Analytische Chemie
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The importance of microRNA (miRNA) dysregulation for the development and progression of diseases and the discovery of stable miRNAs in peripheral blood have made these short-sequence nucleic acids next-generation biomarkers. Here we present a fully homogeneous multiplexed miRNA FRET assay that combines careful biophotonic design with various RNA hybridization and ligation steps. The single-step, single-temperature, and amplification-free assay provides a unique combination of performance parameters compared to state-of-the-art miRNA detection technologies. Precise multiplexed quantification of miRNA-20a, -20b, and -21 at concentrations between 0.05 and 0.5 nm in a single 150 mL sample and detection limits between 0.2 and 0.9 nm in 7.5 mL serum samples demonstrate the feasibility of both highthroughput and point-of-care clinical diagnostics.
A new method for sampling wear particles directly from the lubricant reservoir has been developed and applied successfully for analyzing wear particles by high-resolution scanning electron microscopy in transmission mode having coupled energy-dispersive X-ray spectroscopy. The lubricated tribological testing was carried out with fully formulated as well as with non-formulated synthetic base oil. It was possible to analyze individual particles with dimensions as small as about 5–30 nm which are likely the 'primary' wear particles. A majority of the particles, however, are agglomerated and, thus, lead to the formation of larger agglomerates of up to a few micrometers. Chemical analysis led to the conclusion that most of the observed particles generated in formulated oil, especially the larger ones, are composed of the additives of the lubricant oil. In non-formulated base oil, the primary particles are of similar dimensions but contain only iron, chromium and oxygen, but most likely stem from the mating materials. This finding points to the fact that the main wear mechanism under lubricated conditions with fully formulated oil is more like a continuous shearing process rather than a catastrophic failure with the generation of larger primary particles. When the oil is non-formulated, however, several wear mechanisms act simultaneously and the wear rate is increased significantly. Generated larger primary particles are milled down to the nanoscale. When the oil is fully formulated, wear mainly takes places at the additive layer or tribofilm; thus, the steel surface is protected.
The catalytic efficiency of two magnetically responsive nanocatalysts was evaluated for the Degradation of Reactive Black 5 (RB5) and Reactive Yellow 84 (RY84) azo dyes using hydrogen peroxide as oxidant undervery mild conditions (atmospheric pressure, room temperature). In order to obtain the nanocatalysts, thesurface of magnetite (Fe3O4) nanoparticles, prepared by a co-precipitation method, was further modified with ferrous oxalate, a highly sensitive non-hazardous reducing agent. The sensitized nanomaterials were characterized by X-ray diffraction, scanning and transmission electron microscopy, energy-dispersive X-ray spectroscopy and vibrating sample magnetometry, and used in the catalytic wet hydrogen peroxideoxidation (CWHPO) of RB5 and RY84, in laboratory-scale experiments. The effect of important variables such as catalyst dosage, H2O2 concentration, and contact time was studied in the dye Degradation kinetics. The results showed that it was possible to remove up to 99.7% dye in the presence of 20 mM H2O2 after 240 min of oxidation for a catalyst concentration of 10 g L−1at 25◦C and initial pH value of 9.0.CWHPO of reactive dyes using sensitized magnetic nanocatalysts can be a suitable pre-treatment methodfor complete decolorization of effluents from textile dyeing and finishing processes, once the Optimum operating conditions are established.
In carrier gas hot extraction the calibration of low amounts of non-metals with masses of a few micrograms with small uncertainty remains a challenge. To achieve high flexibility a high precision gas mixture pump was combined with an automated syringe drive. The gas mixing pump allows filling the syringe with different gas compositions; the automated syringe drive allows matching to modulate the signal profiles to those of real samples. The system was designed and its experimental potential explored. The resulting calibration curves were comparable to those obtained by calibration using solid materials of sufficient purity and stoichiometry. However smaller uncertainties and lower limits of quantification (i.e. 0.5 µg and 0.6 µg for O and N, respectively) were found using the gas calibration device.
An experimental investigation has been carried out to characterize and discriminate seven saffron samples and to verify their declared geographical origin using a voltammetric electronic tongue (VE-tongue). The ability of multivariable analysis methods such as Principal Component Analysis (PCA), Hierarchical Cluster Analysis (HCA) to classify the saffron samples according to their geographical origin have been investigated. A good discrimination has reached using PCA and HCA in the VE-tongue characterization case. Furthermore, cross validation and Partial Least Square (PLS) techniques were applied in order to build suitable management and prediction models for the determination of safranal concentration in saffron samples based on SPME-GC-MS and UV-Vis Spectrophotometry. The obtained results reveals that some relationships were established between the VE-tongue signal, SPMEGC-MS and UV-Vis spectrophotometry methods to predict safranal concentration levels in saffron samples by using the PLS model. In the light of these results, we can say that the proposed electronic system offer a fast, simple and efficient tool to recognize the declared geographical origin of the saffron samples.
Micro structured reactors are attractive candidates for further process intensification in heterogeneous catalysis. However, they require catalytic coatings with significantly improved space-time yields compared to traditional supported catalysts. We report the facile synthesis of homogeneous nanocrystalline Pt coatings with hierarchical pore structure by electrochemical dealloying of amorphous sputter-deposited platinum silicide layers. Thickness, porosity and surface composition of the catalysts can be controlled by the dealloying procedure. XPS analysis indicates that the catalyst surface is primarily composed of metallic Pt. Catalytic tests in gas-phase hydrogenation of butadiene reveal the typical activity, selectivity and activation energy of nanocrystalline platinum. However, space time yields are about 13 to 200 times higher than values reported for Pt-based catalysts in literature. The highly open metallic pore structure prevents heat and mass transport limitations allowing for very fast reactions and reasonable stability at elevated temperatures.
Recently developed new transducers for ultrasonic transmission, which can be embedded right into concrete, are now used for non-destructive permanent monitoring of concrete. They can be installed during construction or thereafter. Large volumes of concrete can be monitored for changes of material properties by a limited number of transducers. The transducer design, the main properties as well as installation procedures are presented. It is shown that compressional waves with a central frequency of 62 kHz are mainly generated around the transducer's axis. The transducer can be used as a transmitter or receiver. Application examples demonstrate that the transducers can be used to monitor concrete conditions parameters (stress, temperature,
) as well as damages in an early state or the detection of acoustic events (e.g., crack opening). Besides application in civil engineering our setups can also be used for model studies in geosciences.
In this paper, we present a new dataset consisting of 19,407 X-ray images. The images are organized in a public database called GDXray that can be used free of charge, but for research and educational purposes only. The database includes five groups of X-ray images: castings, welds, baggage, natural objects and settings. Each group has several series, and each series several X-ray images. Most of the series are annotated or labeled. In such cases, the coordinates of the bounding boxes of the objects of interest or the labels of the images are available in standard text files. The size of GDXray is 3.5 GB and it can be downloaded from our website. We believe that GDXray represents a relevant contribution to the X-ray testing community. On the one hand, students, researchers and engineers can use these X-ray images to develop, test and evaluate image analysis and computer vision algorithms without purchasing expensive X-ray equipment. On the other hand, these images can be used as a benchmark in order to test and compare the performance of different approaches on the same data. Moreover, the database can be used in the training programs of human inspectors.
A novel synthetic strategy toward highly fluorinated BODIPY dyes with exceptional photostabilities relying on sustainable gold catalysis has been developed. A key to the tailored pyrrole precursors is the gold catalysis performed in ionic liquids as the reaction medium, allowing a facile recycling of the catalysts. The dyes prepared are well-matching with the spectral windows of popular rhodamine dyes and possess high brightness while showing a distinctly higher photostability than the rhodamines especially in aprotic solvents.
CONRAD-2 is an imaging instrument using low-energy (cold) neutrons. The instrument is installed at the end of a curved neutron guide which avoids the direct line of sight towards the reactor core. This ensures a very low background of high-energy neutrons and. photons at the sample position. The cold neutron beam provides a wavelength range which is suitable for phase-and diffraction-contrast imaging such as grating interferometry and Bragg edge mapping. The instrument is well suited for high resolution imaging due to the high efficiency of the very thin scintillators that can be used for the detection of cold neutrons. An instrument upgrade was performed recently as a part of an upgrade program for the cold neutron instrumentation at HZB. The parameters of the instrument as well as some research highlights will be presented.