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Working towards a comprehensive understanding of introduction pathways, number, and fate of micro¬plastics in the environment, suitable analytical methods are a precondition. Micro-spectroscopic methods are probably the most widely used techniques. Besides their ability to measure single spectra of a particle or fiber, most modern FTIR- and Raman microscopes are also capable of two-dimensional imaging. This is very appealing to microplastics research because it allows to simultaneously characterize the analytes chemically as well as their size (distribution) and shape.
Two-dimensional imaging on extensive sample areas with FTIR-micros¬copes is facilitated by focal plane array (FPA) detectors resulting in large data sets comprised of up to several million spectra. With numbers too large for manual inspection of each individual spectrum, automated data evaluation is inevitable. Identifying different polymers based on the comparison with known reference spectra (library search) has proven to be a suitable approach. For that purpose, FTIR-spectra of common plastics can be collected to create an individual reference library.
To Supplement this ‘targeted analysis’, looking for known substances via library search, an exploratory approach was tested. Principal component analysis (PCA) proved to be a helpful tool to drastically reduce the size of the data set while maintaining the significant information. Subsequently, cluster analysis was used to find groups of similar spectra. Spectra found in different clusters could be assigned to different polymer types. The variation observed within clusters gives a hint on chemical variability of microplastics of the same polymer found in the sample. Spectra labeled according to the respective cluster/polymer type were used to build a classification model which allowed to quickly predict the polymer type based on the FTIR spectrum. Classification was tested on a second, independent data set and results were compared to the spectral library search procedure.
During the service life of structural sealant glazing (SSG) facades, the loadbearing capacity of the silicone bonds needs to be guaranteed. Laboratory Tests can assess the durability of SSG-systems based on mechanical characteristics of the bond after simultaneous exposure to both climatic and mechanical loads.
This article studies how the material characteristics of two common structural sealants are affected by laboratory and field exposure. Dynamic mechanical Analysis (DMA) confirms a reduction in the dynamic modulus of exposed Silicone samples. Results from thermogravimetric analysis, Fourier-transform infrared spectroscopy, differential scanning calorimetry, and small-angle X-ray scattering/wide-angle X-ray scattering show differences between the two sealants and indicate no/minor changes in the composition and morphology of the laboratory and field exposed sealants. Mechanical characterization methods, such as DMA, and tensile and shear testing of the structural bond, are shown to be sensitive toward the combined climatic and mechanical loadings, and are hence suitable for studying degradation mechanisms of structural sealants.
To arrive to sustainable hydrogen-based energy solutions, the understanding of water-splitting catalysts plays the most crucial role. Herein, state-of-the-art hypotheses are combined on electrocatalytic active metal sites toward the oxygen evolution reaction (OER) to develop a highly efficient catalyst based on Earth-abundant cobalt and zinc oxides.
The precursor catalyst Zn0.35Co0.65O is synthesized via a fast microwaveassisted approach at low temperatures. Subsequently, it transforms in situ from the wurtzite structure to the layered γ-Co(O)OH, while most of its zinc leaches out. This material shows outstanding catalytic Performance and stability toward the OER in 1 m KOH (overpotential at 10 mA cm−2 ηinitial = 306 mV, η98 h = 318 mV). By comparing the electrochemical results and ex situ analyses to today’s literature, clear structureactivity correlations are able to be identified. The findings suggest that coordinately unsaturated cobalt octahedra on the surface are indeed the active centers for the OER.
The characterization of the active structure of water-splitting catalysts is crucial to evolve to a sustainable energy future based on hydrogen. Such information can only be obtained by operando methods. We present a diffuse reflectance UV-vis (DRUV) spectroelectrochemical study that allows tracking the changes of solid oxygen evolution catalysts under working conditions. The versatility of our approach is demonstrated on two cobalt-containing catalysts, Zn0.35Co0.65O and CoAl2O4. The changes the catalysts undergo during the oxygen evolution reaction can be tracked by probing the electronic structure using UV-vis spectroscopy. These findings are compared to ex situ analyses, which support the assignments of the structures stabilized under different potentials. Thus, structure–activity correlations can be proposed, and deeper insights into the catalytically active structures can be obtained.
Nonporous corundum powder, known as an abrasive material in the industry, was functionalized covalently with protein binders to isolate and enrich specific proteins from complex matrices. The materials based on corundum were characterized by TEM, ESEM, BET, DLS, EDS, and zeta potential measurements. The strong Al-O-P bonds between the corundum surface and amino phosphonic acids were used to introduce functional groups for further conjugations. The common crosslinker glutaraldehyde was compared with a hyperbranched polyglycerol (PG) of around 10 kDa. The latter was oxidized with periodate to generate aldehyde groups that can covalently react with the amines of the surface and the amino groups from the protein via a reductive amination process. The amount of bound protein was quantified via aromatic amino acid analysis (AAAA). This work shows that oxidized polyglycerol can be used as an alternative to glutaraldehyde. With polyglycerol, more of the model protein bovine serum albumin (BSA) could be attached to the surface under the same conditions, and lower non-specific binding (NSB) was observed. As a proof of concept, IgG was extracted with protein A from crude human plasma. The purity of the product was examined by sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE). A binding capacity of 1.8 mg IgG per gram of corundum powder was achieved. The advantages of corundum include the very low price, extremely high physical and chemical stability, pressure resistance, favorable binding kinetics, convenient handling, and flexible application.
Nonporous corundum powder, known as an abrasive material in the industry, was functionalized covalently with protein binders to isolate and enrich specific proteins from complex matrices. The materials based on corundum were characterized by TEM, ESEM, BET, DLS, and zeta potential measurements. The strong Al-O-P bonds between the corundum surface and amino phosphonic acids are used to introduce functional groups for further conjugations. The common cross-linker glutaraldehyde was compared with a hyperbranched polyglycerol (PG) of around 10 kDa. The latter is oxidized with periodate to generate aldehyde groups that can covalently react with the amines of the surface and the amino groups from the protein via a reductive amination process. The amount of bound protein was quantified via aromatic amino acid analysis (AAAA). This work shows that oxidized polyglycerol can be used as an alternative to glutaraldehyde. With polyglycerol, more of the model protein bovine serum albumin (BSA) could be attached to the surface under the same conditions, and lower nonspecific binding (NSB) was observed. As a proof of concept, IgG was extracted with protein A from crude human plasma. The purity of the product was examined by SDS-PAGE. A binding capacity of 1.8 mg IgG per g of corundum powder was achieved. The advantages of corundum are the very low price, extremely high physical and chemical stability, pressure resistance, favorable binding kinetics, and flexible application.
Nonporous corundum powder was functionalized covalently with protein binders to isolate and enrich specific proteins from complex matrices.The common crosslinker glutaraldehyde was compared with a hyperbranched polyglycerol (PG) of around 10 kDa. The latter was oxidized with periodate to generate aldehyde groups that can covalently react with the amines of the surface and the amino groups from the protein via a reductive amination process. The amount of bound protein was quantified via aromatic amino acid analysis (AAAA). As a proof of concept, IgG was extracted with protein A from crude human plasma. The advantages of corundum include the very low price, extremely high physical and chemical stability, pressure resistance, favorable binding kinetics, convenient handling, and flexible application.
ZnO nanoparticles are found in different food and consumer products, and their toxicological effects are still under investigation. It is therefore important to understand their behavior in the gastrointestinal tract. Here, we used an in vitro model to assess the physicochemical fate of ZnO nanoparticles during the digestive process in artificial saliva, stomach juice, and intestinal juice. Atomic absorption spectrometry and small-angle X-ray scattering were employed to investigate two ZnO nanomaterials, one intensively characterized reference material and soluble ZnCl2 in a broad range of concentrations between 25 and 1000 μg/mL in the intestinal fluid. Because food components may influence the behavior of nanomaterials in the gastrointestinal tract, starch, milk powder, and olive oil were used to mimic carbohydrates, protein, and fat, respectively. Additionally, ion release of all Zn species was assessed in cell culture media and compared to artificial intestinal juice to investigate relevance of typical cell culture conditions in ZnO nanotoxicology. ZnCl2 as well as the ZnO species were present as particles in artificial saliva but were solubilized completely in the acidic stomach juice. Interestingly, in the intestinal fluid a concentration-independent de novo formation of particles in the nanoscale range was shown. This was the case for all particles as well as for ZnCl2, regardless of the concentration used. Neither of the food components affected the behavior of any Zn species. On the contrary, all Zn species showed a Zn-concentration-dependent ion release in common cell culture medium. This questions the suitability of cell culture studies to investigate the effect of ZnO nanoparticles on intestinal cells. Our results show that Zn-containing nanoparticles reach the intestine. This underlines the importance of determining the influence of the test environment on nanoparticle fate.
Iron oxides used as food colorants are listed in the European Union with the number E172. However, there are no specifications concerning the fraction of nanoparticles in these pigments.
Here, seven E172 products were thoroughly characterized. Samples of all colors were analyzed with a Broad spectrum of methods to assess their physico-chemical properties. Small-Angle X-ray Scattering (SAXS), Dynamic Light Scattering (DLS), Transmission Electron Microscopy (TEM), zeta-potential, Inductively Coupled Plasma-Mass Spectrometry (ICP-MS), X-ray diffraction (XRD), Brunauer-Emmett-Teller analysis (BET), Asymmetric Flow Field-Flow Fractionation (AF4) and in vitro cell viability measurements were used.
Nanoparticles were detected in all E172 samples by TEM or SAXS measurements. Quantitative results from both methods were comparable. Five pigments were evaluated by TEM, of which four had a size median below 100 nm, while SAXS showed a size median below 100 nm for six evaluated pigments. Therefore, consumers May be exposed to iron oxide nanoparticles through the consumption of food pigments.
Iron oxide nanoparticles gain increasing attention due to their broad industrial use. However, safety concerns exist since their effects on human cells are still under investigation. The presence of iron oxide nanoparticles in the food pigment E172 has been shown recently. Here, we studied four iron oxide nanoparticles, one food pigment E172 and the ionic control FeSO4 regarding dissolution in biological media, uptake and transport, and cellular effects in vitro in human intestinal Caco-2 and HepaRG hepatocarcinoma cells. The iron oxide nanoparticles passed the gastrointestinal passage without dissolution and reached the intestine in the form of particles. Minor uptake was seen into Caco-2 cells but almost no transport to the basolateral site was detected for any of the tested particles. HepaRG cells showed higher particle uptake. Caco-2 cells showed no alterations in reactive oxygen species production, apoptosis, or mitochondrial membrane potential, whereas two particles induced apoptosis in HepaRG cells, and one altered mitochondrial membrane potential at non-cytotoxic concentrations. No correlation between physicochemical particle characteristics and cellular effects was observed, thus emphasizing the Need for case-by-case assessment of iron oxide nanoparticles.