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Paper des Monats
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An extraordinary deviceless self-sustained oscillatory diffusive burning is observed in tert-butyl peroxybenzoate (TBPB) (technical pure) and hybrid fuel, i.e., TBPB and kerosene (both 50%) flames when burned in form of pool fires. Such oscillations or more precisely self-sustained deviceless control of mass burning (flow) is not reported till date. Generally, devices comprising electronic control system and/or mechanical means (valves) are necessary to produce such oscillatory burning or control of fuel flow. This unique oscillation is strongly recorded for pool diameters of 6 cm ≤ d ≤ 11 cm beyond which the effect was weakened and unseen (hid) visually. The fuel regression (loss) takes place in irregular time steps and is formulated in form of a step function. The variation in fuel mass burning rates, visible flame lengths and radiation heat fluxes with time are measured as respective representatives of oscillations. The periodicity in the strongest oscillations in relative visible flame lengths is investigated and the measured data are found to be best fitted in sinusoidal form. Both, chemical and thermal effects are shown to be possibly responsible for such effects. Furthermore, a theory is offered to characterise similar effect showing fuels.
In the late 1980s, a new type of corrosion appeared in drinking water installations where galvanized steel pipes failed forming a deep groove with no corrosion at the other surfaces. The reason was discussed quite fiercely between failure analysts and material suppliers. In the end the discussion lead to the solution: inductive welded pipes of a certain sulphur content were prone to selective corrosion. The history of the arguments is discussed using old communications between Wilhelm Schwenk and Wolfgang Stichel, who later published the results in a paper unfortunately only I german.
Thus the knowledge got lost and new cases based on the same material problems are observed in application of so-called C-Steel piping systems. Failure cases are shown.
Analytical Sciences has developed from Ostwald’s “unentbehrlichen Dienstmagd” to a chemical discipline at the core of many of today’s fundamental and applied scientific problems and innovations. An atomic or molecular understanding of basic processes in chemistry, soft matter physics, materials and life science is enabled only through new analytical methods and instrumentation. Similar observations can be found for pressing sociopolitical conflicts of the future: A rational discussion of global climate change or new energy sources is only possible with reliable analytical results. Progress in Analytical Sciences is only possible if the underlying interdisciplinary character is acknowledged and valued. The talk will illustrate the scope of modern Analytical Science through examples from process analysis relevant to modern process intensification and industry 4.0 to bioanalysis and the use of synchrotron radiation to elucidate fundamental reactions materials.
Carrier gas hot extraction (CGHE) is a commonly applied technique for determination of hydrogen in welded joints using a thermal conductivity device (TCD) for quantitative measurement. The CGHE is based on the accelerated hydrogen effusion due to thermal activation at elevated temperatures. The ISO 3690 standard suggests different specimen geometries as well as necessary minimum extraction time vs. temperature. They have the biggest influence on precise hydrogen determination. The present study summarizes the results and experience of numerous test runs with different specimen temperatures, geometries and factors that additionally influence hydrogen determination. They are namely: specimen surface (polished/as-welded), limited TCD sensitivity vs. specimen volume, temperature measurement vs. effects of PID-furnace controller as well as errors due to insufficient data assessment. Summarized, the temperature is the driving force of the CGHE. Two different methods are suggested to increase the heating rate up the reach the desired extraction temperature without changing the experimental equipment. Suggestions are made to improve the reliability of hydrogen determination depended on the hydrogen signal stability during extraction accompanied by evaluation of the recorded data. Generally, independent temperature measurement with calibration specimens is useful for further data analysis, especially if this data is used for calculation of trapping kinetics by thermal desorption analysis (TDA).
This talk highlights a proof-of-concept that demonstrates the ability to calculate high-resolution Fourier transforms. These can be combined with multi-scale modeling to simulate scattering over a wide range, from small-angle scattering to XRD and PDF.
The preprint documenting this is available on the ArXiv here:
https://doi.org/10.48550/arXiv.2303.13435
The Jupyter notebook, VASP calculation details and MOUSE measured scattering patterns are available from this Zenodo repository: https://dx.doi.org/10.5281/zenodo.7764045
We demonstrate a strategy for simulating wide-range X-ray scattering patterns, which spans the small- and wide scattering angles as well as the scattering angles typically used for Pair Distribution Function (PDF) analysis. Such simulated patterns can be used to test holistic analysis models, and, since the diffraction intensity is on the same scale as the scattering intensity, may offer a novel pathway for determining the degree of crystallinity.
The "Ultima Ratio" strategy is demonstrated on a 64-nm Metal Organic Framework (MOF) particle, calculated from Q < 0.01 1/nm up to Q < 150 1/nm, with a resolution of 0.16 Angstrom. The computations exploit a modified 3D Fast Fourier Transform (3D-FFT), whose modifications enable the transformations of matrices at least up to 8000^3 voxels in size. Multiple of these modified 3D-FFTs are combined to improve the low-Q behaviour. The resulting curve is compared to a wide-range scattering pattern measured on a polydisperse MOF powder. While computationally intensive, the approach is expected to be useful for simulating scattering from a wide range of realistic, complex structures, from (poly-)crystalline particles to hierarchical, multicomponent structures such as viruses and catalysts.
Termite gut flagellates are colonized by host-specific lineages of ectosymbiotic and endosymbiotic bacteria. Previous studies have shown that flagellates of the genus Trichonympha may harbour more than one type of symbiont. Using a comprehensive approach that combined cloning of SSU rRNA genes with fluorescence in situ hybridization and electron microscopy, we investigated the phylogeny and subcellular locations of the symbionts in a variety of Trichonympha species from different termites. The flagellates in Trichonympha Cluster I were the only species associated with 'Endomicrobia', which were located in the posterior part of the cell, confirming previous results. Trichonympha species of Cluster II from the termite genus Incisitermes (family Kalotermitidae) lacked 'Endomicrobia' and were associated with endosymbiotic Actinobacteria, which is highly unusual. The endosymbionts, for which we suggest the name 'Candidatus Ancillula trichonymphae', represent a novel, deep-branching lineage in the Micrococcineae that consists exclusively of clones from termite guts. They preferentially colonized the anterior part of the flagellate host and were highly abundant in all species of Trichonympha Cluster II except Trichonympha globulosa. Here, they were outnumbered by a Desulfovibrio species associated with the cytoplasmic lamellae at the anterior cell pole. Such symbionts are present in both Trichonympha clusters, but not in all species. Unlike the intracellular location reported for the Desulfovibrio symbionts of Trichonympha agilis (Cluster I), the Desulfovibrio symbionts of T. globulosa (Cluster II) were situated in deep invaginations of the plasma membrane that were clearly connected to the exterior of the host cell.
α(1 0 0) Dislocations are observed in nickel-base superalloys after creep deformation at high temperatures and low stresses. They are formed in the γ/γ´ interfaces by a three step mechanism. First, primary dislocations with Burgers vector α/2(1 0 1) and 60° character are left behind in the interfaces when dislocation loops glide through the γ channels. The 60° dislocations move into edge orientation and react forming secondary dislocations α/2(1 1 0). In the third step, new primary dislocations are knit into the already existing meshes of primary and secondary dislocations, which results in hexagonal misfit dislocation networks consisting of secondary dislocations α/2(1 1 0) and tertiary dislocations α(1 0 0), both of edge type. This self-organisation process is explained by dislocation theory and crystallography.
Creep deformation accelerates when the α(1 0 0) interfacial dislocations enter the γ´ phase. During their climb towards the opposite interface, they attain a characteristic rectangular shape. This shape and the importance of the α(1 0 0) super dislocations for creep deformation are discussed.
The title compound (AHTN-OH), C17H26O, was prepared in order to provide standard materials for the qualitative and quantitative analysis of environmental pollutants. The molecule possesses a chiral C atom, although the structure determination was performed on racemic material, expressed in the structure as disordered chiral sites. The asymmetric unit consists of four AHTN-OH molecules containing an hydroxy group and forming a tetrameric cyclic motif built up by four strong hydrogen bonds between these hydroxy groups and additionally by two weak C–H···π interactions. Furthermore, these tetramers are linked via very weak C–H···π interactions, forming chains along the c axis.
The title compound, also known as cis-zearalenone (cis-ZEN), C18H22O5, has already been reported elsewhere [Griffin et al. (1981). ACA Ser. 29, 35], but no atomic coordinates are publicly available. The molecule is of interest with respect to its toxicity. In the crystal, intramolecular O—H···O hydrogen bonds stabilize the molecular conformation, while intermolecular O—H···O hydrogen bonds link the molecules to form infinite chains along the [110] and [1¯10] directions. The absolute configuration has been assigned by reference to an unchanging chiral centre in the synthetic procedure.
The asymmetric unit of the title compound, C18H26O5, which is known as α-zearalanol, contains two molecules having the same conformation, with a r.m.s. deviation of less than 0.03 Å for all non-H atoms. In each independent molecule, an intramolecular O—H···O hydrogen bond stabilizes the molecular conformation. In the crystal, O—H···O hydrogen bonds link the molecules, forming infinite chains along [110] and [1¯10].
We report on the development of ultra-small core-shell silver nanoparticles synthesized by an up-scaled modification of the polyol process. It is foreseen to use these thoroughly characterized particles as reference material to compare the catalytic and biological properties of functionalized silver nanoparticles. Small-angle X-ray scattering (SAXS) analysis reveal a narrow size distribution of the silver cores with a mean radius of RC = 3.0 nm and a distribution width of 0.6 nm. Dynamic light scattering (DLS) provides a hydrodynamic radius of RH = 10.0 nm and a PDI of 0.09. The particles’ surface is covered with poly(acrylic acid) (PAA) forming a shell with a thickness of 7.0 nm, which provides colloidal stability lasting for more than six months at ambient conditions. The PAA can be easily exchanged by biomolecules to modify the surface functionality. Replacements of PAA with glutathione (GSH) and bovine serum albumin (BSA) have been performed as examples. We demonstrate that the particles effectively catalyze the reduction of 4-nitrophenol to 4-aminophenol with sodium borohydride. The tunable catalytic activity of (436 ± 24) L g-1 s-1 is the highest reported in literature for silver nanoparticles.
Zinc dialkyl dithiocarbamoylsulfinates have been proposed as intermediates in the antioxidant action of the respective zinc dialkyl dithiocarbamate additives in hydrocarbon-based plastics and lubricants. As a model compound, zinc diisobutyl dithiocarbamoylsulfinate, [Zn(C9H18NO2S2)2], has been prepared and its crystal structure determined.
The chapter gives a brief introduction to (nano)compositecomposite materials having the focus on polymer-based nanocomposites. The different dimensionalities of nanoparticles are introduced, along with their distribution in the matrix.
Different application fields of polymer-based nanocomposites, like flame retardancy, filled rubbers, nanofilled thermosets and thermoplastics, separation membranes and nanodielectrics, are considered in greater detail.
(Pre)Standardisation and Metrology in Microbeam Analysis – Ongoing Activities and Opportunities
(2023)
The presentation addresses the current ongoing projects as well as the gaps and opportunities in microbeam analysis within ISO/TC 202 Microbeam Analysis standardisation body and in-liaison Technical Working Areas (TWAs) at the pre-standardization platform of VAMAS (Versailles Project on Advanced Materials and Standards).
Due to their extreme high hydrogen contents, high molecular weight (HMW-) and ultra-high molecular weight (UHMW-) polyethylene (PE) are a comprehensible choice as neutron radiation shielding material in casks for storage and transport of radioactive materials. But as a direct consequence of inserting radioactive material in such casks, gamma radiation occurs. Hence, the impact of gamma radiation on the molecular structure of polyethylene has to be taken into consideration. Consequently, PE has to withstand any type of gamma radiation induced degradation affecting safety relevant aspects in order to be applicable for long term neutron radiation shielding purposes during the whole storage period (in Germany, for instance, up to 40 years). The scope of our investigation comprises an estimation of the impact of gamma radiation and temperature on the molecular and supra molecular structure of the two types of PE used as neutron radiation shielding cask components. A further point which is worth exploring is to what extent these changes are detectable by conventional analysis methods. Therefore, thermoanalytical measurements were performed such as differential scanning calorimetry (DSC), thermo mechanical analysis (TMA), dynamic mechanical analysis (DMA), and thermo gravimetric analysis (TGA). Additionally optical and weighing methods were applied. With those methods it is possible to detect structural changes in polyethylene induced by exposure to gamma radiation. The observed amounts of changes of the irradiated material are not safety relevant for the application of polyethylene as neutron radiation shielding material; moreover, some properties actually improve via irradiation.
1,3,5-Tris-(2,3-dibromopropyl)-1,3,5-triazine-2,4,6-trione (TDBP-TAZTO) is an emerging brominated flame retardant which is widely used in several plastic materials (electric and electronic equipment, musical instruments, automotive components).
However, until today, no photochemical studies as well as the identification of possible phototransformation products (PTPs) were described in literature. Therefore, in this study, UV-(C) and simulated sunlight irradiation experiments were performed to investigate the photolytic degradation of TDBP-TAZTO and to identify relevant PTPs for the first time. The UV-(C) Irradiation experiments show that the photolysis reaction follows a first-order kinetic model. Based on this, the photolysis rate constant k as well as the half-life time t1/2 were calculated to be k = (41 ± 5 ×10−3) min−1 and t1/2=(17±2) min. In comparison, a minor degradation of TDBP-TAZTO and no formed phototransformation products were obtained under simulated sunlight. In order to clarify the photochemical behavior, different chemicals were added to investigate the influence on indirect photolysis: (i) H2O2 for generation of hydroxyl radicals and (ii) two quenchers (2-propanol, sodium azide) for scavenging oxygen species which were formed during the irradiation experiments. Herein, nine previously unknown PTPs of TDBP-TAZTO were detected under UV-(C) irradiation and identified by HPLC-(HR)MS. As a result, debromination, hydroxylation, and dehydrobromination reactions could be presumed as the main degradation pathways by high-resolution mass spectrometry. The direct as well as the OH radical-induced indirect photolysis were observed.
The ionic liquid 1,3-dimethyl-imidazolium-dimethylphosphate ([MMIM]+[DMP]−) was analyzed using (hard) x-ray photoelectron spectroscopy.
Here, XPS and HAXPES spectra are shown in comparison. For the acquisition of the XPS spectra, monochromatic Al Kα radiation at 1486.6 eV was used, while for the acquisition of the HAXPES spectra, monochromatic Cr Kα radiation at 5414.8 eV was applied. Here, survey scans and high-resolution spectra of P 2p, P 2s, C 1s, O 1s, and N 1s for both methods and P 1s, P KL2,3L2,3, and P KL1L2,3 for HAXPES are shown.
The 1,3-diphenyl-1H-pyrazolo[3,4-b]-quinoline chromophore is a versatile building block for the construction of brightly fluorescent molecular sensors. Facile synthetic procedures allow integration of the chromophore into fluorophore-spacer-receptor systems as well as fluoroionophores operating via intramolecular charge transfer. Whereas the former photoinduced electron-transfer probes show strong analyte-induced fluorescence enhancement, the latter exhibit bright ratiometric dual emission. Employing prototype macrocyclic receptors, the favorable signaling features for metal ion recognition are demonstrated.
1-Propyl-3-methyl-imidazolium bis(trifluoromethylsulfonyl)imide (Solarpur®), an ionic liquid was purchased from Merck (formerly Sigma Aldrich), was analyzed using hard x-ray photoelectron spectroscopy (HAXPES). The liquid is UHV stable, vertically and laterally homogeneous, and is easy to clean; thus, it can be used as a reference material. The HAXPES spectra of Solarpur® obtained using monochromatic Cr Kα radiation at 5414.8 eV include a survey scan, high-resolution spectra of C 1s, O 1s, N 1s, S 2p, S 1s, S 2s, F 1s, and S KLL.
TeaABC from the moderate halophilic bacterium Halomonas elongata belongs to the tripartite ATP-independent periplasmic transporters (TRAP-T), a family of secondary transporters functioning in conjunction with periplasmic substrate binding proteins. TeaABC facilitates the uptake of the compatible solutes ectoine and hydroxyectoine that are accumulated in the cytoplasm under hyperosmotic stress to protect the cell from dehydration. TeaABC is the only known TRAP-T activated by osmotic stress. Currently, our knowledge on the osmoregulated compatible solute transporter is limited to ABC transporters or conventional secondary transporters. Therefore, this study presents the first detailed analysis of the molecular mechanisms underlying substrate recognition of the substrate binding protein of an osmoregulated TRAP-T. In the present study we were able to demonstrate by isothermal titration calorimetry measurements that TeaA is a high-affinity ectoine binding protein (Kd = 0.19 μM) that also has a significant but somewhat lower affinity to hydroxyectoine (Kd = 3.8 μM). Furthermore, we present the structure of TeaA in complex with ectoine at a resolution of 1.55 Å and hydroxyectoine at a resolution of 1.80 Å. Analysis of the TeaA binding pocket and comparison of its structure to other compatible solute binding proteins from ABC transporters reveal common principles in compatible solute binding but also significant differences like the solvent-mediated specific binding of ectoine to TeaA.
This study presents for the first time an NMR spectroscopic characterization of the room and high temperature phases of (NH4)3InF6 using 19F and 115In as probe nuclei. The reversible phase transition to the cubic phase at 353 K was followed by MAS NMR in situ. Static NMR experiments of the room temperature phase and MAS NMR experiments of the high temperature phase allowed the determination of the NMR parameters of both nuclei. Finally, the scalar In–F coupling, rarely observed in solid state NMR, is evidenced in both room and high temperature phases of (NH4)3InF6, and measured in the high temperature phase.
Large-language models (LLMs) such as GPT-4 caught the interest of many scientists. Recent studies suggested that these models could be useful in chemistry and materials science. To explore these possibilities, we organized a hackathon. This article chronicles the projects built as part of this hackathon. Participants employed LLMs for various applications, including predicting properties of molecules and materials, designing novel interfaces for tools, extracting knowledge from unstructured data, and developing new educational applications. The diverse topics and the fact that working prototypes could be generated in less than two days highlight that LLMs will profoundly impact the future of our fields. The rich collection of ideas and projects also indicates that the applications of LLMs are not limited to materials science and chemistry but offer potential benefits to a wide range of scientific disciplines.
The preparation and structural investigation of 17O-enriched xNa2O(100-x)P2O5 glasses (46.5<=x<=62.8) by nuclear magnetic resonance (NMR) is described. Enriched phosphoric acid was prepared by hydrolysis of PCl5 with 17O-enriched water and neutralized with sodium carbonate. The sodium metaphosphate was then melted at 800 °C for 15 h and quenched. Polyphosphate and ultraphosphate glass compositions were prepared by remelting the metaphosphate with sodium carbonate and phosphorus pentoxide, respectively. 31P magic angle sample spinning (MAS) NMR was used to determine the Na2O/P2O5 content in the glasses. 17O NMR spectra (quadrupole echo for non-rotating samples and multiple-quantum excitation for rotating samples (MQMAS)) show two oxygen sites in the samples with large quadrupolar coupling constants (4.7 and 7.7 MHz), in accordance with the high phosphorus electronegativity. According to the correlation of 17O quadrupolar constants with bond ionicity, these two components are attributed to bridging POP and non-bridging PO...Na oxygens. The average POP bond angle is estimated with the quadrupolar asymmetry derived from the fit of the static echo spectra. The MQMAS spectrum shows a distribution of non-bridging oxygen chemical shifts, attributed to a variation of bond length and angle.
Shortly after midnight on 15th November 1992, a severe train crash was caused by the break off of a buffer from a tool and gear wagon of a freight train. The buffer fell between the rails, tumbled, and then lifted one axle of a following freight wagon off the rails. Several freight wagons derailed in the station of Northeim, Germany, blocking the adjacent track. A night train travelling on that blocked track was already too close (only 180 m) to stop, despite emergency braking initiated immediately and automatically by the track signalling system. When the night train crashed into the freight wagons, some of its coaches were heavily damaged. Eleven people were killed, and 51 injured, some of them seriously.
The task for failure analysts was to find out why the buffer broke off from the front frame of the tool and gear wagon. Therefore, the material of the attachment, the front frame, and the welds were tested. Chemical composition, hardness, and microstructure were allowable. The welds showed imperfections which were determined not to be causal. The fracture surfaces had graded corrosion which again was not causal and beach marks that depicted fatigue cracks before final fracture.
The cause for the break off was the fact that the front frame had been repaired at this same buffer attachment some years before and that the repair patch used was thinner than the original front frame profile.
Additionally, the force characteristics of the buffer showed reduced stroke but increased forces which was due to several friction springs that had been broken for a long time. The buffer forces in service were assessed from standards, literature, and the deformations of the attachment. The in-service stresses at the welds were estimated using FEM analysis. High cyclic stresses at the welds resulted in fatigue cracking and finally break off of the attachment with the buffer.
1Brominated carbon nanotubes as effective catalysts for petroleum hydrocarbons aerobic oxidation
(2012)
The small-pore framework sodium stannosilicate AV-10, chemical composition Na2SnSi3O9⋅2H2O and known crystallographic structure, was synthesized by hydrothermal crystallization. This stannosilicate is built up of a three-dimensional network of corner-shared SiO4 tetrahedra and SnO6 octahedra. The SnO6 sites are linked to six SiO4 tetrahedra (Sn(6Si)) while each of the two crystallographically different SiO4 units are connected to two SnO6 and SiO4 units (Si(2Si,2Sn)). This material was used as model compound for developing a solid-state MAS NMR strategy aimed on the challenges and possibilities for structural studies, particularly considering the short and medium range order to verify the connectivity of SiO4 and SnO6 of such compounds despite the low natural abundances of 4.68% for 29Si and 8.59% for 119Sn nuclei as a real challenge. 29Si{119Sn} and 119Sn{29Si} REDOR (Rotational-Echo Double-Resonance) NMR measurements after 1H cross-polarization (CP) were carried out. The REDOR curves show a significant change after the “normal” quadratic short time evolution from which both (i) the shortest internuclear 29Si – 119Sn distances (and vice versa) and (ii) the number of corner-sharing SiO4 tetrahedra around the SnO6 octahedra (and vice versa) can be obtained. Based on these data, optimized 29Si {119Sn} and 119Sn{29Si} REPT-HMQC (Recoupled Polarization Transfer-Heteronuclear Multiple-Quantum Correlation, again after 1H CP) experiments were implemented, which directly show those heterogroup connectivity as correlation peaks in a 2D spectrum. This information was also obtained using 2D29Si{119Sn}-J-Coupling NMR experiments. Furthermore, 2D29Si INADEQUATE NMR experiments are also feasible, showing the connectivity of SiO4 tetrahedra. The combination of REDOR, REPT-HMQC, J-Coupling and INADEQUATE experiments yielded a complete analysis of the short and medium range structure of this microporous stannosilicate, in agreement with the previously published structure obtained Ab Initio from powder X-Ray diffraction data (XRD).
There is no applicable existing standard for the determination of safety characteristics for hybrid mixtures. While developing a new standard in a joint research project in Germany first results from parameter studies led to a standard procedure that can be adopted by laboratories that are already testing dusts in the so called 20L-sphere with as little additional effort as necessary. In fact, one of the main objectives of this research project was to keep modifications and adjustments from the generally accepted dust testing procedures as easy and minimal as possible so as to limit potential deviations from one laboratory to another.
In this first round robin test on hybrid mixtures ever, with methane as gas component and a specific corn starch as dust sample, the practicality of the whole procedure, the scattering of the results and the deviation between the testing apparatuses is investigated. This paper summarizes the experimental procedure adopted and objectives of the first round-robin phase involving three of the four original German companies, plus volunteering laboratories from Australia, Belgium, Czech Republic, France, Poland and P.R. China. The results will have an impact on the new standard and may lead to robust data for later simulation purposes.
A novel fluorescent host-guest material, molecular sieves of AlPO4-5-type doped with 2,2'-bipyridyl-3,3'-diol, was prepared and spectroscopically characterized. The composite crystals show a pronounced optical anisotropy, indicating a high degree of alignment of the guest molecules within the zeolitic pore system. A mean tilting angle of 22 was found for the orientation of the individual dye molecules in the straight channels. The corrected fluorescence emission spectra were determined, and time-resolved fluorescence studies revealed that the dye molecules are preferentially found in three different types of microenvironment. By invoking pH-dependent studies of the dye in aqueous solution, we could trace these spectroscopic features back to two main influences, coadsorbed water within AlPO4-5 pores and guest-host interactions with a few relatively weak Brnsted acid (defect) sites of the inorganic host network.
A novel cop olyme r based on supramolecular motif2,6-diaminopyridin e and water-soluble acrylamide, poly[N-(6-ace tamidopyridin-2-yl) acrylamide-co-acrylamide], was synthe-size d via rev ersible addi tion–fragmentation chain transfer (RAFT)polymerization with various monomer compositions. The thermo-respon sive behavior of the copolymers was studied by turbidime-try and dynamic light scattering (DLS). The obtained copolymersshowed an upper critical solution temperature (UCST)-typ e phasetransition behavior in water and electrolyte solution. The phasetransition temperature was found to increase with decreasingam ount of acrylamide in the copolymer and increasing concentra-tion of the solution. Furth ermore, the phase transition temperatureva ried in aqueous solutions of electrolytes according to the naturean d concentration of the electrolyte in accordance with theHoffmeister series. A dramatic solvent isotope effect on thetransition temperature was o bserved in this study, as the transitiontemperature was almost 10–12C higher in D2OthaninH2Oatthesame concentration and acrylamide co mposition. The size of theaggregates below the transition temperature was larger in D2Ocompared to that in H2O that can be explained by deuterium iso-tope effect. The thermoresponsive behavior of the copolymers wasalso investigated in different cell medium and found to be exhibitedUCST-type phase transition behavior in different cell medium.Such behavior of the copo lyme rs can be useful in many a pplica-tions including biomedical, microfluidics, optical materials, and indrug delivery.
The implementation of new 2-D materials based technologies in production processes requires the development of quality management tools. These have to be underpinned by appropriate measurements. Consequently there is a need for the development of the metrology for measurement methods, the development of certified reference materials (CRM) and finally standardization. This chain represents the ideal way to practically useful standards. The presentation will give an overview on the main players in the field and summarize the recent status of activities. At the highest level the metrology of chemical characterization of 2D materials is in the scope of the International Meter Convention, specifically the Consultative Committee for Amount of Substance: Metrology in Chemistry and Biology (CCQM). Pre-standardization is an activity field of the Versailles Project on Advanced Materials and Standards (VAMAS). Standardization is mainly addressed by addressed ISO Technical Committees. A summary on available CRMs relevant to the characterization of nano materials has been prepared by BAM. Examples from the work of BAM’s Division 6.1 “Surface Analysis and Interfacial Chemistry” showcasing the characterization of chemically modified graphene surfaces are given and specific needs for the development of metrology are addressed.
In the discussion the audience is invited to define specific needs which will be streamlined to the respective bodies!
Tribological profile of hydraulic oils by using SRV. The determination of a set of critical, tribological by using different SRV-based test methods. The SRV-based concept of tribological profile generates the wear volumes on two triboelements (specimen), the extreme pressure properties and friction under different contact pressures.
Thus, the benchmark and validation of hydraulic oils bear on a wider range of tribological properties.
The RR2016 extends with six hydraulic oils to other base oil types including biodegradable fluids, which were all tested according to ASTM D7043 in order to consolidate the correlation between SRV and V104C.
2015 Tianjin explosions
(2016)
In 2015 a series of explosions occurred at a container storage station at the Port of Tianjin, China, on Wednesday, 12 August 2015, that killed over one hundred people and injured hundreds of firemen and others. The first two explosions happened within 30 seconds of each other at the facility. The second explosion was larger and involved the detonation of about 800 tons of ammonium nitrate. The cause of the explosions was not known at first, but an investigation of the Chinese authorities concluded in February 2016 that an overheated container of dry nitrocellulose was the cause of the initial explosion. Colleagues of the Nanjing University of Science and Technology and BAM worked together to analyze the reasons and the process of that incident based on knowledge about the properties of the involved substances, particularly ammonium nitrate and nitrocellulose, and potential mechanism of initiation and propagation.
2015 Tianjin Explosions
(2016)
In 2015 a series of explosions occurred at a container storage station at the Port of Tianjin, China, on Wednesday, 12 August 2015, that killed over one hundred people and injured hundreds of firemen and others. The first two explosions happened within 30 seconds of each other at the facility. The second explosion was larger and involved the detonation of about 800 tons of ammonium nitrate. The cause of the explosions was not known at first, but an investigation of the Chinese authorities concluded in February 2016 that an overheated container of dry nitrocellulose was the cause of the initial explosion. Colleagues of the Nanjing University of Science and Technology and BAM worked together to analyze the reasons and the process of that incident based on knowledge about the properties of the involved substances, particularly ammonium nitrate and nitrocellulose, and potential mechanism of initiation and propagation.
Actions from the meeting in April 2016: 1. Four SAC test methods are in place and were revised: SH/T 0721 (Grease, coefficient of friction and wear), SH/T 0784 (Grease, pass load/O.K. load), SH/T 0847 (Oil, coefficient of friction and wear) and SH/T 0882 released by 11-2014 (Oil, pass load/O.K. load). 2. New test method to evaluate anti-fretting properties of greases based was approved by SAC TC280 and will be released. 3. SAC TC280 accepted the project “Simulation of synchronizer by using SRV”. Draft text to be submitted by 03-2017. Discussions on a parallel ASTM test method. 4. A procedure for “Wear Volume” is under development for SAC TC280.
Gold nanocubes with a monodispersed size distribution (edge = 55 nm) deposited on a silicon wafer. These tiny uniform cubes were produced as reference nanoparticles within the EMPIR project nPSize - Improved traceability chain of nanoparticle size measurements. SEM image acquired at 10 kV with an in-lens secondary electron detector. Image colored in ImageJ using LUT “Orange hot.” Published in Microscopy and Microanalysis 25(S2) (2019) 2328.
A new method of preparing concentrated alumo-sols, the hydrolysis of Al-tri-sec-butylate in acidic aqueous media at 85°C, was studied in detail by varying the H2O/Al- and NO3 -/Al-ratios in wide ranges. The components of the sols were characterized by 27Al NMR spectroscopy. The pH-value depends on both the chosen H2O/Al- and NO3 -/Al-ratio and on the aging time of the sols and reflects the composition of the sols. Al13 polycations were detected in sols with a pH-value between 3.0 and 3.7. As a new result its presence was shown by NMR below 3.4. The Al13 content of the sols increased with pH and the maximum fraction of Al13 polycations was detected in the sol with the highest pH (3.7). Nearly 65% of the entire aluminium content of this solution is bound in the Al13 polycations. Hence, a new synthetic method for the preparation of Al13 ions containing sols was developed.
Aging studies of the sols showed, that the Al13 polycations were more stable in solutions with higher pH-value. Al13 polycations were detected after an aging time of four months only in sols with a pH-value of 3.7. Tempering the aged sols at 40° to 80°C caused formation of Al13 and also of Al30 polycations.
The production and processing of ordinary Portland cement are responsible for nearly 5% of the world C02 emissions. Due to the world’s increasing requirement for building materials, this air pollution is growing up in the next decades. Alternative cement such as geopolymers can reduce these emissions effectively, Conventional geopolymer binders, produced ffom fly ash or metakaolin as aluminosilicate source and water-glass or alkali hydroxide Solutions as activator, are often used and studied. It is known that under appropriate conditions the starting materials form a three-dimensional aluminosilicate structure and create a gel-like matrix, In our case, a silica source from wastewater treatment of chlorosilane production and solid sodium aluminate as starting materials are initiated to harden by water. This procedure is known as “just add water” or “one-part” geopolymer formulation. These composites have significant advantages for use on construction site, but their Chemical structure is not extensively analyzed. In this work, a well known one-part geopolymer is investigated by 'H and 27A1 magic-angle spinning nuclear magnetic resonance (MAS NMR) spectroscopy. Furthermore, it is shown that overlapping NMR lines can resolved with echo experiments and
One-part-geopolymers, produced by addition of water to a mixture of solid silica and sodium alumi-nate, are a less exhaustively studied approach to form geopolymeric binders. Depending on the silica source, the reaction products show significant amounts of zeolite Na-A besides amorphous compounds. Previously, 29Si MAS NMR has been used to analyze the chemical structure of such one-part geopolymers, having crystalline structures and amorphous phases (Q2, Q3, Q4).
In this work, pure zeolites and three different one-part-geopolymers cured for 1 day were investigated by 29Si-27Al TRAPDOR NMR. It was used to identify aluminum phases in overlapping silicon sites. Zeolites Na-X (Si/Al=1.4) and Na-Y (Si/Al=2.7) served as model systems to measure the TRAPDOR effect of the structural units Q4(mAl). Both materials show several Q4(mAl) signals, which are all separated by their chemical shifts. The more aluminum surrounds the silicon tetrahedron the higher are the normalized TRAPDOR difference signals (S0/∆S). The intensity ratios between Q4(mAl) to Q4({m-1}Al) of these signals is fixed but vary slightly between both zeolites. These results are transferred to the complex geopolymer structure.
29Si{27Al} TRAPDOR MAS NMR was applied to two faujasite-type zeolites with Si/Al ratios of 1.3 (Na-X) and 2.7 (Na-Y). The aim of this test study is to show that different Q4(mAl) sites (m=4,3,2,1) can be distinguished by differently strong TRAPDOR effects (ΔS/S0). Indeed, it was found that the TRAPDOR effect depends on the number m of AlO4 units connected to the Q4 silicon tetrahedrons. For Na-X, the measured ΔS/S0 values are 1:0.81:0.56 for Q4(4Al), Q4(3Al) and Q4(2Al), respectively (normalized to Q4(4Al)). The corresponding ΔS/S0 values are the same for Na-Y within the error bars, although the silicon sites are different: Q4(3Al), Q4(2Al) and Q4(1Al) and now normalized to Q4(3Al) as no Q4(4Al) is present. Nevertheless, the proposed method opens up the possibility to distinguish overlapping 29Si NMR signals of the Qn(mAl) sites in amorphous materials as the main goal of these investigations.
The influence of starting materials and synthesis route on the properties and the structure of cementitious sodium aluminosilicate gels is not fully understood, partly due their amorphous nature and the fact that they often contain residual reactants, which can make the results of single-pulse NMR spectroscopy applied to these materials difficult to interpret or ambiguous. To overcome some of these limitations, 29Si{27Al} TRAPDOR NMR as well as 27Al{29Si} and 27Al{1H} REDOR NMR spectroscopy were applied to materials synthesized by the one-part alkali-activation route from three different amorphous silica starting materials, including rice husk ash. The latter led to formation of a fully amorphous sodium aluminosilicate gel (geopolymer), while the materials produced from the other silicas contained amorphous phase and crystalline zeolites. Application of the double-resonance NMR methods allowed to identify hydrous alumina gel domains in the rice husk ash-based material as well as significantly differing amounts of residual silica in the three cured materials. Four-coordinated Al existed not only in the aluminosilicate gel framework but also in a water-rich chemical environment with only a small amount of Si in proximity, likely in the alumina gel or possibly present as extra-framework Al in the aluminosilicate gel. The results demonstrate how the employment of different silica starting materials determines the phase assemblage of one-part alkali-activated materials, which in turn influences their engineering properties such as the resistance against chemically/biologically aggressive media.
The combination of microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on porous material properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. I will show a few examples of possible use of X-ray tomographic data for quantitative assessment of porosity in ceramics.
Moreover, I will show how not-so-novel 2D characterization techniques, based X-ray refraction, can allow a great deal of insights in the damage evolution in microcracked (and porous) ceramics. I will show how X-ray refraction can detect objects (e.g. microcracks) below its own spatial resolution.
Finally, I will discuss the link between the microstructural findings and the mechanical properties of porous microcracked ceramics.
The combination of microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on porous material properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. I will show a few examples of possible use of X-ray tomographic data for quantitative assessment of porosity in ceramics.
Moreover, I will show how not-so-novel 2D characterization techniques, based X-ray refraction, can allow a great deal of insights in the damage evolution in microcracked (and porous) ceramics. I will show how X-ray refraction can detect objects (e.g. microcracks) below its own spatial resolution.
Finally, I will discuss the link between the microstructural findings and the mechanical properties of porous microcracked ceramics.
AbstractThis work addresses the critical need for multifunctional materials and substrate‐independent high‐precision surface modification techniques that are essential for advancing microdevices and sensing elements. To overcome existing limitations, the versatility of mussel‐inspired materials (MIMs) is combined with state‐of‐the‐art multiphoton direct laser writing (DLW) microfabrication. In this way, 2D and 3D MIM microstructures of complex designs are demonstrated with sub‐micron to micron resolution and extensive post‐functionalization capabilities. This study includes polydopamine (PDA), mussel‐inspired linear, and dendritic polyglycerols (MI‐lPG and MI‐dPG), allowing their direct microstructure on the substrate of choice with the option to tailor the patterned topography and morphology in a controllable manner. The functionality potential of MIMs is demonstrated by successfully immobilizing and detecting single‐stranded DNA on MIM micropattern and nanoarray surfaces. In addition, easy modification of MIM microstructure with silver nanoparticles without the need of any reducing agent is shown. The methodology developed here enables the integration of MIMs in advanced applications where precise surface functionalization is essential.
In civil engineering the information about the quantitative ingress of harmful species like Cl⁻, Na⁺ and SO²⁻₄ is of great interest to evaluate the remaining life time of structures. These species are triggering different damage processes like the alkali-silica reaction (ASR) or the chloride-induced corrosion of the reinforcement. For the evaluation of the heterogeneous concrete it is necessary to discriminate between the different phases mainly cement matrix and aggregates. The transport processes are only proceeding in the cement matrix therefore the measured concentrations should be regarded to the cement content. For the 2D evaluation of element distributions different multivariate cluster-algorithms like k-means and Expectation-Maximization-algorithm (EM-algorithm) have been tested. The methods are compared and different figures of merit will be presented. After phase separation non-relevant information of the aggregates can be excluded. The ingress of harmful species is then quantified using chemometrics. Due to concrete cores from a parking deck the methods have been validated and verified with standard methods of wet-chemistry.
2D evaluation of spectral LIBS data derived from heterogeneous materials using cluster algorithm
(2017)
Laser-induced Breakdown Spectroscopy (LIBS) is capable of providing spatially resolved element maps in regard to the chemical composition of the sample. The evaluation of heterogeneous materials is often a challenging task, especially in the case of phase boundaries. In order to determine information about a certain phase of a material, the need for a method that offers an objective evaluation is necessary. This paper will introduce a cluster algorithm in the case of heterogeneous building materials (concrete) to separate the spectral information of non-relevant aggregates and cement matrix. In civil engineering, the information about the quantitative ingress of harmful species like Cl−, Na+ and SO2−4 is of great interest in the evaluation of the remaining lifetime of structures (Millar et al., 2015; Wilsch et al., 2005). These species trigger different damage processes such as the alkali-silica reaction (ASR) or the chloride-induced corrosion of the reinforcement. Therefore, a discrimination between the different phases, mainly cement matrix and aggregates, is highly important (Weritz et al., 2006). For the 2D evaluation, the expectation-maximizationalgorithm (EM algorithm; Ester and Sander, 2000) has been tested for the application presented in this work. The method has been introduced and different figures of merit have been presented according to recommendations given in Haddad et al. (2014). Advantages of this method will be highlighted. After phase separation, non-relevant information can be excluded and only the wanted phase displayed. Using a set of samples with known and unknown composition, the EM-clustering method has been validated regarding to Gustavo González and Ángeles Herrador (2007).
Graphene derivatives have shown great promise in the field of pathogen binding and sensing. Due to their diverse applications, they show a variety of activities that range from bacterial adhesion to bacterial resistance. Therefore, domination of the graphene-pathogen interactions is highly relevant for producing 2D platforms with the desired applications. In order to gain control over the interactions between graphene and biosystems, mechanisms should be fully understood. The surface functionality of graphene is one of the most important factors that dominates its interactions with biosystems and pathogens. Covalent functionalization is a robust method through which functionality, chemical structure, and subsequently physicochemical properties of graphene are abundantly manipulated. A critical issue for preparing graphene-based 2D materials with a defined surface structure, however, is controlling the functionalization in terms of number, position, and type of functional groups.
Graphene and its derivatives have recently attracted much attention for sensing and deactivating pathogens. However, mechanism of multivalent interactions at the graphene-pathogen interface are not fully understood. Since different physicochemical parameters of graphene play a role at this interface, control over graphene’s structure is necessary to study the mechanism of these interactions. In this work, zwitterionic graphene nanomaterials (ZGNMs) were synthesized with defined isoelectric points and exposure, in terms of polymer coverage and functionality. Then, the switchable interactions of ZGNMs with E. coli were investigated to study the validity of the generally proposed “trapping” mechanism for inactivating pathogens by functionalized graphene derivatives. The ZGNMs were able to controllably trap and release E. coli by crossing their isoelectric points.
Non-destructive testing (NDT) of concrete structures is performed using pulse-echo methods. According to the type of the applied waves it can be classified as acoustic (Impact-Echo, Ultrasonics) and electromagnetic methods (Radar). The results are visualised through different imaging processes. This work is performed in the frame of a research project promoted by Deutsche Forschungsgemeinschaft (FOR384). The objective of data fusion is to use the complementary information of the different methods. Radar can detect metallic reflectors in concrete (metallic ducts and concrete reinforcement) very well. This method is not able to locate defects behind these reflectors (injecting defects, defects behind close concrete reinforcement), because the electromagnetic waves are completely reflected at metals. The acoustic methods are able to compensate this deficit i.e. Acoustic waves can penetrate through metal. But acoustic waves in the ultrasonic range are completely reflected by air layers. Air layers have smaller influence on radar propagation, so that both methods complement each other. In order to be able to combine the NDT-data from several methods records at the same volume, the different data setsmodes of signals must be adapted. The ultrasonic and radar data have to be reconstructed with programs based on the Synthetic Aperture Focusing Technique (SAFT) before data fusion. Subsequently, a conversion of the data into a uniform format has to be carried out. This is a prerequisite in order to keep the data exchange between the project partners as simple as possible. After the data sets are imported and transferred into a common reference system, they can be processed with operations according to the purpose of the investigation. Results, which have been achieved in concrete test specimen with radar and ultrasonics, will be presented and will show the feasibility of the data fusion method.
Thermographic super resolution techniques allow the spatial resolution of defects/inhomogeneities below the classical limit, which is governed by the diffusion properties of thermal wave propagation. In this work, we report on the extension of this approach towards a full frame 2D super resolution technique. The approach is based on a repeated spatially structured heating using high power lasers. In a second post-processing step, several measurements are coherently combined using mathematical optimization and taking advantage of the (joint) sparsity of the defects in the sample
Thermographic super resolution techniques allow the spatial resolution of defects/inhomogeneities below the classical limit, which is governed by the diffusion properties of thermal wave propagation. In this work, we re-port on the extension of this approach towards a full frame 2D super resolution technique. The approach is based on a repeated spatially structured heating using high power lasers. In a second post-processing step, several measurements are coherently combined using mathematical optimization and taking advantage of the (joint) sparsity of the defects in the sample.
The slip-rolling 2Disk tribometer from Optimol Instruments represented the technological evolution in tribotesting of the well-known AMSLER-type tribometer marketed in 1922. Both use two discs with the same outer diameter rolling against each other on their circumference. In the AMSLER, the lower disc dips into an oil reservoir, whereas in the 2Disk the oil is injected into the contact. The oil supply of the 2Disk is controlled by pump and temperature by a heat exchanger.
2PM FlySCAN: Innovative approach for wide field high resolution imaging of skin tissue volumes
(2016)
Two Photon Microscopy (2PM) is an innovative Technology for high resolution imaging of human skin in vivo and ex vivo. Up to now the method is limited by its interdependence between the field of view and the attainable resolution. The new FlySCAN Technology overcomes these boundaries and enable images sizes of many millimeters by resolutions in the submicrometer range revealing very specific information on clinically and biologically relevant tissue and cell structures. The advantages of the new approach are demonstrated by excellent in vivo and ex vivo tissue images.
2PP-TestArtifact
(2023)
This repository contains a test artifact (TA), also called test structure, designed for two-photon polymerization (also known as Direct Laser Writing (DLW) or Two/Multi-photon lithography (2PA/MPA)). Test artifacts can be used to compare structures, to check options used by the slicer, check the state of the 2PP machine itself or to get a construction guidelines for a certain combination of power, velocity and settings.
The associated paper can be found here: https://dx.doi.org/10.1088/1361-6501/acc47a
General ideas behind the test artifact:
1. optimized for 2PP-DLW
2. should be fast and easy to analyse with optical microscopy or 3. scanning electron microscopy without tilt.
3. short time to fabricate
4. include a reasonable amount of different features
5. bulk and small structures on the substrate
The modeling of waveguides by means of the Scaled Boundary Finite Element Method (SBFEM) has recently been addressed and is considered an effective procedure for the simulation of ultrasonic guided waves in plates and uniform structures, as well as their interaction with defects. This work presents the extension of the known applications like uniform concrete foundation cylinders to structures with more complex shapes and defects. The main focus is the required modeling of 3-D structures in SBFEM to solve these efficiently. Furthermore the coupling of different models is discussed. This involves models like a mainly uniform foundation cylinder with varying material behavior or geometry in certain areas which has to be modeled in 3-D SBFEM. With the presentation of numerical examples the accuracy and performance of the modeling is discussed and the advantages in improving numerical stability are shown.
A series of twelve 3-piperazinyl propenylidene indolone merocyanines was synthesized in a one-pot fashion using a consecutive three-component insertion-coupling-Michael addition sequence. Physicalorganic treatment of the absorption data of a consanguineous series of this library allows semiquantitative Linear Free Energy Relationships (LFERs) to be established and confirmation of the positive Absorption solvatochromicity. All Boc-substituted piperazinyl merocyanines display aggregation induced Emission (AIE), which was corroborated for two solvent systems. In particular, crystallization-induced Emission enhancement (CIEE) induced by ultrasonication could be shown for a model chromophore by confocal laser scanning microscopy (CLSM).
Structure elucidation of complex synthetic copolymers still represents a challenge. A one-dimensional separation technique cannot give the answer to the question: What are the molar mass distribution (MMD), the functionality distribution (FTD), the chemical composition distribution (CCD), the monomer sequence distribution (MSD), the topology differences within a single broad distributed polymer sample?
Is the coupling of liquid chromatographic separation techniques to mass spectrometry able to fill the gaps to a certain degree?
Different LC separation techniques as size exclusion chromatography (SEC), liquid adsorption chromatography (LAC), liquid chromatography at critical conditions (LCCC) and gradient elution liquid chromatography (GELC) combined with Matrix assisted Laser Desorption Ionization (MALDI) respectively Electrospray Ionization (ESI) Time of Flight (TOF) mass spectrometry are able to give information which otherwise are completely inaccessible. In some cases, CID tandem mass spectrometry is applied. Fragmentation of suitable precursor ions resulted in typical fragment ion patterns. This technique enables an additional information on e.g. sequences, structural defects and topology of complex polymer mixtures.
Often the deficiencies of stand-alone methods can be bridged. LC, blind to structural information needs mass spectrometry as one of the most powerful detectors able to give detailed information on e.g. the repeat units, functionalization or copolymer composition of the chromatographic separated constituents. A separation prior to MS reduces radical the dispersity which is one of the reasons for failing of MS. Also problems with different ionization probabilities in complex mixtures can partly be overcame.
The lecture will provide a series of examples where LC-MS has been applied to evaluate complex macromolecules and mixtures of these.
On- and offline coupling principles will be compared and the pros and cons of both mass spectrometric techniques will be discussed.
The Alpine Fault zone in New Zealand marks a major transpressional plate boundary that is late in its typical earthquake cycle. Understanding the subsurface structures is crucial to understand the tectonic processes taking place. A unique seismic survey including 2D lines, a 3D array, and borehole recordings, has been performed in the Whataroa Valley and provides new insights into the Alpine Fault zone down to ∼2 km depth at the location of the Deep Fault Drilling Project (DFDP)-2 drill site. Seismic images are obtained by focusing prestack depth migration approaches. Despite the challenging conditions for seismic imaging within a sediment filled glacial valley and steeply dipping valley flanks, several structures related to the valley itself as well as the tectonic fault system are imaged. A set of several reflectors dipping 40°–56° to the southeast are identified in a ∼600 m wide zone that is interpreted to be the minimum extent of the damage zone. Different approaches image one distinct reflector dipping at ∼40°, which is interpreted to be the main Alpine Fault reflector located only ∼100 m beneath the maximum drilled depth of the DFDP-2B borehole. At shallower depths (z < 0.5 km), additional reflectors are identified as fault segments with generally steeper dips up to 56°. Additionally, a glacially over-deepened trough with nearly horizontally layered sediments and a major fault (z < 0.5 km) are identified 0.5–1 km south of the DFDP-2B borehole. Thus, a complex structural environment is seismically imaged and shows the complexity of the Alpine Fault at Whataroa.