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- 5.3 Polymere Verbundwerkstoffe (1)
- 6.6 Physik und chemische Analytik der Polymere (1)
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Hydroformylation represents an important homogeneous catalyzed process, which is widely used within chemical industry. Usually applied with simple alkenes like Propene and Butene aldehydes obtained from alkenes >C6 are relevant intermediates in production of plasticizers, surfactants and polymers. Today the active catalyst species is often based on valuable Rhodium complexes in aqueous solution. This implies the problem of limited water solubility of the reactands, which is acceptable for short chain lengths, but states a problem in case of higher alkenes. Along with that efficient separation and recycling of the catalyst becomes more complicated. There are different approaches tackling this problem, e.g., by using of salt formation in the BASF process or downstream distillation within the Shell process
Homogen katalysierte Reaktionen sind wichtige Werkzeuge der chemischen Industrie. Milde Reaktionsbedingungen und hohe Selektivitäten führen zu einer energie- und ressourcenschonenden Produktion. Ein bedeutender Prozessschritt ist die Hydroformylierung. Hier kommen Kobalt- und Rhodiumkomplexe mit mehrzähnigen Liganden zum Einsatz, die zumeist in wässriger Lösung vorliegen. Die Anwendbarkeit beschränkt sich demnach auf kurzkettige Edukte mit hinreichender Wasserlöslichkeit.
Recent publications indicate that the order of electrochemical anodization (before or after the laser processing step) plays an important role for the response of bone-forming osteoblasts—an effect that can be utilized for improving permanent dental or removable bone implants. For exploring these different surface functionalities, multimethod morphological, structural, and chemical characterizations are performed in combination with electrochemical pre- and postanodization for two different characteristic microspikes covered by nanometric laser-induced periodic surface structures on Ti–6Al–4V upon irradiation with near-infrared ps-laser pulses (1030 nm wavelength, ≈1 ps pulse duration, 67 and 80 kHz pulse repetition frequency) at two distinct sets of laser fluence and beam scanning parameters. This work involves morphological and topographical investigations by scanning electron microscopy and white light interference microscopy, structural material examinations via X-ray diffraction, and micro-Raman spectroscopy, as well as near-surface chemical analyses by X-ray photoelectron spectroscopy and hard X-ray photoelectron spectroscopy. The results allow to qualify the mean laser ablation depth, assess the spike geometry and surface roughness parameters, and provide new detailed insights into the near-surface oxidation that may affect the different cell growth behavior for pre- or postanodized medical implants.
Microplastics are small plastic fragments that are widely distributed in marine and terrestrial environments. While the soil ecosystem represents a large reservoir for plastic, research so far has focused mainly on the impact on aquatic ecosystems and there is a lack of information on the potentially adverse effects of microplastics on soil biota. Earthworms are key organisms of the soil ecosystem and are due to their crucial role in soil quality and fertility a suitable and popular model organism in soil ecotoxicology.
Therefore, the aim of this study was to gain insight into the effects of environmentally relevant concentrations of microplastics on the earthworm Eisenia andrei on multiple levels of biological organization after different exposure periods. Earthworms were exposed to two types of microplastics: (1) polystyrene-HBCD and (2) car tire abrasion in natural soil for 2, 7, 14 and 28 d. Acute and chronic toxicity and all subcellular investigations were conducted for all exposure times, avoidance behavior assessed after 48 h and reproduction after 28 d. Subcellular endpoints included enzymatic biomarker responses, namely, carboxylesterase, glutathione peroxidase, acetylcholinesterase, glutathione reductase, glutathione S-transferase and catalase activities, as well as fluorescence-based measurements of oxidative stress-related markers and multixenobiotic resistance activity. Multiple biomarkers showed significant changes in activity, but a recovery of most enzymatic activities could be observed after 28 d. Overall, only minor effects could be observed on a subcellular level, showing that in this exposure scenario with environmentally relevant concentrations based on German pollution levels the threat to soil biota is minimal. However, in areas with higher concentrations of microplastics in the environment, these results can be interpreted as an early warning signal for more adverse effects. In conclusion, these findings provide new insights regarding the ecotoxicological effects of environmentally relevant concentrations of microplastics on soil organisms.
The fluorolytic sol–gel synthesis is applied with the intention to obtain two different types of core–shell nanoparticles, namely, SrF2–CaF2 and CaF2–SrF2. In two separate fluorination steps for core and shell formation, the corresponding metal lactates are reacted with anhydrous HF in ethylene glycol. Scanning transmission electron microscopy (STEM) and dynamic light scattering (DLS) confirm the formation of particles with mean dimensions between 6.4 and 11.5 nm. The overall chemical composition of the particles during the different reaction steps is monitored by quantitative Al Kα excitation X-ray photoelectron spectroscopy (XPS). Here, the formation of stoichiometric metal fluorides (MF2) is confirmed, both for the core and the final core–shell particles. Furthermore, an in-depth analysis by synchrotron radiation XPS (SR-XPS) with tunable excitation energy is performed to confirm the core–Shell character of the nanoparticles. Additionally, Ca2p/Sr3d XPS intensity ratio in-Depth profiles are simulated using the software Simulation of Electron Spectra for Surface Analysis (SESSA). In principle, core–shell like particle morphologies are formed but without a sharp interface between calcium and strontium containing phases.
Surprisingly, the in-depth chemical distribution of the two types of nanoparticles is equal within the error of the experiment. Both comprise a SrF2-rich core domain and CaF2-rich shell domain with an intermixing zone between them. Consequently, the internal morphology of the final nanoparticles seems to be independent from the synthesis chronology.
Measurements of ion distributions at a charged solid–liquid interface using X-ray standing waves (XSW) are presented. High energy synchrotron radiation (17.48 keV) is used to produce an XSW pattern inside a thin water film on a silicon wafer. The liquid phase is an aqueous solution containing Br and Rb ions. The surface charge is adjusted by titration. Measurements are performed over a pH range from 2.2–9, using the native Si oxide layer and functional (amine) groups as surface charge. The Debye length, indicating the extension of the diffuse layer, could be measured with values varying between 1–4 nm. For functionalized wafers, the pH dependent change from attraction to repulsion of an ion species could be detected, indicating the isoelectric point. In combination with the measurement of the streaming current, the surface charge of the sample could be quantified.
Phoenician ivory objects (8th century B.C., Syria) from the collections of the Badisches Landesmuseum, Karlsruhe, Germany, have been studied with full field X-ray fluorescence microimaging, using synchrotron radiation (SR-FF-microXRF). The innovative Color X-ray Camera (CXC), a full-field detection device (SLcam), was used at the X-ray fluorescence beamline of the ANKA synchrotron facility (ANKA-FLUO, KIT, Karlsruhe, Germany) to noninvasively study trace metal distributions at the surface of the archeological ivory objects. The outstanding strength of the imaging technique with the CXC is the capability to record the full XRF spectrum with a spatial resolution of 48 µm on a zone of a size of 11.9 × 12.3 mm² (264 × 264 pixels). For each analyzed region, 69696 spectra were simultaneously recorded. The principal elements detected are P, Ca, and Sr, coming from the ivory material itself; Cu, characteristic of pigments; Fe and Pb, representing sediments or pigments; Mn, revealing deposited soil minerals; Ti, indicating restoration processes or correlated with Fe sediment traces; and Au, linked to a former gilding. This provides essential information for the assessment of the original appearance of the ivory carvings. The determined elemental maps specific of possible pigments are superimposed on one another to visualize their respective distributions and reconstruct the original polychromy and gilding. Reliable hypotheses for the reconstruction of the original polychromy of the carved ivories are postulated on this basis.
The Brazilian sugarcane industry produced around 173 million tons (Mt) of bagasse in 2018. Bagasse is a by-product of juice extraction for ethanol and sugar production and is combusted in order to generate power, producing up to 10 Mt of ash per year. This ash contains various concentrations of plant nutrients, which allow the ash to be used as a crop fertilizer. However, the concentration and extractability of phosphorus (P), an essential plant nutrient, are low in bagasse ash. To increase the P content, we co-gasified and co-combusted bagasse with P-rich chicken manure. The resulting ash was thermochemically post-treated with alkali additives (Na2SO4 and K2SO4) to increase the availability of P to plants. We aimed to: (i) investigate the effect of thermochemical post-treatment of co-gasification residue and co-combustion ash on P availability to soybeans, (ii) explore the potential of chemical extraction methods (citric acid, neutral ammonium citrate, formic acid, and Mehlich-I) and diffusive gradients in thin films (DGT) to predict the availability of P to soybeans, and (iii) identify the responsible P-phases using X-ray diffraction . We evaluated P availability to soybeans growing in Brazilian Oxisol soil in two independent greenhouse pot experiments. The positive effect of thermochemical treatment on P availability from gasification residue was confirmed through the observation of increased P uptake and biomass in soybean plants. These findings were confirmed by chemical extraction methods and DGT. The gasification residue contained whitlockite as its main P-bearing phase. Thermochemical post-treatment converted whitlockite into highly soluble CaNaPO4. In contrast, co-combustion ash already contained highly soluble Ca(Na,K)PO4 as its main P-bearing phase, making thermochemical post-treatment unnecessary for increasing P availability. In conclusion, increased extractability and availability of P for soybeans were closely connected to the formation of calcium alkali phosphate. Our findings indicate that this combined methodology allows for the prediction of P-fertilization effects of ash.
The Micro Structure of Traditional Brazilian Lime Plasters - The Custom House of Florianopolis
(2005)
We have developed lanthanide labeling strategies for antibodies to adapt conventional biochemical workflows like Western blot immunoassays for detection by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) analysis with a special interest to apply the multi-element capabilities of ICP-MS for the design of multiplexed immunoassays. In this paper the lanthanide labeling of antibodies with MeCAT was investigated and the reaction conditions were optimized for application in a Western blot immunoassay analyzed by LA-ICP-MS. Furthermore, the MeCAT labeling strategy was compared with two other commercially available labeling reagents, MAXPAR and SCN-DOTA. As a proof-of-principle experiment chemically induced alterations of cytochrome P450 protein expression were investigated and the suitability of the differentially labeled antibodies for Western blot immunoassays of a complex liver microsomal protein fraction was tested. Limits of detection (LODs) in the lower fmol range were reached in the Western blot application using MeCAT and MAXPAR as element labeling reagents, whereas even sub-fmol LODs can be achieved in a dot blot experiment for the pure antibodies.
To properly understand and assess the long-term behaviour of geosynthetic materials it is necessary to investigate the various types of possible degradation mechanims. This includes both chemical and mechanical behaviour, and sometimes even their interactions with one another. Clearly, chemical degradation of geosynthetics depends on the polymer type. For example, polyolefins are vulnerable to oxidation; polyesters are susceptible to hydrolysis; and plasticizers can leach from polyvinyl chloride. This paper describes the concept of these three types of degradation, but focuses on the oxidation of polyolefins since the majority of the geosynthetics is made from this type of polymer. The methods used to predict the lifetime of antioxidants and service life of the geosynthetic material will be illustrated. Furthermore, the influence of temperature, pressure, and ultraviolet light on the service life are also demonstrated. Finally, the current specifications targeting the longevity of different geosynthetics are presented.
Regarding mechanical degradation, the paper mainly focuses upon the creep deformation of geogrids and stress crack resistance (SCR) of polyethylene geomembranes and geopipe. The method to assess stress crack resistance is described, and the microscopic mechanisms that lead to such failure are explained. For creep evaluation, different acceleration tests are presented and their applicability with respect to the different types of polymers is illustrated. In addition, the long-term shear behaviour of geocomposites and geosynthetic clay liners is presented.
We measured and collected literature data for the crystal growth rate, u(T), of µ-cordierite (2MgO · 2Al2O3 · 5SiO2) and diopside (CaO · MgO · 2SiO2) in their isochemical glass forming melts. The data cover exceptionally wide temperature ranges, i.e. 8001350 °C for cordierite and 7501378 °C for diopside. The maximum of u(T) occurs at about 1250 °C for both systems. A smooth shoulder is observed around 970 °C for µ-cordierite. Based on measured and collected viscosity data, we fitted u(T) using standard crystal growth models. For diopside, the experimental u(T) fits well to the 2D surface nucleation model and also to the screw dislocation growth mechanism. However, the screw dislocation model yields parameters of more significant physical meaning. For cordierite, these two models also describe the experimental growth rates. However, the best fittings of u(T) including the observed shoulder, were attained for a combined mechanism, assuming that the melt/crystal interface growing from screw dislocations is additionally roughened by superimposed 2D surface nucleation at large undercoolings, starting at a temperature around the shoulder. The good fittings indicate that viscosity can be used to assess the transport mechanism that determines crystal growth in these two systems, from the melting point Tm down to about Tg, with no sign of a breakdown of the StokesEinstein/Eyring equation.
Aims: A laboratory study was conducted to evaluate the influence of cocultivation of toxigenic Fusarium (F.) and Alternaria (A.) fungi with respect to growth and mycotoxin production.
Methods and Results: Fusarium culmorum Fc13, Fusarium graminearum Fg23 and two Alternaria tenuissima isolates (At18 and At220) were simultaneously or consecutively co-incubated on wheat kernels in an in vitro test system. Fungal biomass was quantified by determining ergosterol content. Three Fusarium toxins (DON, NIV and ZON) and three Alternaria toxins (AOH, AME and ALT) were analysed by a newly developed HPLC/MS/MS method. In simultaneous cocultures, the fungal biomass was enhanced up to 460% compared with individual cultures; Alternaria toxins were considerably depressed down to <5%. Combining At18 and At220 with Fg23 inhibited the toxin production of both fungal partners. In contrast, Fc13 increased its DON and ZON production in competitive interaction with both A. strains.
Conclusions: The interfungal competitive effects aid the understanding of the processes of competition of both fungi in natural environments and the involvement of mycotoxins as antifungal factors.
Significance and Impact of Study:
Cocultivation significantly affects fungal growth and mycotoxin production of phytopathogenic Alternaria and Fusarium strains. The impact of mycotoxins on the interfungal competition is highlighted.
Today, quantitative data play a pivotal role in the understanding of biological processes. This is particularly true for the proteome: protein quantification always follows protein identification. To obtain useful and reliable quantitative data, rather sophisticated strategies using electrospray and MALDI mass spectrometry have been developed, which allow relative and sometimes even absolute quantification. All of those strategies have merits and limitations. In order to overcome some of these limits, methods based on the reliable and sensitive detection and quantification of heavy metals present in proteins using inductively coupled plasma (ICP)-MS have been reported. With specific labels carrying heavy metals, the applicability of ICP-MS has been extended to almost every protein. One of such covalently bound metal tags, allowing the quantification of low abundant proteins, uses 1,4,7,10-tetraazacyclododecane N,N',N'',N''-tetraacetic acid (DOTA) chelate complexes carrying lanthanides as the metal core. In this review the scope and limitations of peptide and protein quantification will be addressed. The metal tags do not only provide low detection limits, but also due to the large number of different lanthanides and lanthanide isotopes, multiplexing capabilities and previously unknown accuracy based on inherently possible isotope dilution methods came into reach. The developed workflows, including electrophoretic and chromatographic separation and preconcentration techniques, will be addressed to allow a comparison with already established procedures.
The role of mycotoxins in the microbial competition in an ecosystem or on the same host plant is still unclear. Therefore, a laboratory study was conducted to evaluate the influence of mycotoxins on growth and mycotoxin production of Fusarium and Alternaria fungi. Fusarium culmorum Fc13, Fusarium graminearum Fg23 and two Alternaria tenuissima isolates (At18 and At220) were incubated on wheat kernels supplemented with alternariol (AOH), tetramic acid derivates (TeA), deoxynivalenol (DON) and zearalenone (ZEA) in an in vitro test system. Fungal biomass was quantified by determining ergosterol content. Three Fusarium toxins (DON, nivalenol and ZEA) and three Alternaria toxins (AOH, alternariol methyl ether (AME) and altenuene) were analysed by HPLC-MS/MS. If Alternaria strains grew in wheat kernels spiked with Fusarium mycotoxins, their growth rates were moderately increased, their AOH and AME production was enhanced and they were simultaneously capable of degrading the Fusarium mycotoxins DON and ZEA. In contrast, both Fusarium strains behaved quite differently. The growth rate of Fc13 was not distinctly influenced, while Fg23 increased its growth in wheat kernels spiked with AOH. TeA depressed the ergosterol content in Fc13 as well as in Fg23. The DON production of Fc13 was slightly depressed, whereas the ZEA production was significantly increased. In contrast, Fg23 restricted its ZEA production. Both Fusarium strains were not capable of degrading the Alternaria mycotoxin AOH. Mycotoxins might play an important role in the interfungal competitive processes. They influence growth rates and mycotoxin production of the antagonistic combatants. The observed effects between phytopathogenic Alternaria and Fusarium strains and their mycotoxins aid the understanding of the complexity of microbial competitive behaviour in natural environments.
A glass of the composition 37BaO·16CaO·47SiO2 wt% produced on an industrial scale is crystallized at 970 °C for times ranging from 15 min to 2 h. The crystallization at the immediate surface as well as the crystal growth into the bulk are analyzed using scanning electron microscopy (SEM) including energy dispersive X-ray spectroscopy (EDXS) and electron backscatter diffraction (EBSD) as well as X-ray diffraction in the Θ–2Θ setup (XRD). The immediate surface shows the oriented nucleation of walstromite as well as the formation of wollastonite and an unknown phase of the composition BaCaSi3O8. All three phases also grow into the bulk where walstromite ultimately dominates the kinetic selection and grows throughout the bulk due to a lack of bulk nucleation. Walstromite shows systematic orientation changes as well as twinning during growth. A critical analysis of the XRD-patterns acquired from various crystallized samples indicates that their evaluation is problematic and that phases detected by XRD in this system should be verified by another method such as EDXS.
Mycotoxigenic fungal pathogens Fusarium and Alternaria are a leading cause of loss in cereal production. On wheat-ears, they are confronted by bacterial antagonists such as pseudomonads.
Studies on these groups’ interactions often neglect the infection process’s temporal aspects and the associated priority effects. In the present study, the focus was on how the first colonizer affects the subsequent ones. In a climate chamber experiment, wheat-ears were successively inoculated with two different strains (Alternaria enuissima At625, Fusarium graminearum Fg23, or Pseudomonas simiae Ps9).
Over three weeks, microbial abundances and mycotoxin concentrations were analyzed and visualized via Self Organizing Maps with Sammon Mapping (SOM-SM). All three strains revealed different characteristics and strategies to deal with co-inoculation: Fg23, as the first colonizer, suppressed the establishment of At625 and Ps9. Nevertheless, primary inoculation of At625 reduced all of the Fusarium toxins and stopped Ps9 from establishing. Ps9 showed priority effects in delaying and blocking the production of the fungal mycotoxins. The SOM-SM analysis visualized the competitive strengths: Fg23 ranked first, At625 second, Ps9 third. Our findings of species-specific priority effects in a natural environment and the role of the mycotoxins involved are relevant for developing biocontrol strategies.
Die Synchrotron-Refraktions-Topographie basiert auf der Brechung von Röntgenstrahlung an den Grenzflächen zwischen Materialien mit unterschiedlichem Brechungsindex. Refraktionseffekte verändern die Ausbreitungsrichtung der Röntgenstrahlung, welche mit Hilfe der Methode des Analyser-Based Imaging analysiert wird. Dabei wird ein Silizium-Einkristall im Strahlengang zwischen Probe und Detektor platziert. Dieser Analysator-Kristall filtert, innerhalb seiner Streuebene, die Röntgenstrahlung gemäß ihrer Ausbreitungsrichtung. Durch das Rastern verschiedener Winkelpositionen des Analysator-Kristalls erhält man das Winkelspektrum der von der Probe gebrochenen Strahlung. Aus dieser Rocking Curve lässt sich die spezifische innere Oberfläche der Probe bestimmen. Diese Information wird über einen 2D-Detektor mit einer nominellen Pixelgröße von 3,6 μm gewonnen. Die Installation einer Zugprüfmaschine ermöglicht es die Proben in verschiedenen Lastzuständen insitu zu untersuchen. Damit ist es möglich die spezifische innere Oberfläche in Abhängigkeit der Last darzustellen und so Schädigungsmechanismen abzuleiten. Der Vorteil bei der Ausnutzung des Refraktionseffekts gegenüber der einfachen Durchstrahlung ist die höhere Sensitivität gegenüber Defekten mit geringem Volumen aber großer Oberfläche. Somit werden auch Mikrorisse und, speziell bei Kompositen, die Enthaftung zwischen Matrix und Verstärkung (Partikel, Fasern) erfasst. In dieser Studie wurden Metall-Matrix-Komposite bestehend aus einer Aluminium-Matrix verstärkt mit Aluminiumoxid-Partikeln untersucht. Hierzu wurden knochenförmige Zugproben präpariert, deren Messlänge einen rechteckigen Querschnitt von 1,7 mm × 1,3 mm aufwies. Die Proben wurden einem Zugversuch unterzogen, welcher in Intervallen unterbrochen wurde. Bei jeder Unterbrechung wurde unter quasi-statischer Last die Rocking Curve gemessen und ein Radiogramm der spezifischen inneren Oberflächen berechnet. Dabei konnte ab dem Erreichen einer Last von ca. 600 N ein Anstieg der spezifischen inneren Oberfläche beobachtet werden. Demgegenüber zeigen die zum Vergleich durchgeführten Durchstrahlungsaufnahmen keinerlei Defekte. Daher belegt diese Untersuchung das Potential der Refraktion-Topographie zur frühzeitigen Erkennung von Schädigungen mit hoher Empfindlichkeit.