660 Chemische Verfahrenstechnik
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Nitrosamines have been identified as a probable human carcinogen and thus are of high concern in many manufacturing industries and various matrices (for example pharmaceutical, cosmetic and food products, workplace air or potable- and wastewater). This study aims to analyse nine nitrosamines relevant in the field of occupational safety using a gas chromatography-drift tube ion mobility spectrometry (GC-DT-IMS) system. To do this, single nitrosamine standards as well as a standard mix, each at 0.1 g/L, were introduced via liquid injection. A GC-DT-IMS method capable of separating the nitrosamine signals according to retention time (first dimension) and drift time (second dimension) in 10 min was developed. The system shows excellent selectivity as each nitrosamine gives two signals pertaining to monomer and dimer in the second dimension. For the first time, reduced ion mobility values for nitrosamines were determined, ranging from 1.18 to 2.03 cm2s−1V−1. The high selectivity of the GC-DT-IMS method could provide a definite advantage for monitoring nitrosamines in different manufacturing industries and consumer products.
Monitoring the content of dissolved ozone in purified water is often mandatory to ensure the appropriate levels of disinfection and sanitization. However, quantification bears challenges as colorimetric assays require laborious off-line analysis, while commercially available instruments for electrochemical process analysis are expensive and often lack the possibility for miniaturization and discretionary installation. In this study, potentiometric ionic polymer metal composite (IPMC) sensors for the determination of dissolved ozone in ultrapure water (UPW) systems are presented. Commercially available polymer electrolyte membranes are treated via an impregnation-reduction method to obtain nanostructured platinum layers. By applying 25 different synthesis conditions, layer thicknesses of 2.2 to 12.6 µm are obtained. Supporting radiographic analyses indicate that the platinum concentration of the impregnation solution has the highest influence on the obtained metal loading. The sensor response behavior is explained by a Langmuir pseudo-isotherm model and allows the quantification of dissolved ozone to trace levels of less than 10 µg L−1. Additional statistical evaluations show that the expected Pt loading and radiographic blackening levels can be predicted with high accuracy and significance (R2adj. > 0.90, p < 10−10) solely from given synthesis conditions.
Thermo-chemical conversion of cucumber peel waste for biobased energy and chemical production
(2022)
Modeling of Creep Behavior of Particulate Composites with Focus on Interfacial Adhesion Effect
(2022)
Evaluation of creep compliance of particulate composites using empirical models always provides parameters depending on initial stress and material composition. The effort spent to connect model parameters with physical properties has not resulted in success yet. Further, during the creep, delamination between matrix and filler may occur depending on time and initial stress, reducing an interface adhesion and load transfer to filler particles. In this paper, the creep compliance curves of glass beads reinforced poly(butylene terephthalate) composites were fitted with Burgers and Findley models providing different sets of time-dependent model parameters for each initial stress. Despite the finding that the Findley model performs well in a primary creep, the Burgers model is more suitable if secondary creep comes into play; they allow only for a qualitative prediction of creep behavior because the interface adhesion and its time dependency is an implicit, hidden parameter. As Young’s modulus is a parameter of these models (and the majority of other creep models), it was selected to be introduced as a filler content-dependent parameter with the help of the cube in cube elementary volume approach of Paul. The analysis led to the time-dependent creep compliance that depends only on the time-dependent creep of the matrix and the normalized particle distance (or the filler volume content), and it allowed accounting for the adhesion effect. Comparison with the experimental data confirmed that the elementary volume-based creep compliance function can be used to predict the realistic creep behavior of particulate composites.
Silicon carbide and graphene possess extraordinary chemical and physical properties. Here, these different systems are linked and the changes in structural and dynamic properties are investigated. For the simulations performed a classical molecular dynamic (MD) approach was used. In this approach, a graphene layer (N = 240 atoms) was grafted at different distances on top of a 6H-SiC structure (N = 2400 atoms) and onto a 3C-SiC structure (N = 1728 atoms). The distances between the graphene and the 6H are 1.0, 1.3 and 1.5 Å and the distances between the graphene layer and the 3C-SiC are 2.0, 2.3, and 2.5 Å. Each system has been equilibrated at room temperature until no further relaxation was observed. The 6H-SiC structure in combination with graphene proves to be more stable compared to the combination with 3C-SiC. This can be seen well in the determined energies. Pair distribution functions were influenced slightly by the graphene layer due to steric and energetic changes. This becomes clear from the small shifts of the C-C distances. Interactions as well as bonds between graphene and SiC lead to the fact that small shoulders of the high-frequency SiC-peaks are visible in the spectra and at the same time the high-frequency peaks of graphene are completely absent.
The cube in cube approach was used by Paul and Ishai-Cohen to model and derive formulas for filler content dependent Young's moduli of particle filled composites assuming perfect filler matrix adhesion. Their formulas were chosen because of their simplicity, and recalculated using an elementary volume approach which transforms spherical inclusions to cubic inclusions. The EV approach led to expression of the composites moduli that allows introducing an adhesion factor kadh ranging from 0 and 1 to take into account reduced filler matrix adhesion. This adhesion factor scales the edge length of the cubic inclusions, thus reducing the stress transfer area between matrix and filler. Fitting the experimental data with the modified Paul model provides reasonable kadh for PA66, PBT, PP, PE-LD and BR which are in line with their surface energies. Further analysis showed that stiffening only occurs if kadh exceeds [Formula: see text] and depends on the ratio of matrix modulus and filler modulus. The modified model allows for a quick calculation of any particle filled composites for known matrix modulus EM, filler modulus EF, filler volume content vF and adhesion factor kadh. Thus, finite element analysis (FEA) simulations of any particle filled polymer parts as well as materials selection are significantly eased. FEA of cubic and hexagonal EV arrangements show that stress distributions within the EV exhibit more shear stresses if one deviates from the cubic arrangement. At high filler contents the assumption that the property of the EV is representative for the whole composite, holds only for filler volume contents up to 15 or 20% (corresponding to 30 to 40 weight %). Thus, for vast majority of commercially available particulate composites, the modified model can be applied. Furthermore, this indicates that the cube in cube approach reaches two limits: (i) the occurrence of increasing shear stresses at filler contents above 20% due to deviations of EV arrangements or spatial filler distribution from cubic arrangements (singular), and (ii) increasing interaction between particles with the formation of particle network within the matrix violating the EV assumption of their homogeneous dispersion.
Approximately 45% of global greenhouse gas emissions are caused by the construction and use of buildings. Thermal insulation of buildings in the current context of climate change is a well-known strategy to improve the energy efficiency of buildings. The development of renewable insulation material can overcome the drawbacks of widely used insulation systems based on polystyrene or mineral wool. This study analyzes the sustainability and thermal conductivity of new insulation materials made of Miscanthus x giganteus fibers, foaming agents, and alkali-activated fly ash binder. Life cycle assessments (LCA) are necessary to perform benchmarking of environmental impacts of new formulations of geopolymer-based insulation materials. The global warming potential (GWP) of the product is primarily determined by the main binder component sodium silicate. Sodium silicate's CO2 emissions depend on local production, transportation, and energy consumption. The results, which have been published during recent years, vary in a wide range from 0.3 kg to 3.3 kg CO2-eq. kg-1. The overall GWP of the insulation system based on Miscanthus fibers, with properties according to current thermal insulation regulations, reaches up to 95% savings of CO2 emissions compared to conventional systems. Carbon neutrality can be achieved through formulations containing raw materials with carbon dioxide emissions and renewable materials with negative GWP, thus balancing CO2 emissions.
Operating an ozone-evolving PEM electrolyser in tap water: A case study of water and ion transport
(2022)
While PEM water electrolysis could be a favourable technique for in situ sanitization with ozone, its application is mainly limited to the use of ultrapure water to achieve a sufficient long-time stability. As additional charge carriers influence the occurring transport phenomena, we investigated the impact of different feed water qualities on the performance of a PEM tap water electrolyser for ozone evolution. The permeation of water and the four most abundant cations (Na+, K+, Ca2+, Mg2+) is characterised during stand-by and powered operation at different charge densities to quantify underlying transport mechanisms. Water transport is shown to linearly increase with the applied current (95 ± 2 mmol A−1 h−1) and occurs decoupled from ion permeation. A limitation of ion permeation is given by the transfer of ions in water to the anode/PEM interface. The unstabilized operation of a PEM electrolyser in tap water leads to a pH gradient which promotes the formation of magnesium and calcium carbonates and hydroxides on the cathode surface. The introduction of a novel auxiliary cathode in the anolytic compartment has shown to suppress ion permeation by close to 20%.
Polymer fibers with liquid crystals (LCs) in the core have potential as autonomous sensors of airborne volatile organic compounds (VOCs), with a high surface-to-volume ratio enabling fast and sensitive response and an attractive non-woven textile form factor. We demonstrate their ability to continuously and quantitatively measure the concentration of toluene, cyclohexane, and isopropanol as representative VOCs, via the impact of each VOC on the LC birefringence. The response is fully reversible and repeatable over several cycles, the response time can be as low as seconds, and high sensitivity is achieved when the operating temperature is near the LC-isotropic transition temperature. We propose that a broad operating temperature range can be realized by combining fibers with different LC mixtures, yielding autonomous VOC sensors suitable for integration in apparel or in furniture that can compete with existing consumer-grade electronic VOC sensors in terms of sensitivity and response speed.
The molecular weight properties of lignins are one of the key elements that need to be analyzed for a successful industrial application of these promising biopolymers. In this study, the use of 1H NMR as well as diffusion-ordered spectroscopy (DOSY NMR), combined with multivariate regression methods, was investigated for the determination of the molecular weight (Mw and Mn) and the polydispersity of organosolv lignins (n = 53, Miscanthus x giganteus, Paulownia tomentosa, and Silphium perfoliatum). The suitability of the models was demonstrated by cross validation (CV) as well as by an independent validation set of samples from different biomass origins (beech wood and wheat straw). CV errors of ca. 7–9 and 14–16% were achieved for all parameters with the models from the 1H NMR spectra and the DOSY NMR data, respectively. The prediction errors for the validation samples were in a similar range for the partial least squares model from the 1H NMR data and for a multiple linear regression using the DOSY NMR data. The results indicate the usefulness of NMR measurements combined with multivariate regression methods as a potential alternative to more time-consuming methods such as gel permeation chromatography.
The promotion of sustainable packaging is part of the European Green Deal and plays a key role in the EU’s social and political strategy. One option is the use of renewable resources and biomass waste as raw materials for polymer production. Lignocellulose biomass from annual and perennial industrial crops and agricultural residues are a major source of polysaccharides, proteins, and lignin and can also be used to obtain plant-based extracts and essential oils. Therefore, these biomasses are considered as potential substitute for fossil-based resources. Here, the status quo of bio-based polymers is discussed and evaluated in terms of properties related to packaging applications such as gas and water vapor permeability as well as mechanical properties. So far, their practical use is still restricted due to lower performance in fundamental packaging functions that directly influence food quality and safety, the length of shelf life, and thus the amount of food waste. Besides bio-based polymers, this review focuses on plant extracts as active packaging agents. Incorporating extracts of herbs, flowers, trees, and their fruits is inevitable to achieve desired material properties that are capable to prolong the food shelf life. Finally, the adoption potential of packaging based on polymers from renewable resources is discussed from a bioeconomy perspective.
New sustainable, environmentally friendly materials for thermal insulation of buildings are necessary to reduce their carbon footprints. In this study, Miscanthus fiber-reinforced geopolymer composites, foamed with sodium dodecyl sulfate (SDS), were developed using fly ash as a geopolymer precursor. The effects of fiber content, fiber size, curing temperature, foaming agent content, fumed silica specific surface area and fumed silica content on thermal conductivity and compressive strength were evaluated using a Plackett-Burman design of experiment. Furthermore, the microstructure of geopolymer composites was investigated using X-ray diffraction (XRD), X-ray micro-computed tomography (μCT) and scanning electron microscopy (SEM). The measured characteristic values were in the following ranges: Thermal conductivity 0.057 W (m K)−1 to 0.127 W (m K)−1, compressive strength 0.007 MPa–0.719 MPa and porosity 49 vol% to 76 vol%. The results reveal an enhancement of thermal conductivity by elevated fiber size and foaming agent content. In contrast, the compressive strength is enhanced by high fiber content. Additionally, SEM images indicate a good interaction between the fibers and the geopolymer matrix, because nearly the whole fiber surface is covered by the geopolymer.
A series of reactive binaphthyl‐diimine‐based dopants is prepared and investigated with respect to their potential for the chiral induction of structural coloration in nematic liquid crystal mixture E7 and the selective photonic sensing of nitrogen dioxide (NO2). Studies of the helical twisting power (HTP) in 4‐cyano‐4′‐pentylbiphenyl (5CB) reveal HTP values as high as 375 µm‐1 and the tremendous impact of structural compatibility and changes of the dihedral binaphthyl angle on the efficiency of the chiral transfer. Detailed investigation of the sensing capabilities of the systems reveals an extraordinarily high selectivity for NO2 and a response to concentrations as low as 100 ppm. The systems show a direct response to the analyte gas leading to a concentration‐dependent shift of the reflectance wavelength of up to several hundred nanometers. Incorporation of copper ions remarkably improves the sensor's properties in terms of sensitivity and selectivity, enabling the tailored tweaking of the system's properties.
The development of sustainable, environmentally friendly insulation materials with a reduced carbon footprint is attracting increased interest. One alternative to conventional insulation materials are foamed geopolymers. Similar to foamed concrete, the mechanical properties of geopolymer foams can also be improved by using fibers for reinforcement. This paper presents an overview of the latest research findings in the field of fiber-reinforced geopolymer foam concrete with special focus on natural fibers reinforcement. Furthermore, some basic and background information of natural fibers and geopolymer foams are reported. In most of the research, foams are produced either through chemical foaming with hydrogen peroxide or aluminum powder, or through mechanical foaming which includes a foaming agent. However, previous reviews have not sufficiently addresses the fabrication of geopolymer foams by syntactic foams. Finally, recent efforts to reduce the fiber degradation in geopolymer concrete are discussed along with challenges for natural fiber reinforced-geopolymer foam concrete.
Optical gas sensors based on chiral-nematic liquid crystals (N* LCs) forming one-dimensional photonic crystals do not require electrical energy and have a considerable potential to supplement established types of sensors. A chiral-nematic phase with tunable selective reflection is induced in a nematic host LC by adding reactive chiral dopants. The selective chemical reaction between dopant and analyte is capable to vary the pitch length (the lattice constant) of the soft, self-assembled, one-dimensional photonic crystal. The progress of the ongoing chemical reaction can be observed even by naked eye because the color of the samples varies. In this work, we encapsulate the responsive N* LC in microscale polyvinylpyrrolidone (PVP) fibers via coaxial electrospinning. The sensor is, thus, given a solid form and has an improved stability against nonavoidable environmental influences. The reaction behavior of encapsulated and nonencapsulated N* LC toward a gaseous analyte is compared, systematically. Making use of the encapsulation is an important step to improve the applicability.
Explorative experiments were done to figure out differences in the emission of volatile organic compounds (VOCs) of not infested trees and trees infested by Anoplophora glabripennis (Asian longhorn beetle, ALB), a quarantine pest. Therefore, VOCs from some native insect species, Anoplophora glabripennis infested Acer, stressed Acer, healthy Acer, Populus and Salix were obtained by enrichment on adsorbents. Qualitative analysis was done by thermal desorption gas chromatography coupled with a mass selective detector (TD-GC/MS). Altogether 169 substances were identified. 11 substances occur from ALB infested or mechanically damaged trees i.e. stressed trees, but not from healthy trees. (+)-Cyclosativene, (+)-α-longipinene, copaene and caryophyllene are detectable only from ALB-infested Acer not from mechanically damaged or healthy Acer. However, these substances are also emitted by healthy Salix. 2,4-Dimethyl-1-heptene is among all tree samples exclusively present in the ambience of ALB-infested trees. It´s rarely detectable from native insect species’ samples.
The choice of suitable semiconducting metal oxide (MOX) gas sensors for the detection of a specific gas or gas mixture is time-consuming since the sensor’s sensitivity needs to be characterized at multiple temperatures to find its optimal operating conditions. To obtain reliable measurement results, it is very important that the power for the sensor’s integrated heater is stable, regulated and error-free (or error-tolerant). Especially the error-free requirement can be only be achieved if the power supply implements failure-avoiding and failure-detection methods. The biggest challenge is deriving multiple different voltages from a common supply in an efficient way while keeping the system as small and lightweight as possible. This work presents a reliable, compact, embedded system that addresses the power supply requirements for fully automated simultaneous sensor characterization for up to 16 sensors at multiple temperatures. The system implements efficient (avg. 83.3% efficiency) voltage conversion with low ripple output (<32 mV) and supports static or temperature-cycled heating modes. Voltage and current of each channel are constantly monitored and regulated to guarantee reliable operation. To evaluate the proposed design, 16 sensors were screened. The results are shown in the experimental part of this work.