Wissenschaftliche Artikel der BAM
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Various plant compartments of a single bell pepper plant were studied to verify the variability of boron isotope composition in plants and to identify possible intra-plant isotope fractionation. Boron mass fractions varied from 9.8 mg/kg in the fruits to 70.0 mg/kg in the leaves. Boron (B) isotope ratios reported as δ11B ranged from -11.0 to +16.0 (U ≤ 1.9, k=2) and showed a distinct trend to heavier δ11B values the higher the plant compartments were located in the plant. A fractionation of Δ11Bleaf-roots = 27 existed in the studied bell pepper plant, which represents about about 1/3 of the overall natural boron isotope variation (ca. 80). Two simultaneous operating processes are a possible explanation for the observed systematic intra-plant δ11B variation: 1) B is fixed in cell walls in its tetrahedral form (borate), which preferentially incorporates the light B isotope and the remaining xylem sap gets enriched in the heavy B isotope and 2) certain transporter preferentially transport the trigonal 11B-enriched boric acid molecule and thereby the heavy 11B towards young plant compartments which were situated distal of the roots and typically high in the plant. Consequently, an enrichment of the heavy 11B isotope in the upper young plant parts located at the top of the plant could explain the observed isotope systematic. The identification and understanding of the processes generating systematic intra-plant δ11B variations will potentially enable the use of B isotope for plant metabolism studies.
Lewis and Brønsted sites were quantified in a series of weak acidic hydroxylated magnesium fluorides by Fourier transform infrared spectroscopy (FTIR) and solid state nuclear magnetic resonance spectroscopy (NMR) with pyridine as probe molecule. Molar extinction coefficients, which are necessary for quantitative FTIR measurements, were calculated by an easy approach. It utilizes the fact that both signals, used for the quantification by FTIR, are caused by the same deformation vibration mode of pyridine. Comparison of quantitative FTIR experiments and quantification by NMR shows that concentrations of acidic sites determined by FTIR spectroscopy have to be interpreted with caution. Furthermore, it is shown that the transfer of molar extinction coefficients from one catalyst to another may lead to wrong results. Molar extinction coefficients and concentrations of acidic sites determined by FTIR spectroscopy are affected by grinding and probably the particle size of the sample. High temperature during FTIR experiments has further impact on the quantification results.
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.
The need for technological progress in bio-diagnostic assays of high complexity requires both fundamental research and constructing efforts on nano-scaled assay recognition elements that can provide unique selectivity and design-enhanced sensitivity features. Nanoparticle induced sensitivity enhancement and its application related to multiplexed capability Surface-Enhanced InfraRed Absorption (SEIRA) assay formats are well suitable for these purposes. The potential of diverse fluorophore–antibody conjugates, being chemisorbed onto low-cost gold nanoparticulate SEIRA substrates, has been explored with respect to their spectral discriminability. These novel biolabels deliver molecular SEIRA fingerprints that have been successfully analyzed by both uni- and multivariate analyzing tools, to discriminate their multiplexing capabilities. We show that this robust spectral encoding via SEIRA fingerprints opens up new opportunities for a fast, reliable and multiplexed high-end screening in biodiagnostics.
The reaction of iron chlorides with an alkaline reagent is one of the most prominent methods for the synthesis of iron oxide nanoparticles. We studied the particle formation mechanism using triethanolamine as reactant and stabilizing agent. In situ fast-X-ray absorption near edge spectroscopy and small-angle X-ray scattering provide information on the oxidation state and the structural information at the same time. In situ data were complemented by ex situ transmission electron microscopy, wide-angle X-ray scattering and Raman analysis of the formed nanoparticles. The formation of maghemite nanoparticles (γ-Fe2O3) from ferric and ferrous chloride was investigated. Prior to the formation of these nanoparticles, the formation and conversion of intermediate phases (akaganeite, iron(II, III) hydroxides) was observed which undergoes a morphological and structural collapse. The thus formed small magnetite nanoparticles (Fe3O4) grow further and convert to maghemite with increasing reaction time.
While polymorphism is a common phenomenon in the crystallization processes of organic compounds, polyamorphism has gained importance only recently. Using sophisticated sample environments and applying in situ scattering methods and vibrational spectroscopy, the complete crystallization process of organic compounds from solution can be traced and characterized. Diffuse scattering from amorphous intermediates can be investigated by analyzing the atomic pair distribution function (PDF) to gain further insights into molecular pre-orientation. The crystallization behavior of paracetamol was studied exemplarily under defined, surface-free conditions. Based on the choice of the solvent, the formation of different polymorphs is promoted. The thermodynamically stable form I and the metastable orthorhombic form II could be isolated in pure form directly from solution. For both polymorphs, the crystallization from solution proceeds via a distinct amorphous precursor phase. PDF analyses of these different amorphous states indicate a specific pre-orientation of the analyte molecules introduced by the solvent. The resulting crystalline polymorph is already imprinted in these proto-crystalline precursors. Direct experimental evidence for the polyamorphism of paracetamol is provided.
We present the results of several machine learning (ML)- inspired data fusion algorithms applied to multi-sensory nondestructive testing (NDT) data. Our dataset consists of Impact-Echo (IE), Ultrasonic Pulse Echo (US) and Ground Penetrating Radar (GPR) data collected on large-scale concrete specimens with built–in simulated honeycombing defects. The main objective is to improve the detectability of honeycombs by fusing the information from the three different sensors. We describe normalization, feature detection and optimal feature selection. We have used unsupervised and supervised ML, i.e., classification and clustering, for data fusion. We demonstrate the advantage of data fusion in reducing the false positives up to 10% compared to the best single sensor, thus, improving the detectability of the defects. The methods were evaluated on a concrete specimen. The effectiveness of the proposed approach was demonstrated on a separate full-scale concrete specimen. The results indicate the transportability of the conclusions from one specimen to the other.
Für die Prüfung von Leichtbaustrukturen ist in den letzten Jahren ein vermehrter Einsatz der Luftultraschallprüfung zu verzeichnen. Insbesondere eignet sich Luftultraschall für die Prüfung von Faserkunststoffverbunden und hybrider Werkstoffverbunde, die ihre Anwendung in der Automobilindustrie und Luftfahrt finden. Für den Bau von marktüblichen Luftultraschall-Wandlern werden Piezokomposite mit Anpassschichten versehen. Ihre Herstellung ist allerdings sehr anspruchsvoll und die erreichbaren Signal-Rausch-Abstände sind für viele Prüfprobleme als noch nicht ausreichend einzustufen. Zwecks gesteigerter Effizienz beim Schallübertrag in die Luft wurden Luftultraschall-Sender und -Empfänger aus zellulärem Polypropylen entwickelt. Dieses piezoelektrische Material ist aufgrund seiner geringer Dichte und seiner sehr geringen Schallgeschwindigkeit an die niedrige akustische Impedanz der Luft deutlich besser angepasst, als die üblicherweise verwendeten Anpassschichten. Letztere können bei Polypropylen-Wandlern daher gänzlich vermieden werden.
In diesem Beitrag wird Luftultraschall-Prüfung an zwei verschiedenen CFK-Testkörpern vorgestellt: an einer Platte mit T-Stringern aus dem Seitenleitwerk eines Flugzeugs und an einer Platte mit künstlich eingebrachten Fehlern. Es wurde mit unterschiedlichen planaren und fokussierenden Wandlern geprüft. Marktübliche Wandler mit Anpassschichten wurden mit den selbstentwickelten Wandlern aus zellulärem Polypropylen verglichen. Der Signal-Rausch-Abstand und die laterale Auflösung wurden sowohl im Prüfaufbau mit senkrechter Einschallung als auch mit Schrägeinschallung gemessen. Die Ergebnisse zeigen, dass die Schrägeinschallung zwar den Signal-Rauschabstand erhöht, aber die laterale Auflösung verschlechtern kann.
Effect of fluorescent staining on size measurements of polymeric nanoparticles using DLS and SAXS
(2015)
The influence of fluorescence on nanoparticle size measurements using dynamic light scattering (DLS) and small angle X-ray scattering (SAXS) was investigated. For this purpose, two series of 100 nm-sized polymer nanoparticles stained with different concentrations of the fluorescent dyes DY555 and DY680 were prepared, absorbing/emitting at around 560 nm/590 nm and 695 nm/715 nm, respectively. SAXS measurements of these particle series and a corresponding blank control (without dye) revealed similar sizes of all particles within an uncertainty of 1 nm. DLS measurements carried out at three different laboratories using four different DLS instruments and two different laser wavelengths, i.e., 532 nm and 633 nm, revealed also no significant changes in size (intensity-weighted harmonic mean diameter, ZAverage) and size distribution (polydispersity index, PI) within and between the two dye-stained particle series and the blank sample. Nevertheless, a significant decrease of the detected correlation coefficients was observed with increasing dye concentration, due to the increased absorption of the incident light and thus, less coherent light scattering. This effect was wavelength dependent, i.e. only measurable for the dye-stained particles that absorb at the laser wavelength used for the DLS measurements.
This paper describes the production and characteristics of the nanoparticle test materials prepared for common use in the collaborative research project NanoChOp (Chemical and optical characterization of nanomaterials in biological systems), in casu suspensions of silica nanoparticles and CdSe/CdS/ZnS quantum dots (QDs). This paper is the first to illustrate how to assess whether nanoparticle test materials meet the requirements of a "reference material" (ISO Guide 30, 2015) or rather those of the recently defined category of "representative test material (RTM)" (ISO/TS 16195, 2013). The NanoChOp test materials were investigated with small-angle X-ray scattering (SAXS), dynamic light scattering (DLS), and centrifugal liquid sedimentation (CLS) to establish whether they complied with the required monomodal particle size distribution. The presence of impurities, aggregates, agglomerates, and viable microorganisms in the suspensions was investigated with DLS, CLS, optical and electron microscopy and via plating on nutrient agar. Suitability of surface functionalization was investigated with attenuated total reflection Fourier transform infrared spectrometry (ATR-FTIR) and via the capacity of the nanoparticles to be fluorescently labeled or to bind antibodies. Between-unit homogeneity and stability were investigated in terms of particle size and zeta potential. This paper shows that only based on the outcome of a detailed characterization process one can raise the status of a test material to RTM or reference material, and how this status depends on its intended use.