that the quantification of short oligonucleotides that exist in low copy numbers is achieved in a better way with the DNA origami nanostructures as reporters. KW - Origami KW - Nanostructures KW - Microbeads KW - DNA origami KW - Oligonucleotides PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-476443 DO - https://doi.org/10.1038/s41598-019-41136-x SN - 2045-2322 VL - 9 SP - 4769, 1 EP - 8 PB - Nature AN - OPUS4-47644 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Treiling, S. A1 - Wang, Cui A1 - Förster, C. A1 - Reichenauer, F. A1 - Kalmbach, J. A1 - Boden, P. A1 - Harris, J. P. A1 - Carrella, L. M. A1 - Rentschler, E. A1 - Resch-Genger, Ute A1 - Reber, C. A1 - Seitz, M. A1 - Gerhards, M. A1 - Heinze, K. T1 - Luminescence and Light-Driven Energy and Electron Transfer from an Exceptionally Long-Lived Excited State of a Non-Innocent Chromium(III) Complex N2 - Photoactive metal complexes employing Earth‐abundant metal ions are a key to sustainable photophysical and photochemical applications. We exploit the effects of an inversion center and ligand non‐innocence to tune the luminescence and photochemistry of the excited state of the [CrN6] chromophore [Cr(tpe)2]3+ with close to octahedral symmetry (tpe=1,1,1‐tris(pyrid‐2‐yl)ethane). [Cr(tpe)2]3+ exhibits the longest luminescence lifetime (τ=4500 μs) reported up to date for a molecular polypyridyl chromium(III) complex together with a very high luminescence quantum yield of Φ=8.2 % at room temperature in fluid solution. Furthermore, the tpe ligands in [Cr(tpe)2]3+ are redox non‐innocent, leading to reversible reductive chemistry. The excited state redox potential and lifetime of [Cr(tpe)2]3+ surpass those of the classical photosensitizer [Ru(bpy)3]2+ (bpy=2,2′‐bipyridine) enabling energy transfer (to oxygen) and photoredox processes (with azulene and tri(n‐butyl)amine). KW - Quantum yield KW - Cr(III) complex KW - Longst luminescence lifetime KW - Electron transfer PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-494870 DO - https://doi.org/10.1002/anie.201909325 VL - 58 SP - 2 EP - 13 PB - Wiley-VCH AN - OPUS4-49487 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Anja A1 - Heinrich, Thomas A1 - Tougaard, S. A1 - Werner, W. S. M. A1 - Hronek, M. A1 - Kunz, Valentin A1 - Radnik, Jörg A1 - Stockmann, Jörg M. A1 - Hodoroaba, Vasile-Dan A1 - Benemann, Sigrid A1 - Nirmalananthan-Budau, Nithiya A1 - Geißler, Daniel A1 - Sparnacci, K. A1 - Unger, Wolfgang T1 - Determining the thickness and completeness of the shell of polymer core-shell nanoparticles by X-ray photoelectron spectroscopy, secondary ion mass spectrometry, and transmission scanning electron microscopy N2 - Core–shell nanoparticles (CSNPs) have become indispensable in various industrial applications. However, their real internal structure usually deviates from an ideal core–shell structure. To control how the particles perform with regard to their specific applications, characterization techniques are required that can distinguish an ideal from a nonideal morphology. In this work, we investigated poly(tetrafluoroethylene)–poly(methyl methacrylate) (PTFE–PMMA) and poly(tetrafluoroethylene)–polystyrene (PTFE–PS) polymer CSNPs with a constant core diameter (45 nm) but varying shell thicknesses (4–50 nm). As confirmed by transmission scanning electron microscopy (T-SEM), the shell completely covers the core for the PTFE–PMMA nanoparticles, while the encapsulation of the core by the shell material is incomplete for the PTFE–PS nanoparticles. X-ray photoelectron spectroscopy (XPS) was applied to determine the shell thickness of the nanoparticles. The software SESSA v2.0 was used to analyze the intensities of the elastic peaks, and the QUASES software package was employed to evaluate the shape of the inelastic background in the XPS survey spectra. For the first time, nanoparticle shell thicknesses are presented, which are exclusively based on the analysis of the XPS inelastic background. Furthermore, principal component analysis (PCA)-assisted time-of-flight secondary-ion mass spectrometry (ToF-SIMS) of the PTFE–PS nanoparticle sample set revealed a systematic variation among the samples and, thus, confirmed the incomplete encapsulation of the core by the shell material. As opposed to that, no variation is observed in the PCA score plots of the PTFE–PMMA nanoparticle sample set. Consequently, the complete coverage of the core by the shell material is proved by ToF-SIMS with a certainty that cannot be achieved by XPS and T-SEM. KW - XPS KW - T-SEM KW - ToF-SIMS KW - Core-shell nanoparticles PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-499165 DO - https://doi.org/10.1021/acs.jpcc.9b09258 VL - 123 IS - 49 SP - 29765 EP - 29775 PB - American Chemical Society CY - Washington, DC AN - OPUS4-49916 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jürgens, Maria A1 - Olbricht, Jürgen A1 - Fedelich, Bernard A1 - Skrotzki, Birgit T1 - Low Cycle Fatigue and Relaxation Performance of Ferritic–Martensitic Grade P92 Steel N2 - Due to their excellent creep resistance and good oxidation resistance, 9–12% Cr ferritic–martensitic stainless steels are widely used as high temperature construction materials in power plants. However, the mutual combination of different loadings (e.g., creep and fatigue), due to a “flexible” operation of power plants, may seriously reduce the lifetimes of the respective components. In the present study, low cycle fatigue (LCF) and relaxation fatigue (RF) tests performed on grade P92 helped to understand the behavior of ferritic–martensitic steels under a combined loading. The softening and lifetime behavior strongly depend on the temperature and total strain range. Especially at small strain amplitudes, the lifetime is seriously reduced when adding a hold time which indicates the importance of considering technically relevant small strains. KW - Ferritic–martensitic steel KW - P92 KW - Low cycle fatigue KW - Relaxation fatigue KW - Cyclic softening PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-473905 DO - https://doi.org/10.3390/met9010099 VL - 9 IS - 1 SP - 99, 1 EP - 25 PB - MDPI AN - OPUS4-47390 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kömmling, Anja A1 - Jaunich, Matthias A1 - Pourmand, P. A1 - Wolff, Dietmar A1 - Hedenqvist, M. T1 - Analysis of O-ring seal failure under static conditions and determination of end-of-lifetime criterion N2 - Determining a suitable and reliable end-of-lifetime criterion for O-ring seals is an important issue for long-term seal applications. Therefore, seal failure of ethylene propylene diene rubber (EPDM) and hydrogenated nitrile butadiene rubber (HNBR) O-rings aged in the compressed state at 125 °C and at 150 °C for up to 1.5 years was analyzed and investigated under static conditions, using both non-lubricated and lubricated seals. Changes of the material properties were analyzed with dynamic-mechanical analysis and permeability experiments. Indenter modulus measurements were used to investigate DLO effects. It became clear that O-rings can remain leak-tight under static conditions even when material properties have already degraded considerably, especially when adhesion effects are encountered. As a feasible and reliable end-of-lifetime criterion for O-ring seals under static conditions should include a safety margin for slight dimensional changes, a modified leakage test involving a small and rapid partial decompression of the seal was introduced that enabled determining a more realistic but still conservative end-of-lifetime criterion for an EPDM seal. KW - EPDM KW - HNBR KW - Seal failure KW - Leak-tightness KW - DLO KW - Oxygen permability KW - DMA KW - Indenter modulus PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-486125 DO - https://doi.org/10.3390/polym11081251 SN - 2073-4360 VL - 11 IS - 8 SP - 1251, 1 EP - 19 PB - MDPI CY - Basel, CH AN - OPUS4-48612 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lisec, Jan A1 - Jaeger, Carsten A1 - Rashid, R. A1 - Munir, R. A1 - Zaidi, N. T1 - Cancer cell lipid class homeostasis is altered under nutrient-deprivation but stable under hypoxia N2 - Background: Cancer cells modify the balance between fatty acid (FA) synthesis and uptake under metabolic stress, induced by oxygen/nutrient deprivation. These modifications were shown to alter the levels of individual triglyceride (TG) or phospholipid sub-species. To attain a holistic overview of the lipidomic profiles of cancer cells under stress we performed a broad lipidomic assay, comprising 244 lipids from six major classes. This assay allowed us to perform robust analyses and assess the changes in averages of broader lipid-classes, stratified on the basis of saturation index of their fatty-acyl side chains. Methods: Global lipidomic profiling using Liquid Chromatography-Mass Spectrometry was performed to assess lipidomic profiles of biologically diverse cancer cell lines cultivated under metabolically stressed conditions. Results: Neutral lipid compositions were markedly modified under serum-deprived conditions and, strikingly, the cellular level of triglyceride subspecies decreased with increasing number of double bonds in their fatty acyl chains. In contrast and unexpectedly, no robust changes were observed in lipidomic profiles of hypoxic (2% O2) cancer cells despite concurrent changes in proliferation rates and metabolic gene expression. Conclusions: Serum-deprivation significantly affects lipidomic profiles of cancer cells. Although, the levels of individual lipid moieties alter under hypoxia (2% O2), the robust averages of broader lipid classes remain unchanged. KW - Tumor metabolism KW - Fatty acid metabolism KW - Lipidomic profile KW - Metabolic stress PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-483186 DO - https://doi.org/10.1186/s12885-019-5733-y SN - 1471-2407 VL - 19 SP - 501 PB - Springer Nature CY - Berlin AN - OPUS4-48318 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steger, Simon A1 - Oesterle, D. A1 - Bretz, S. A1 - Frenzel, L. A1 - Stege, H. A1 - Winkelmeyer, I. A1 - Hahn, Oliver A1 - Geiger, G. T1 - Kandinsky’s fragile art: a multidisciplinary investigation of four early reverse glass paintings (1911–1914) by Wassily Kandinsky N2 - This work highlights the rediscovery of the technique of reverse glass painting by the artists of the “Blaue Reiter” collective in the early 20th-century and focusses particularly on the role of Wassily Kandinsky (1866–1944). Kandinsky created more than 70 reverse paintings on glass and showed several of them in exhibitions together with paintings on canvas and cardboard, implying a coequal importance of these techniques. Four of his early (1911–1914) reverse glass paintings (Auferstehung, Allerheiligen II, Rudern, Apokalyptischer Reiter II) were selected for investigation and their iconography, painting techniques and painting materials were examined. Two paintings were executed on so-called cathedral glass, revealing a “hammered surface”, whereas Kandinsky used a corrugated glass panel for Rudern. A multi-analytical, non-invasive approach [X-ray fluorescence (XRF), diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS), VIS spectroscopy (VIS), Raman spectroscopy] was taken to identify the pigments and classify the binding media. The results reveal a broad palette of materials. Several pigments like lead white, zinc white, Strontium yellow, Prussian blue, viridian, cadmium yellow, ultramarine blue, cinnabar and carbon black were found in most of the four paintings. The use of the rare synthetic organic pigments PR60 and PB52 is discussed. In two works of art, cadmium carbonate is associated with cadmium yellow. The identification of aluminium foil along with tin foils in Rudern indicates an early use of this material for reverse glass paintings. KW - Reverse glass painting KW - Non-invasive analysis KW - Raman spectroscopy KW - DRIFTS PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-480075 DO - https://doi.org/10.1186/s40494-019-0268-8 VL - 7 IS - 27 SP - 1 EP - 17 PB - Springer AN - OPUS4-48007 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Carl, Peter A1 - Ramos, Inês I. A1 - Segundo, Marcela A. A1 - Schneider, Rudolf T1 - Antibody conjugation to carboxyl-modified microspheres through N-hydroxysuccinimide chemistry for automated immunoassay applications: A general procedure N2 - Immunochemical techniques are the workhorse for sample enrichment and detection of a large variety of analytes. In contrast to classical microtiter plate-based assays, microparticles are a next generation solid support, as they promote automation of immunoassays using flow-based techniques. Antibody immobilization is a crucial step, as these reagentsmare expensive, and inefficient coupling can result in low sensitivities. This paper proposes a general procedure for efficient immobilization of antibodies onto TentaGel particles, via Nhydroxysuccinimide chemistry. The goal was the preparation of solid supports with optimum immunorecognition, while increasing the sustainability of the process. The influence of buffer composition, activation and coupling time, as well as the amount of antibody on the immobilization efficiency was investigated, resorting to fluorophore-labeled proteins and fluorescence imaging. Buffer pH and activation time are the most important parameters for efficient coupling. It is demonstrated, that the hydrolysis of N-hydroxysuccinimide esters occurs at similar rates as in solution, limiting the utilizable time for coupling. Finally, applicability of the generated material for automated affinity extraction is demonstrated on the mesofluidic platform lab-on-valve. KW - Mesofluidics KW - Bead injections KW - ELISA KW - Carbamazepine KW - Biomarkers PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-483919 DO - https://doi.org/10.1371/journal.pone.0218686 SN - 1932-6203 VL - 14 IS - 6 SP - e0218686, 1 EP - 18 PB - Public Library of Science CY - San Francisco, California, USA AN - OPUS4-48391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Souza Machado, A. A. A1 - Lau, C. W. A1 - Kloas, W. A1 - Bergmann, J. A1 - Bachelier, J. B. A1 - Faltin, E. A1 - Becker, Roland A1 - Görlich, A. S. A1 - Rillig, M. C. T1 - Microplastics can change soil properties and affect plant performance N2 - Microplastics can affect biophysical properties of the soil. However, little is known about the cascade of events in fundamental levels of terrestrial ecosystems, i.e., starting with the changes in soil abiotic properties and propagating across the various components of soil−plant interactions, including soil microbial communities and plant traits. We investigated here the effects of six different microplastics (polyester fibers, polyamide beads, and four fragment types: polyethylene, polyester terephthalate, polypropylene, and polystyrene) on a broad suite of proxies for soil health and performance of spring onion (Allium fistulosum). Significant changes were observed in plant biomass, tissue elemental composition, root traits, and soil microbial activities. These plant and soil responses to microplastic exposure were used to propose a causal model for the mechanism of the effects. Impacts were dependent on particle type, i.e., microplastics with a shape similar to other natural soil particles elicited smaller differences from control. Changes in soil structure and water dynamics may explain the observed results in which polyester fibers and polyamide beads triggered the most pronounced impacts on plant traits and function. The findings reported here imply that the pervasive microplastic contamination in soil may have consequences for plant performance and thus for agroecosystems and terrestrial biodiversity. KW - Mikroplastik KW - Boden KW - Pflanzenwachstum PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-484181 DO - https://doi.org/10.1021/acs.est.9b01339 SN - 0013-936X SN - 1520-5851 VL - 53 IS - 10 SP - 6044 EP - 6052 PB - ACS AN - OPUS4-48418 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kotthoff, Lisa A1 - Lisec, Jan A1 - Schwerdtle, T. A1 - Koch, Matthias T1 - Prediction of transformation products of monensin by electrochemistry compared to microsomal assay and hydrolysis N2 - The knowledge of transformation pathways and identification of transformation products (TPs) of veterinary drugs is important for animal health, food, and environmental matters. The active agent Monensin (MON) belongs to the ionophore antibiotics and is widely used as a veterinary drug against coccidiosis in broiler farming. However, no electrochemically (EC) generated TPs of MON have been described so far. In this study, the online coupling of EC and mass spectrometry (MS) was used for the generation of oxidative TPs. EC-conditions were optimized with respect to working electrode material, solvent, modifier, and potential polarity. Subsequent LC/HRMS (liquid chromatography/high resolution mass spectrometry) and MS/MS experiments were performed to identify the structures of derived TPs by a suspected target analysis. The obtained EC-results were compared to TPs observed in metabolism tests with microsomes and hydrolysis experiments of MON. Five previously undescribed TPs of MON were identified in our EC/MS based study and one TP, which was already known from literature and found by a microsomal assay, could be confirmed. Two and three further TPs were found as products in microsomal tests and following hydrolysis, respectively. We found decarboxylation, O-demethylation and acid-catalyzed ring-opening reactions to be the major mechanisms of MON transformation. KW - Transformation products KW - Monensin KW - Veterinary drugs KW - Electrochemistry KW - Hydrolysis KW - LC/HRMS PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-485689 DO - https://doi.org/10.3390/molecules24152732 SN - 1420-3049 VL - 24 IS - 15 SP - 2732, 1 EP - 12 PB - MDPI CY - Basel AN - OPUS4-48568 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Geißler, Daniel A1 - Wegmann, Marc A1 - Jochum, T. A1 - Somma, V. A1 - Sowa, M. A1 - Scholz, J. A1 - Fröhlich, E. A1 - Hoffmann, Katrin A1 - Niehaus, J. A1 - Roggenbuck, D. A1 - Resch-Genger, Ute T1 - An automatable platform for genotoxicity testing of nanomaterials based on the fluorometric γ-H2AX assay reveals no genotoxicity of properly surface-shielded cadmium-based quantum dots N2 - The large number of nanomaterial-based applications emerging in the materials and life sciences and the foreseeable increasing use of these materials require methods that evaluate and characterize the toxic potential of these nanomaterials to keep safety risks to people and environment as low as possible. As nanomaterial toxicity is influenced by a variety of parameters like size, shape, chemical composition, and surface chemistry, high throughput screening (HTS) platforms are recommended for assessing cytotoxicity. Such platforms are not yet available for genotoxicity testing. Here, we present first results obtained for application-relevant nanomaterials using an automatable genotoxicity platform that relies on the quantification of the phosphorylated histone H2AX (γ-H2AX) for detecting DNA double strand breaks (DSBs) and the automated microscope system AKLIDES® for measuring integral fluorescence intensities at different excitation wavelengths. This platform is used to test the genotoxic potential of 30 nm-sized citrate-stabilized gold nanoparticles (Au-NPs) as well as micellar encapsulated iron oxide nanoparticles (FeOx-NPs) and different cadmium (Cd)-based semiconductor quantum dots (QDs), thereby also searching for positive and negative controls as reference materials. In addition, the influence of the QD shell composition on the genotoxic potential of these Cd-based QDs was studied, using CdSe cores as well as CdSe/CdS core/shell and CdSe/CdS/ZnS core/shell/shell QDs. Our results clearly revealed the genotoxicity of the Au-NPs and its absence in the FeOx-NPs. The genotoxicity of the Cd-QDs correlates with the shielding of their Cd-containing core, with the core/shell/shell architecture preventing genotoxicity risks. The fact that none of these nanomaterials showed cytotoxicity at the chosen particle concentrations in a conventional cell viability assay underlines the importance of genotoxicity studies to assess the hazardous potential of nanomaterials. KW - Nanomaterial KW - Genotoxicity testing KW - γ-H2AX assay KW - Quantum dot PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-486318 DO - https://doi.org/10.1039/C9NR01021A SN - 2040-3372 SN - 2040-3364 VL - 11 IS - 28 SP - 13458 EP - 13468 PB - The Royal Society of Chemistry AN - OPUS4-48631 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Saleh, Maysoon I. A1 - Panas, I. A1 - Frenzel, Florian A1 - Würth, Christian A1 - Rühle, Bastian A1 - Slominskii, Y. A1 - Demchenko, A. A1 - Resch-Genger, Ute T1 - Sensitization of upconverting nanoparticles with a NIR-emissive cyanine dye using a micellar encapsulation approach N2 - Photon upconversion nanomaterials have a wide range of applications, including biosensing and deep-tissue imaging. Their typically very weak and narrow absorption bands together with their size dependent luminescence efficiency can limit their application potential. This has been addressed by increasingly sophisticated core-shell particle architectures including the sensitization with organic dyes that strongly absorb in the near infrared (NIR). In this work, we present a simple water-dispersible micellar system that features energy transfer from the novel NIR excitable dye, 1859 SL with a high molar absorption coefficient and a moderate fluorescence quantum yield to oleate-capped NaYF4:20%Yb(III), 2%Er(III) upconversion nanoparticles (UCNP) upon 808 nm excitation. The micelles were formed using the surfactants Pluronic F-127 and Tween 80 to produce a hydrophilic dye-UCNP system. Successful energy transfer from the dye to the UCNP could be confirmed by emission measurements that revealed the occurrence of upconversion emission upon excitation at 808 nm and an enhancement of the green Er(III) emission compared to direct Er(III) excitation at 808 nm. KW - Upconversion nanoparticles KW - Sensitization KW - NIR dyes KW - Energy transfer PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-472300 DO - https://doi.org/10.1088/2050-6120/aafe1f SN - 2050-6120 VL - 7 IS - 1 (Special issue: Upconversion Methods, Applications and Materials) SP - 014003-1 EP - 014003-9 PB - IOP AN - OPUS4-47230 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kröcke, N. A1 - Grebenteuch, S. A1 - Keil, C. A1 - Demtröder, S. A1 - Koch, L. A1 - Thünemann, Andreas A1 - Benning, R. A1 - Haase, H. T1 - Effect of different drying methods on nutrient quality of the yellow mealworm (Tenebrio molitor L.) N2 - Yellow mealworm (Tenebrio molitor L.) represents a sustainable source of proteins and fatty acids for feed and food. Industrial production of mealworms necessitates optimized processing techniques, where drying as the first postharvest procedure is of utmost importance for the quality of the final product. This study examines the nutritional quality of mealworm larvae processed by rack oven drying, vacuum drying or freeze drying, respectively. Proximate composition and fatty acid profile were comparable between the dried larvae. In contrast, larvae color impressions and volatile compound profiles were very much dependent on processing procedure. High-temperature rack oven drying caused pronounced darkening with rather low content of volatiles, pointing toward the progress of Maillard reaction. On the other hand, vacuum drying or freeze drying led to enrichment of volatile Maillard reaction and lipid oxidation intermediates, whose actual sensory relevance needs to be clarified in the future. Beyond sensory and visual importance drying intermediates have to be considered with regard to their metal ion chelating ability; in particular for essential trace elements such as Zn2+. This study found comparable total zinc contents for the differently dried mealworm samples. However, dried larvae, in particular after rack oven drying, had only low zinc accessibility, which was between 20% and 40%. Therefore, bioaccessibility rather than total zinc has to be considered when their contribution to meeting the nutritional requirements for zinc in humans and animals is evaluated. KW - Food PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-476320 DO - https://doi.org/10.3390/insects10040084 SN - 2075-4450 VL - 10 IS - 4 SP - 84, 1 EP - 13 PB - MDPI AN - OPUS4-47632 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kotthoff, Lisa A1 - Keller, Julia A1 - Lörchner, Dominique A1 - Mekonnen, Tessema F. A1 - Koch, Matthias T1 - Transformation products of organic contaminants and residues - Overview of current simulation methods N2 - The formation of transformation products (TPs) from contaminants and residues is becoming an increasing focus of scientific community. All organic compounds can form different TPs, thus demonstrating the complexity and interdisciplinarity of this topic. The properties of TPs could stand in relation to the unchanged substance or be more harmful and persistent. To get important information about the generated TPs, methods are needed to simulate natural and manmade transformation processes. Current tools are based on metabolism studies, photochemical methods, electrochemical methods, and Fenton's reagent. Finally, most transformation processes are based on redox reactions. This review aims to compare these methods for structurally different compounds. The groups of pesticides, pharmaceuticals, brominated flame retardants, and mycotoxins were selected as important residues/contaminants relating to their worldwide occurrence and impact to health, food, and environmental safety issues. Thus, there is an increasing need for investigation of transformation processes and identification of TPs by fast and reliable methods. KW - Transformation product KW - Electrochemistry KW - Photochemistry KW - Fenton’s reagent PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-474108 DO - https://doi.org/10.3390/molecules24040753 SN - 1420-3049 VL - 24 IS - 4 SP - 753, 1 EP - 23 PB - MDPI CY - Basel AN - OPUS4-47410 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dorgerloh, Ute A1 - Becker, Roland A1 - Kaiser, M. T1 - Evidence for the formation of difluoroacetic acid in chlorofluorocarbon-contaminated ground water N2 - The concentrations of difluoroacetic acid (DFA) and trifluoroacetic acid (TFA) in rainwater and surface water from Berlin, Germany resembled those reported for similar urban areas, and the TFA/DFA ratio in rainwater of 10:1 was in accordance with the literature. In contrast, nearby ground water historically contaminated with 1,1,2-trichloro-1,2,2-trifluoroethane (R113) displayed a TFA/DFA ratio of 1:3. This observation is discussed versus the inventory of microbial Degradation products present in this ground water along with the parent R113 itself. A microbial Transformation of chlorotrifluoroethylene (R1113) to DFA so far has not been reported for environmental media, and is suggested based on well-established mammalian metabolic pathways. KW - Fluoroacetic acid KW - DFA KW - TFA KW - Rainwater KW - Ground water KW - Degradation of refrigerants PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-475569 DO - https://doi.org/10.3390/molecules24061039 SN - 1420-3049 VL - 24 IS - 6 SP - 1039, 1 EP - 6 PB - MDPI CY - Basel AN - OPUS4-47556 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tarantini, A. A1 - Wegner, Karl David A1 - Dussert, F. A1 - Sarret, G. A1 - Beal, D. A1 - Mattera, L. A1 - Lincheneau, C. A1 - Proux, O. A1 - Truffier-Boutry, D. A1 - Moriscot, C. A1 - Gallet, B. A1 - Jouneau, P.-H. A1 - Reiss, P. A1 - Carriere, M. T1 - Physicochemical alterations and toxicity of InP alloyed quantum dots aged in environmental conditions: A safer by design evaluation N2 - Due to their unique optical properties, quantum dots (QDs) are used in a number of optoelectronic devices and are forecasted to be used in the near future for biomedical applications. The most popular QD composition consists of cadmium selenide (CdSe) or cadmium telluride (CdTe), which has been shown to pose health risks due to the release of toxic cadmium (Cd) ions. Due to similar optical properties but lower intrinsic toxicity, indium phosphide (InP) QDs have been proposed as a safer alternative. Nevertheless, investigations regarding their safety and possible toxicological effects are still in their infancy. The fate and toxicity of seven different water-dispersible indium (In) based QDs, either pristine or after ageing in a climatic chamber, was evaluated. The core of these QDs was composed of indium, zinc and phosphorus (InZnP) or indium, zinc, phosphorus and sulfur (InZnPS). They were assessed either as core-only or as core-shell QDs, for which the core was capped with a shell of zinc, selenium and sulfur (Zn(Se,S)). Their Surface was functionalized using either penicillamine or glutathione. In their pristine form, these QDs showed essentially no cytotoxicity. The particular case of InZnPS QD showed that core-shell QDs were less cytotoxic than core-only QDs. Moreover, surface functionalization with either penicillamine or glutathione did not appreciably influence cytotoxicity but affected QD stability. These QDs did not lead to over-accumulation of reactive oxygen species in exposed cells, or to any oxidative damage to cellular DNA. However, accelerated weathering in a climatic chamber led to QD precipitation and degradation, together with significant cytotoxic effects. Ageing led to dissociation of IneP and ZneS bonds, and to complexation of In Zn ions with carboxylate and/or phosphate moieties. These results show that InZnP and InZnPS alloyed QDs are safer alternatives to CdSe QDs. They underline the necessity to preserve as much as possible the structural integrity of QDs, for instance by developing more robust shells, in order to ensure their safety for future applications. KW - Indium phosphide KW - Safe by design KW - Toxicity KW - EXAFS PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-483070 DO - https://doi.org/10.1016/j.impact.2019.100168 VL - 14 SP - 100168-1 EP - 100168-13 PB - Elsevier AN - OPUS4-48307 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neumann, Patrick P. A1 - Kohlhoff, Harald A1 - Hüllmann, Dino A1 - Krentel, Daniel A1 - Kluge, Martin A1 - Dzierliński, M. A1 - Lilienthal, A. J. A1 - Bartholmai, Matthias T1 - Aerial-based gas tomography – from single beams to complex gas distributions N2 - In this paper, we present and validate the concept of an autonomous aerial robot to reconstruct tomographic 2D slices of gas plumes in outdoor environments. Our platform, the so-called Unmanned Aerial Vehicle for Remote Gas Sensing (UAV-REGAS), combines a lightweight Tunable Diode Laser Absorption Spectroscopy (TDLAS) gas sensor with a 3-axis aerial stabilization gimbal for aiming at a versatile octocopter. While the TDLAS sensor provides integral gas concentration measurements, it does not measure the distance traveled by the laser diode’s beam nor the distribution of gas along the optical path. Thus, we complement the set-up with a laser rangefinder and apply principles of Computed Tomography (CT) to create a model of the spatial gas distribution from a set of integral concentration measurements. To allow for a fundamental ground truth evaluation of the applied gas tomography algorithm, we set up a unique outdoor test environment based on two 3D ultrasonic anemometers and a distributed array of 10 infrared gas transmitters. We present results showing its performance characteristics and 2D plume reconstruction capabilities under realistic conditions. The proposed system can be deployed in scenarios that cannot be addressed by currently available robots and thus constitutes a significant step forward for the field of Mobile Robot Olfaction (MRO). KW - Aerial robot olfaction KW - Mobile robot olfaction KW - Gas tomography KW - TDLAS KW - Plume PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-487843 DO - https://doi.org/10.1080/22797254.2019.1640078 SP - 1 EP - 16 PB - Taylor & Francis CY - London AN - OPUS4-48784 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rastayesh, S. A1 - Long, Lijia A1 - Sørensen, J. D. A1 - Thöns, Sebastian T1 - Risk Assessment and Value of Action Analysis for Icing Conditions of Wind Turbines Close to Highways N2 - The paper presents research results from the Marie Skłodowska-Curie Innovative Training Network INFRASTAR in the field of reliability approaches for decision-making for wind turbines and bridges. This paper addresses the application of Bayesian decision analysis for installation of heating systems in wind turbine blades in cases where an ice detection system is already installed in order to allow wind turbines to be placed close to highways. Generally, application of ice detection and heating systems for wind turbines is very relevant in cases where the wind turbines are planned to be placed close to urban areas and highways, where risks need to be considered due to icing events, which may lead to consequences including human fatality, functional disruptions, and/or economic losses. The risk of people being killed in a car passing on highways near a wind turbine due to blades parts or ice pieces being thrown away in cases of overicing is considered in this paper. The probability of being killed per kilometer and per year is considered for three cases: blade parts thrown away as a result of a partial or total failure of a blade, ice thrown away in two cases, i.e., of stopped wind turbines and of wind turbines in operation. Risks due to blade parts being thrown away cannot be avoided, since low strengths of material, maintenance or manufacturing errors, mechanical or electrical failures may result in failure of a blade or blade part. The blade (parts) thrown away from wind turbines in operation imply possible consequences/fatalities for people near the wind turbines, including in areas close to highways. Similar consequences are relevant for ice being thrown away from wind turbine blades during icing situations. In this paper, we examine the question as to whether it is valuable to put a heating System on the blades in addition to ice detection systems. This is especially interesting in countries with limited space for placing wind turbines; in addition, it is considered if higher power production can be obtained due to less downtime if a heating system is installed. KW - Risk assessment KW - Value of action analysis KW - Icing conditions KW - Wind turbine KW - Blade PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-487805 DO - https://doi.org/10.3390/en12142653 VL - 12 IS - 14 SP - 2653-1 EP - 2653-15 PB - MDPI AN - OPUS4-48780 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Markwart, J. C. A1 - Battig, Alexander A1 - Kuckhoff, T. A1 - Schartel, Bernhard A1 - Wurm, F. R. T1 - First phosphorus AB2 monomer for flame-retardant hyperbranched polyphosphoesters: AB2vs. A2 + B3 N2 - Branched polymers are an important class of polymers with a high number of terminal groups, lower viscosity compared to their linear analogs and higher miscibility, which makes them especially interesting for flame retardant applications, where the flame retardants (FR) are blended with another polymer matrix. Hyperbranched polyphosphoesters (hbPPEs) are gaining more and more interest in the field of flame retardancy, as low molar mass FRs often have the disadvantage of blooming out or leaching, which is not desired in consumer products. Here, we present the first phosphorus-based AB2 monomer for the synthesis of hbPPEs and assess its flame-retardant performance in an epoxy resin compared to a hbPPE synthesized by an A2 + B3 approach. The hbPPE synthesized from an AB2 monomer exhibited a slightly higher performance compared to a similar hbPPE, which was prepared by A2 + B3 polyaddition, probably due to its higher phosphorus content. KW - Polyphosphoester KW - Hyperbranched KW - Flame retardant KW - Synthesis PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-497570 DO - https://doi.org/10.1039/c9py01156k SN - 1759-9962 VL - 10 IS - 43 SP - 5920 EP - 5930 PB - RSC AN - OPUS4-49757 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stajanca, Pavol A1 - Hicke, Konstantin A1 - Krebber, Katerina T1 - Distributed Fiberoptic Sensor for Simultaneous Humidity and Temperature Monitoring Based on Polyimide-Coated Optical Fibers N2 - Along temperature, humidity is one of the principal environmental factors that plays an important role in various application areas. Presented work investigates possibility of distributed fiberoptic humidity monitoring based on humidity-induced strain measurement in polyimide (PI)-coated optical fibers. Characterization of relative humidity (RH) and temperature response of four different commercial PI- and one acrylate-coated fiber was performed using optical backscattering reflectometry (OBR). The study addresses issues of temperature-humidity cross sensitivity, fiber response stability, repeatability, and the influence of annealing. Acrylate-coated fiber exhibited rather unfavorable nonlinear RH response with strong temperature dependence, which makes it unsuitable for humidity sensing applications. On the other hand, humidity response of PI-coated fibers showed good linearity with fiber sensitivity slightly decreasing at rising temperatures. In the tested range, temperature sensitivity of the fibers remained humidity independent. Thermal annealing was shown to considerably improve and stabilize fiber RH response. Based on performed analysis, a 20 m sensor using the optimal PI-coated fibers was proposed and constructed. The sensor uses dual sensing fiber configuration for mutual decoupling and simultaneous measurement of temperature and RH variations. Using OBR, distributed dual temperature-RH monitoring with cm spatial resolution was demonstrated for the first time. KW - Distributed humidity sensing KW - Fiberoptic sensors KW - Polyimide-coated optical fibers KW - Optical frequency-domain reflectometry KW - Dual sensing PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-498871 DO - https://doi.org/10.3390/s19235279 VL - 19 IS - 23 SP - 5279 PB - MDPI AN - OPUS4-49887 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hicke, Konstantin A1 - Eisermann, René A1 - Chruscicki, Sebastian T1 - Enhanced Distributed Fiber Optic Vibration Sensing and Simultaneous Temperature Gradient Sensing Using Traditional C-OTDR and Structured Fiber with Scattering Dots N2 - We present results demonstrating several beneficial effects on distributed fiber optic vibration sensing (DVS) functionality and performance resulting from utilizing standard single mode optical fiber (SMF) with femtosecond laser-inscribed equally-spaced simple scattering dots. This modification is particularly useful when using traditional single-wavelength amplitude-based coherent optical time domain reflectometry (C-OTDR) as sensing method. Local sensitivity is increased in quasi-distributed interferometric sensing zones which are formed by the fiber segments between subsequent pairs of the scattering dots. The otherwise nonlinear transfer function is overwritten with that of an ordinary two-beam interferometer. This linearizes the phase response to monotonous temperature variations. Furthermore, sensitivity fading is mitigated and the demodulation of low-frequency signals is enabled. The modification also allows for the quantitative determination of local temperature gradients directly from the C-OTDR intensity traces. The dots’ reflectivities and thus the induced attenuation can be tuned via the inscription process parameters. Our approach is a simple, robust and cost-effective way to gain these sensing improvements without the need for more sophisticated interrogator technology or more complex fiber structuring, e.g., based on ultra-weak FBG arrays. Our claims are substantiated by experimental evidence. KW - Fiber optic sensors KW - Distributed vibration sensing KW - DVS KW - Distributed temperature gradient sensing KW - DTGS KW - C-OTDR KW - Phase-sensitive KW - OTDR KW - Fiber structuring KW - Fs-inscription PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-499281 DO - https://doi.org/10.3390/s19194114 VL - 19 IS - 19 SP - 4114 PB - MDPI CY - Basel, Switzerland AN - OPUS4-49928 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Markwart, J. C. A1 - Battig, Alexander A1 - Velencoso, M. M. A1 - Pollok, D. A1 - Schartel, Bernhard A1 - Wurm, F. R. T1 - Aromatic vs. Aliphatic Hyperbranched Polyphosphoesters as Flame Retardants in Epoxy Resins N2 - The current trend for future flame retardants (FRs) goes to novel efficient halogen-free materials, due to the ban of several halogenated FRs. Among the most promising alternatives are phosphorus-based FRs, and of those, polymeric materials with complex shape have been recently reported. Herein, we present novel halogen-free aromatic and aliphatic hyperbranched polyphosphoesters (hbPPEs), which were synthesized by olefin Metathesis polymerization and investigated them as a FR in epoxy resins. We compare their efficiency (aliphatic vs. aromatic) and further assess the differences between the monomeric compounds and the hbPPEs. The decomposition and vaporizing behavior of a compound is an important factor in its flame-retardant behavior, but also the interaction with the pyrolyzing matrix has a significant influence on the performance. Therefore, the challenge in designing a FR is to optimize the chemical structure and its decomposition pathway to the matrix, with regards to time and temperature. This behavior becomes obvious in this study, and explains the superior gas phase activity of the aliphatic FRs. KW - Phosphorus KW - Metathesis KW - Dendritic KW - Cone calorimeter KW - Fire test PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-494535 DO - https://doi.org/10.3390/molecules24213901 SN - 1420-3049 VL - 24 IS - 21 SP - 3901 PB - MDPI AN - OPUS4-49453 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Habib, Abdel Karim A1 - Schalau, Bernd T1 - Pool evaporation - experimental data collection and modelling N2 - When handling flammable or toxic liquids or liquefied gases, the occurrence of a leakage and formation of a liquid pool is a scenario to be considered for risk assessment. Several models are available for the estimation of the evaporating mass flow, but only a very reduced number of experimental data is available for Validation purposes. In the last years, the Federal Institute for Materials Research and Testing (BAM) in Berlin, Germany, carried out pool Evaporation experiments with different substances in basins with a Diameter ranging from 0,50 m to 1 m mainly on open air test sites with a built up (inner city) and a non-built-up (flat terrain) topography, but also in an enclosed space. The resulting experimental data sets cover a range of vapor pressures from 0,1 bar to 0,94 bar. The aim of this work is to make the füll data set publicly available and to provide a description of the experimental boundary conditions. Based on these data, a Validation of existing pool Evaporation models has been carried out and eventually led to a new formulation of an evaporation model, which is also presented here, covering the whole ränge from low wind speeds up to high vapor pressures. KW - Lache KW - Verdunstung KW - Verdampfung KW - Dampfdruck KW - Windgeschwindigkeit PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-491826 DO - https://doi.org/10.1002/ceat.201800093 VL - 42 IS - 11 SP - 2450 EP - 2457 PB - WILEY‐VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-49182 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sarma, Dominik A1 - Carl, Peter A1 - Climent Terol, Estela A1 - Schneider, Rudolf A1 - Rurack, Knut T1 - Multifunctional polystyrene core/silica shell microparticles with antifouling properties for bead-based multiplexed and quantitative analysis N2 - Commercial bead-based assays are commonly built upon polystyrene particles. The polymeric carrier can be encoded with organic dyes and has ideal material properties for cytometric applications such as low density and high refractive index. However, functional groups are conventionally integrated during polymerization and subsequent modification is limited to the reactivity of those groups. Additionally, polystyrene as the core material leads to many hydrophobic areas still being present on the beads’ surfaces even after functionalization, Rendering the particles prone to nonspecific adsorption during an application. The latter calls for several washing steps and the use of additives in (bio)analytical assays. In this contribution, we show how these limitations can be overcome by using monodisperse polystyrene (PS) core/silica (SiO2) shell particles (SiO2@PS). Two different hydrophobic BODIPY (boron−dipyrromethene) dyes were encapsulated inside a poly(vinylpyrrolidone) (PVP) -stabilized polystyrene core in different concentrations to create 5-plex arrays in two separate detection channels of a cytometer. A subsequent modification of the silica shell with an equimolar APTES/PEGS (aminopropyltriethoxysilane/polyethylene glycol silane) blend added multifunctional properties to the hybrid core/Shell microparticles in a single step: APTES provides amino groups for the attachment of a caffeine derivative (as a hapten) to create antigen-coupled microspheres; the PEG moiety effectively suppresses nonspecific binding of antibodies, endowing the surface with antifouling properties. The particles were applied in a competitive fluorescence immunoassay in suspension, and a highly selective wash-free assay for the detection of caffeine in beverages was developed as a proof of concept. KW - Core−shell particles KW - Bead-based assay KW - Multiplex KW - Antifouling surface KW - Mixed surface PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-472931 UR - https://pubs.acs.org/doi/10.1021/acsami.8b10306 DO - https://doi.org/10.1021/acsami.8b10306 SN - 1944-8244 VL - 11 IS - 1 SP - 1321 EP - 1334 PB - American Chemical Society CY - Online Library AN - OPUS4-47293 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yadav, Anur A1 - Iost, R. M. A1 - Neubert, T. J. A1 - Baylan, S. A1 - Schmid, Thomas A1 - Balasubramanian, Kannan T1 - Selective electrochemical functionalization of the graphene edge N2 - We present a versatile and simple method using electrochemistry for the exclusive functionalization of the edge of a graphene monolayer with metal nanoparticles or polymeric amino groups. The attachment of metal nanoparticles allows us to exploit surface-enhanced Raman scattering to characterize the chemistry of both the pristine and the functionalized graphene edge. For the pristine patterned graphene edge, we observe the typical edge-related modes, while for the functionalized graphene edge we identify the chemical structure of the functional layer by vibrational fingerprinting. The ability to obtain single selectively functionalized graphene edges routinely on an insulating substrate opens an avenue for exploring the effect of edge chemistry on graphene properties systematically. KW - Graphene KW - Nanoparticles KW - Nanosciences KW - Surface-enhanced Raman scattering KW - Atomic force microscopy PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-474357 DO - https://doi.org/10.1039/C8SC04083D SN - 2041-6520 VL - 10 IS - 3 SP - 936 EP - 942 PB - Royal Society of Chemistry AN - OPUS4-47435 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kalbe, Ute A1 - Lehnik-Habrink, Petra A1 - Bandow, Nicole A1 - Sauer, Andreas T1 - Validation of European horizontal methods for the analysis of PAH, PCB and dioxins in sludge, treated biowaste and soil N2 - Draft standards for the determination of organic pollutants in the solid matter of environmental matrices such as sludge, treated biowaste and soil have been basically developed in the framework of the European standardization project HORIZONTAL. A research project financed by the German Federal Environment Agency was initiated to finalize some of these CEN standard drafts, since fully validated standard procedures are crucial for the evaluation of their reliability in the context of implementation in legislation on environmental health. Approach: Appropriate test materials (< 2mm particle size) were prepared and homogenized from contaminated soils, sludge and treated biowaste containing polycyclic aromatic hydrocarbons (PAH), polychlorinated biphenyls (PCB), dioxins, furans and dioxin-like-PCB and served, along with reference solutions, as the basis for international interlaboratory comparisons. Performance data of three analytical standard procedures were obtained by the statistical evaluation of results received from 11 to 29 participants per test material. Results: The overall variation coefficients of reproducibility (between-lab standard deviations) for the sum parameters were roughly between 10 and 35 %. The variation coefficients of repeatability (within-lab standard deviations) range between 3 % and 8 % and show no trend considering the substance groups or matrices. The highest coefficients of reproducibility were found for the analysis of PAHs, which were between 26 and 35 %, depending on the matrix, whereas 7-17 % reproducibility was observed for toxicity equivalents (TEQ) comprising dioxins, furans and dl-PCB. Conclusions: Overall, the results confirm that the procedures described in the Technical Specifications are fit for purpose for all three matrices and that the feasibility of the HORIZONTAL approach, to cover several matrices with one standard per analyte, was thereby proven. KW - Standardization KW - Analytical methods KW - Organic contaminants KW - Validation trial KW - Interlaboratory comparison PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-479914 DO - https://doi.org/10.1186/s12302-019-0211-3 SN - 2190-4715 VL - 31 SP - 29, 1 EP - 10 PB - Springer CY - Berlin, Heidelberg AN - OPUS4-47991 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kern, Simon A1 - Wander, Lukas A1 - Meyer, Klas A1 - Guhl, Svetlana A1 - Gottu Mukkula, A. R. A1 - Holtkamp, M. A1 - Salge, M. A1 - Fleischer, C. A1 - Weber, N. A1 - Engell, S. A1 - Paul, Andrea A1 - Pereira Remelhe, M. A1 - Maiwald, Michael T1 - Flexible automation with compact NMR spectroscopy for continuous production of pharmaceuticals N2 - Modular plants using intensified continuous processes represent an appealing concept for the production of pharmaceuticals. It can improve quality, safety, sustainability, and profitability compared to batch processes; besides, it enables plug-and-produce reconfiguration for fast product changes. To facilitate this flexibility by real-time quality control, we developed a solution that can be adapted quickly to new processes and is based on a compact nuclear magnetic resonance (NMR) spectrometer. The NMR sensor is a benchtop device enhanced to the requirements of automated chemical production including robust evaluation of sensor data. Beyond monitoring the product quality, online NMR data was used in a new iterative optimization approach to maximize the plant profit and served as a reliable reference for the calibration of a near-infrared (NIR) spectrometer. The overall approach was demonstrated on a commercial-scale pilot plant using a metal-organic reaction with pharmaceutical relevance. KW - NMR Spectroscopy KW - NIR Spectroscopy KW - Real-time process monitoring KW - Real-time quality control KW - Continuous processes KW - CONSENS KW - Data Fusion PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-480623 DO - https://doi.org/10.1007/s00216-019-01752-y SN - 1618-2642 SN - 1618-2650 VL - 411 IS - 14 SP - 3037 EP - 3046 PB - Springer Nature CY - Heidelberg AN - OPUS4-48062 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gotor, Raúl A1 - Bell, Jérémy A1 - Rurack, Knut T1 - Tailored fluorescent solvatochromic test strips for quantitative on-site detection of gasoline fuel adulteration N2 - Gasoline adulteration is a frequent problem world-wide, because of the chance of quick, maximized profits. However, addition of cheaper ethanol or hydrocarbons like kerosene does not only result in economic damage but also poses problems for vehicles and the environment. To enable law enforcement forces, customers or enterprises to uncover such a fraudulent activity directly upon suspicion and without the need to organize for sampling and laboratory analysis, we developed a simple strip-based chemical test. Key to the favorable performance was the dedicated materials tailoring, which led to test strips that consisted of a cellulose support coated with silica, passivated with hexamethyldisilazane and functionalized covalently with a molecular probe. The probe fluoresces brightly across a broad solvent polarity range, enabling reliable quantitative measurements and data analysis with a conventional smartphone. The assays showed high reproducibility and accuracy, allowing not only for the detection of gasoline adulteration but also for the on-site monitoring of the quality of commercial E10 gasoline. KW - Gasoline KW - Adulteration KW - Test strips KW - Benzin KW - Teststreifen KW - Fluorescence KW - Cellulose KW - Zellulose KW - Fluoreszenz PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-479231 UR - https://pubs.rsc.org/en/content/articlelanding/2019/tc/c8tc04818e DO - https://doi.org/10.1039/C8TC04818E SN - 2050-7526 VL - 7 IS - 8 SP - 2250 EP - 2256 PB - Royal Society of Chemistry CY - London, UK AN - OPUS4-47923 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Elert, Anna Maria A1 - Kanerva, M A1 - Puolakka, A A1 - Takala, T.M. A1 - Mylläri, V A1 - Jönkkäri, I A1 - Sarlin, E A1 - Seitsonen, J A1 - Ruokolainen, J A1 - Saris, P A1 - Vuorinen, J T1 - Antibacterial polymer fibres by rosin compounding and melt-spinning N2 - The antibacterial features of natural pine/spruce rosin are well established, yet the functionality in various thermoplastics has not been surveyed. This work focuses on the processing of industrial grade purified rosin mixed with polyethylene (PE), polypropylene (PP), polylactic acid (PLA), polyamide (PA) and corn starch based biopolymer (CS). Homopolymer masterbatches were extrusion-compounded and melt-spun to form fibres for a wide range of products, such as filters, reinforcements, clothing and medical textiles. Due to the versatile chemical structure of rosin, it was observed compatible with all the selected polymers. In general, the rosin-blended systems were shear-thinning in a molten condition. The doped fibres spun of PE and PP indicated adequate melt-spinning capability and proper mechanical properties in terms of ultimate strength and Young's modulus. The antibacterial response was found dependent on the selected polymer. Especially PE with a 10 wt% rosin content showed significant antibacterial effects against Escherichia coli DH5α and Staphylococcus aureus ATCC 12598 when analysed in the Ringer's solution for 24 h. KW - Rosin KW - Antibacterial KW - Thermoplastics PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-481785 DO - https://doi.org/10.1016/j.mtcomm.2019.05.003 SN - 2352-4928 VL - 20 SP - 527 EP - 527 PB - Elsevier AN - OPUS4-48178 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rabe, Sebastian A1 - Sánchez-Olivares, G. A1 - Pérez-Chávez, R. A1 - Schartel, Bernhard T1 - Natural keratin and coconut fibres from industrial wastes in flame retarded thermoplastic starch biocomposites N2 - Natural keratin fibres derived from Mexican tannery waste and coconut fibres from coconut processing waste were used as fillers in commercially available, biodegradable thermoplastic starch-polyester blend to obtain sustainable biocomposites. The morphology, rheological and mechanical properties as well as pyrolysis, flammability and forced flaming combustion behaviour of those biocomposites were investigated. In order to open up new application areas for these kinds of biocomposites, ammonium polyphosphate (APP) was added as a flame retardant. Extensive flammability and cone calorimeter studies revealed a good flame retardance effect with natural fibres alone and improved effectiveness with the addition of APP. In fact, it was shown that replacing 20 of 30 wt. % of APP with keratin fibres achieved the same effectiveness. In the case of coconut fibres, a synergistic effect led to an even lower heat release rate and total heat evolved due to reinforced char residue. This was confirmed via scanning electron microscopy of the char structure. All in all, these results constitute a good approach towards sustainable and biodegradable fibre reinforced biocomposites with improved flame retardant properties. KW - Biomaterials KW - Biodegradable KW - Calorimetry KW - Composites KW - Flame retardance PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-472518 DO - https://doi.org/10.3390/ma12030344 SN - 1996-1944 VL - 12 IS - 3 SP - 344, 1 EP - 24 PB - MDPI AN - OPUS4-47251 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sut, Aleksandra A1 - Metzsch-Zilligen, E. A1 - Großhauser, M. A1 - Pfaendner, R. A1 - Schartel, Bernhard T1 - Synergy between melamine cyanurate, melamine polyphosphate and aluminum diethylphosphinate in flame retarded thermoplastic polyurethane N2 - The multicomponent flame retardant system of melamine polyphosphate (MPP), melamine cyanurate (MC) and aluminum diethylphosphinate (AlPi) is proposed and investigated for thermoplastic polyurethane (TPU). The synergy between those additives and the resulting superior fire performance are discussed. Systematically varied sets of flame retarded TPU with various MPP/MC/AlPi ratios were investigated in terms of fire behavior, pyrolysis products and mechanical properties. The total amount of the additives was always 30 wt.-%. Further, the influence of various AlPi concentrations was investigated. The optimal MPP:MC ratio was determined while keeping the amount of AlPi constant. The combination of 8 wt.-% MPP, 12 wt.-% MC and 10 wt.-% is proposed as the most promising halogen free flame retardant formulation for TPU, because it yielded a reduction in PHRR from 2660 kW/m2 (TPU) to 452 kW/m2 and enabled V-0 classification in the UL 94 test. Combinations of MPP and MC as well a high concentration of AlPi are beneficial for the mechanical properties e.g. tensile strength and elongation at break of the formulations and could be a strong competitor to commercial flame retarded TPUs. KW - Thermoplastic polyurethane KW - Synergy KW - Melamine cyanurate KW - Melamine polyphosphate KW - Aluminum diethylphosphinate KW - Rapid mass calorimeter PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-472523 DO - https://doi.org/10.1016/j.polymertesting.2019.01.001 SN - 0142-9418 VL - 74 SP - 196 EP - 204 PB - Elsevier Ltd. AN - OPUS4-47252 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Baer, Wolfram T1 - Chunky graphite in ferritic spheroidal graphite cast iron: Formation, prevention, characterization, impact on properties – An overview N2 - Ferritic spheroidal graphite cast iron (SGI) materials have a remarkable technical poten-tial and economic impact in modern industry. These features are closely related to the question of how the cast materials can be produced without structural defects and graphite degenerations such as for example chunky graphite. Although the chunky graphite degeneration superficially seems to be well known, its metallurgical background is still controversially discussed, appropriate field-tested non-destructive tools for its quantification in castings are lacking and the knowledge on its impact on material properties is fairly limited. Addressing this status, the article is providing a current overview on the subject. Existing theories on formation and growth mechanisms of chunky graphite are briefly reviewed. Furthermore, from a metallurgical point of view, causes for the appearance of chunky graphite as well as preventive measures are concisely summarized. Particular attention is paid to the morphology of chunky graphite and how it can be characterized by destructive and non-destructive techniques. Special emphasis was laid on providing a comprehensive overview on the impact of chunky graphite on strength, ductility, fatigue limit, fatigue crack growth rate as well as fracture tough-ness of ferritic SGI materials based on experimental data. Moreover, conclusions for the assessment of castings affected by chunky graphite are drawn. KW - Characterization KW - Ferritic spheroidal graphite cast iron KW - Chunky graphite KW - Properties KW - Formation KW - Prevention PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-499972 DO - https://doi.org/10.1007/s40962-019-00363-8 SN - 1939-5981 SN - 2163-3193 VL - 14 IS - 2 SP - 454 EP - 488 PB - Springer Verlag AN - OPUS4-49997 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mezera, M. A1 - Bonse, Jörn A1 - Römer, G.R.B.E. T1 - Influence of Bulk Temperature on Laser-Induced Periodic Surface Structures on Polycarbonate N2 - In this paper, the influence of the bulk temperature (BT) of Polycarbonate (PC) on the occurrence and growth of Laser-induced Periodic Surface Structures (LIPSS) is studied. Ultrashort UV laser pulses with various laser peak fluence levels F_0 and various numbers of overscans (N_OS) were applied on the surface of pre-heated Polycarbonate at different bulk temperatures. Increased BT leads to a stronger absorption of laser energy by the Polycarbonate. For N_OS < 1000 High Spatial Frequency LIPSS (HSFL), Low Spatial Frequency LIPSS perpendicular (LSFL-I) and parallel (LSFL-II) to the laser polarization were only observed on the rim of the ablated tracks on the surface but not in the center of the tracks. For N_OS ≥ 1000 , it was found that when pre-heating the polymer to a BT close its glass transition temperature (T_g), the laser fluence to achieve similar LIPSS as when processed at room temperature decreases by a factor of two. LSFL types I and II were obtained on PC at a BT close to T_g and their periods and amplitudes were similar to typical values found in the literature. To the best of the author’s knowledge, it is the first time both LSFL types developed simultaneously and consistently on the same sample under equal laser processing parameters. The evolution of LIPSS from HSFL, over LSFL-II to LSFL I, is described, depending on laser peak fluence levels, number of pulses processing the spot and bulk temperature. KW - Laser-induced periodic surface structures (LIPSS) KW - Polycarbonate KW - Bulk temperature KW - Ultrashort laser pulses PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-498242 UR - https://www.mdpi.com/2073-4360/11/12/1947 DO - https://doi.org/https://doi.org/10.3390/polym11121947 SN - 2073-4360 VL - 11 IS - 12 SP - 1947 PB - MDPI CY - Basel, Switzerland AN - OPUS4-49824 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Oesch, Tyler A1 - Weise, Frank A1 - Meinel, Dietmar A1 - Gollwitzer, Christian T1 - Quantitative in-situ analysis of water transport in concrete completed using X-ray computed tomography N2 - This paper describes a novel methodology for quantitative in-situ moisture measurement without tracking agents using X-ray computed tomography (XCT). The high levels of grey-scale precision required for the measurement of moisture without tracking agents resulted in the need for an additional image calibration procedure to correct for water-related X-ray scattering and for equipment-variability related artefacts arising during in-situ testing. This calibration procedure was developed on the basis of existing principles of XCT image cor-rection. Resulting images of moisture distribution exhibit a high level of agreement with expected material behaviour. This research demonstrated that XCT can be successfully used to measure both moisture-front movement over time and changes in 3D moisture distribution within samples. This approach to moisture measurement lays the groundwork for the planned future investigation of the interaction between cracking induced by varying chemical and mechanical processes and water transport in concrete. KW - X-ray computed tomography (XCT) KW - In-situ testing KW - Water transport KW - Quantitative moisture measurement KW - Concrete PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-474395 DO - https://doi.org/10.1007/s11242-018-1197-9 SN - 1573-1634 VL - 127 IS - 2 SP - 371 EP - 389 PB - Springer Netherlands AN - OPUS4-47439 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lenz, J. A1 - Pospiech, D. A1 - Paven, M. A1 - Albach, R. W. A1 - Günther, Martin A1 - Schartel, Bernhard A1 - Voit, B. T1 - Improving the Flame Retardance of Polyisocyanurate Foams by Dibenzo[d,f][1,3,2]dioxaphosphepine 6-Oxide-Containing Additives N2 - A series of new flame retardants (FR) based on dibenzo[d,f][1,3,2]dioxaphosphepine 6-oxide (BPPO) incorporating acrylates and benzoquinone were developed previously. In this study, we examine the fire behavior of the new flame retardants in polyisocyanurate (PIR) foams. The foam characteristics, thermal decomposition, and fire behavior are investigated. The fire properties of the foams containing BPPO-based derivatives were found to depend on the chemical structure of the substituents. We also compare our results to state-of-the-art non-halogenated FR such as triphenylphosphate and chemically similar phosphinate, i.e. 9,10-dihydro-9-oxa-10- phosphaphenanthrene-10-oxide (DOPO), based derivatives to discuss the role of the phosphorus oxidation state. KW - Polyisocyanurate KW - Dibenzo[d,f][1,3,2]dioxaphosphepine 6-oxide KW - Phospha-Michael addition KW - Flame retardant KW - Foams PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-485590 DO - https://doi.org/10.3390/polym11081242 SN - 2073-4360 VL - 11 IS - 8 SP - Article 1242 PB - MDPI AN - OPUS4-48559 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Battig, Alexander A1 - Markwart, J. C. A1 - Wurm, F. R. A1 - Schartel, Bernhard T1 - Hyperbranched phosphorus flame retardants: multifunctional additives for epoxy resins N2 - We successfully synthesized multifunctional P-based hyperbranched polymeric flame retardants (hb-FRs) with varying oxygen-to-nitrogen (O : N) content and characterized them via 1H and 31P NMR and GPC. Their miscibility in epoxy resins (EP) and impact on glass-transition temperatures (Tg) were determined via differential scanning calorimetry (DSC). Using thermogravimetric and evolved gas Analysis (TGA, TG-FTIR), pyrolysis gas chromatography/mass spectrometry (Py-GC-MS), hot stage FTIR, flammability tests UL-94 and LOI, fire testing via cone calorimetry, residue analysis via scanning electron microscopy (SEM) and elemental analysis, detailed decomposition mechanisms and modes of action are proposed. hb-polymeric FRs have improved miscibility and thermal stability, leading to high FR performance even at low loadings. Polymeric, complex FRs increase flame retardancy, mitigate negative effects of low molecular weight variants, and can compete with commercial aromatic FRs. The results illustrate the role played by the chemical structure in flame retardancy and highlight the potential of hb-FRs as multifunctional additives. KW - Flame retardant KW - Hyperbranched PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-486589 DO - https://doi.org/10.1039/c9py00737g SN - 1759-9962 SN - 1759-9954 VL - 10 IS - 31 SP - 4346 EP - 4358 PB - RSC AN - OPUS4-48658 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bartelmeß, Jürgen A1 - Valderrey, Virginia A1 - Rurack, Knut T1 - Development of a “Turn-on” Fluorescent Probe-Based Sensing System for Hydrogen Sulfide in Liquid and Gas Phase N2 - A “turn-on” fluorescence sensing system based on a BODIPY-cobaloxime complex for the detection of H2S in liquid and gas phase was developed. To that aim, two cobaloxime complexes bearing an axial pyridyl-BODIPY ligand were initially evaluated as sensitive fluorescent HS− indicators in aqueous solution. The sensing mechanism involves the selective substitution of the BODIPY ligand by the HS− anion at the cobalt center, which is accompanied by a strong fluorescence enhancement. The selection of a complex with an ideal stability and reactivity profile toward HS− relied on the optimal interaction between the cobalt metal-center and two different pyridyl BODIPY ligands. Loading the best performing BODIPY-cobaloxime complex onto a polymeric hydrogel membrane allowed us to study the selectivity of the probe for HS− against different anions and cysteine. Successful detection of H2S by the fluorescent “light-up” membrane was not only accomplished for surface water but could also be demonstrated for relevant H2S concentrations in gas phase. KW - Sulfide sensing KW - Fluorescence KW - BODIPYs KW - Cobaloxime complex KW - Gas sensing PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-492186 DO - https://doi.org/10.3389/fchem.2019.00641 SN - 2296-2646 VL - 7 SP - Art. Nr. 641 PB - Frontiers Media CY - Lausanne AN - OPUS4-49218 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Borzekowski, Antje A1 - Anggriawan, R. A1 - Auliyati, M. A1 - Kunte, Hans-Jörg A1 - Koch, Matthias A1 - Rohn, S. A1 - Karlovsky, P. A1 - Maul, Ronald T1 - Formation of Zearalenone Metabolites in Tempeh Fermentation N2 - Tempeh is a common food in Indonesia, produced by fungal fermentation of soybeans using Rhizopus sp., as well as Aspergillus oryzae, for inoculation. Analogously, for economic reasons, mixtures of maize and soybeans are used for the production of so-called tempeh-like products. For maize, a contamination with the mycoestrogen zearalenone (ZEN) has been frequently reported. ZEN is a mycotoxin which is known to be metabolized by Rhizopus and Aspergillus species. Consequently, this study focused on the ZEN transformation during tempeh fermentation. Five fungal strains of the genera Rhizopus and Aspergillus, isolated from fresh Indonesian tempeh and authentic Indonesian inocula, were utilized for tempeh manufacturing from a maize/soybean mixture (30:70) at laboratory-scale. Furthermore, comparable tempeh-like products obtained from Indonesian markets were analyzed. Results from the HPLC-MS/MS analyses show that ZEN is intensely transformed into its metabolites alpha-zearalenol (alpha-ZEL), ZEN-14-sulfate, alpha-ZEL-sulfate, ZEN-14-glucoside, and ZEN-16-glucoside in tempeh production. alpha-ZEL, being significantly more toxic than ZEN, was the main metabolite in most of the Rhizopus incubations, while in Aspergillus oryzae fermentations ZEN-14-sulfate was predominantly formed. Additionally, two of the 14 authentic samples were contaminated with ZEN, alpha-ZEL and ZEN-14-sulfate, and in two further samples, ZEN and alpha-ZEL, were determined. Consequently, tempeh fermentation of ZEN-contaminated maize/soybean mixture may lead to toxification of the food item by formation of the reductive ZEN metabolite, alpha-ZEL, under model as well as authentic conditions. KW - Modified mycotoxins KW - Zearalenone sulfate KW - a-zearalenol KW - Food fermentation KW - Rhizopus and Aspergillus oryzae PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-491126 DO - https://doi.org/10.3390/molecules24152697 VL - 24 IS - 15 SP - 2697 PB - MDPI AN - OPUS4-49112 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rahrig, M. A1 - Torge, Manfred T1 - 3D inspection of the restoration and conservation of stained glass windows using high resolution structured light scanning N2 - The initial focus of this research was on the development of a general workflow for the documentation and monitoring of historical stained glass windows using structured light scanning. Therefore windows from different churches, time periods and with different corrosion and damage phenomena were scanned before and after conservation measures. To evaluate the execution of the restoration measures the data was compared using 3D inspection software to examine the differences in geometry between the two scans. Various problems had to be solved, for example, how to deal with heavily reflective surfaces and the extreme contrast between light and dark surfaces, as seen in the borders between ‘Schwarzlot’ painting and plain glass. The application of materials for matting the surfaces, such as Cyclododecane spray, was impossible due to the high accuracy of the surface measurement required for 3D inspection. Regarding the contrast differences of the surfaces, the creation of exposure fusions and the use of polarization filters to reduce reflections were tested. In addition to the general problems encountered when recording translucent surfaces, the historical glasses caused additional problems in calculating surface comparisons. For example, the windows have to be moved and turned around several times, both during the conservation process and while scanning, causing deformations of the geometry due to the flexible lead rods allowing a certain degree of movement. T2 - 27th CIPA International Symposium “Documenting the past for a better future” CY - Ávila, Spain DA - 01.09.2019 KW - Stained glass KW - Restoration and conservation KW - Structured light scanning KW - 3D inspection KW - Glass scanning PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-491286 DO - https://doi.org/10.5194/isprs-archives-XLII-2-W15-965-2019 VL - XLII-2/W15 SP - 965 EP - 972 PB - International Society of Photogrammetry and Remote Sensing (ISPRS) CY - Hannover AN - OPUS4-49128 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, Q. A1 - Zheng, M. A1 - Huang, Y. A1 - Kunte, Hans-Jörg A1 - Wang, X. A1 - Liu, Y. A1 - Zheng, C. T1 - Long term corrosion estimation of carbon steel, titanium and its alloy in backfill material of compacted bentonite for nuclear waste repository N2 - The container of high-level radioactive waste (HLRW) being in deep geological disposal, the backfill material is needed to serve as the second defense for HLRW and the highly compacted bentonite is generally selected. As the time goes, the underground water will infiltrate the backfill, causing the corrosion of materials for the building of containers in the formed electrolyte. Carbon steel, titanium and its alloy are the potential candidate materials for the fabrication of HLRW containers. The current investigation aims at assessing the safety of HLRW container in deep geological disposal for hundreds of thousands of years and facilitating the material selection for future Container fabrication by estimating their corrosion behavior in compacted bentonite with a series of moisture content at different temperatures through electrochemical methods including open circuit potential (OCP), electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization curve (PC) measurements. The corrosion rates were estimated for a carbon steel, a pure titanium and a titanium alloy in compacted Gaomiaozi Bentonite infiltrated with simulated underground water in Beishan area of China over an expected disposal period up to 106 years respectively, showing that titanium and its alloy are more reliable materials for building HLRW containers than carbon steel. KW - Issues KW - Disposal KW - Performance KW - Moisture KW - Lifetime KW - Water KW - Model PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-492413 DO - https://doi.org/10.1038/s41598-019-39751-9 SN - 2045-2322 VL - 9 SP - 3195 PB - Nature Publishing Group AN - OPUS4-49241 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -