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This mature textbook brings the fundamentals of fluid mechanics in a concise and mathematically understandable presentation. In the current edition, a section on dissipation and viscous potential flows has been added. Exercises with solutions help to apply the material correctly and promote understanding.
The cellulase-producing Trichoderma reesei strain RL-P37 exhibits significant potential, yielding 7.3 g/L of cellulase in 241 hours. Microscopic investigations reveal a link between spore formation and enzyme production, suggesting the need for research into the intricate relationship between enzyme production, stress responses, and the nutritional prerequisites of fungi. Comparatively, the use of sodium hydroxide (NaOH) treatment, as opposed to water treatment, results in the reduction of micronutrient content and carbon source extraction as filtrate. Despite these challenges, research by He et al. (2021) highlights NaOH's efficiency in cellulose extraction from plant-based sources. Using NaOH pretreatment can be proven as effective by designing a proper cultivation method. The selection of inducers for enzyme induction gains importance, with soluble inducers, as emphasized by Zhang et al. (2022), exhibiting superior effectiveness. Hence, adopting soluble inducers in designing cultivation methods for improved enzyme production in shaking flasks is recommended. Enzymatic treatment of bio-waste, as outlined by Hu et al. (2021), shows promise in augmenting essential component content by breaking down plant cell walls and intercellular compartments. However, the feasibility of using an artificial bio-waste medium for cultivating Trichoderma reesei is questioned. Investigating the impact of micronutrient levels, particularly the inhibitory role of zinc, on fungal growth becomes essential. These findings underscore the necessity for ongoing research and optimization in cellulase production, emphasizing both strain productivity and cultivation methodologies.
In this paper a practical way for fatigue life prediction of rubber products under multiaxial loads is shown. This is done by means of fracture mechanical concepts and the energy release rate as the failure criterion. Due to a FEA post-processor the potential energy release rate might be calculated at every material point supposed there was a crack. And therefore the risk of failure and with the help of a strain number curve the time to fatigue is able to be calculated by FEA. This concept is applied for an estimation of the life time of a test specimen with tensile loading from fatigue data of a shear loaded specimen of different design. This rather more theoretical concept of the energy release rate is complemented by experimental crack growth data by a Tear Fatigue Analyzer with its great advantage of reduction of testing time and costs compared to those of fatigue tests. For some materials a thorough characterization of crack growth and fatigue behavior is presented and is applied to estimate the time to fatigue by FEA for a real component under multiaxial loads.
There are additional long-term effects which also change the micro-structure of the polymer network and consequently the effective number of polymer chains in the material. These effects are summarized by ageing processes and will be used in the following to explain the basic assumptions of the model which can be generalized to simulate the viscous behaviour of the material. An implementation of these concepts into FEM codes is straightforward and has been carried out to the solver ABAQUS, Baaser & Ziegler (2006), Baaser et al. (2009).
Biological in situ methanation: Gassing concept and feeding strategy for enhanced performance
(2017)
The expansion of fluctuating renewable electricity production from wind and solar energy requires huge storage capacities. Power-to-gas (PtG) can contribute to tackle that issue via a two-step process, the electrolytic production of hydrogen and a subsequent methanation step (with additional CO2). The resulting fully grid compatible methane, also known as synthetic natural gas (SNG), can be both stored and transported in the vast existing natural gas infrastructure.
To overcome current major drawbacks of PtG, the relatively low efficiency and the high costs, we developed an improved method for the methanation step. In our approach we use a further development of the biological in situ methanation of hydrogen in biogas plants. Because this strategy uses directly internal residual CO2 from the biogas process in the biogas plant, you neither need additional external CO2 nor special reactors. Thus, PtG is combined with the production of an upgraded highly methane rich raw biogas.
However, the low solubility of hydrogen in aqueous solutions and the exploitation of the maximum biological production rates are still an engineering challenge for high performance biological in situ methanation.
In our experiments a setup with membrane gassing turned out to be most promising to ensure a sufficient gas liquid mass transfer of the hydrogen. The monitoring of hydrogenotrophic and aceticlastic archaea showed some adaption of these microbial subgroups to the hydrogen feed.
In order to achieve high methane concentrations of more than 90 % in the raw biogas a CO2-controlled hydrogen feed flow rate is suggested. For methane concentrations lower than 90 % simple current controlled hydrogen supply can be applied.
A system for the on-line/in-line measurement of soot particle sizes and concentrations in the undiluted exhaust gas of diesel engines was developed and successfully tested. The unit uses the individual attenuations of three different laser wavelengths and is combined with an optical cell (white principle) with adjustable path lengths from 2.5 to 15 meters.
Time Resolved Measurements of Soot Concentrations and Mean Particle Sizes during EUDC and ECE Cycles
(2002)
Hybrid drives for automotive application are extensively discussed. In contrast, the company HEINZMANN, the University of Karlsruhe and the University of Applied Sciences Offenburg concentrate on hybrid drives for industrial, offroad purposes in a joint project. These applications promise a much higher fuel saving potential, particularly if highly frequent load cycles are present. Hybrid drive systems offer additional advantages including reduced exhaust aftertreatment requirements due to engine downsizing, better engine dynamics, emissions and noise reduction.
The significant market growth of stationary electrical energy storage systems both for private and commercial applications has raised the question of battery lifetime under practical operation conditions. Here, we present a study of two 8 kWh lithium-ion battery (LIB) systems, each equipped with 14 lithium iron phosphate/graphite (LFP) single cells in different cell configurations. One system was based on a standard configuration with cells connected in series, including a cell-balancing system and a 48 V inverter. The other system featured a novel configuration of two stacks with a parallel connection of seven cells each, no cell-balancing system, and a 4 V inverter. The two systems were operated as part of a microgrid both in continuous cycling mode between 30% and 100% state of charge, and in solar-storage mode with day–night cycling. The aging characteristics in terms of capacity loss and internal resistance change in the cells were determined by disassembling the systems for regular checkups and characterizing the individual cells under well-defined laboratory conditions. As a main result, the two systems showed cell-averaged capacity losses of 18.6% and 21.4% for the serial and parallel configurations, respectively, after 2.5 years of operation with 810 (serial operation) and 881 (parallel operation) cumulated equivalent full cycles. This is significantly higher than the aging of a reference single cell cycled under laboratory conditions at 20 °C, which showed a capacity loss of only 10% after 1000 continuous full cycles.
This article presents a comparative experimental study of the electrical, structural and chemical properties of large‐format, 180 Ah prismatic lithium iron phosphate (LFP)/graphite lithium‐ion battery cells from two different manufacturers. These cells are particularly used in the field of stationary energy storage such as home‐storage systems. The investigations include (1) cell‐to‐cell performance assessment, for which a total of 28 cells was tested from each manufacturer, (2) electrical charge/discharge characteristics at different currents and ambient temperatures, (3) internal cell geometries, components, and weight analysis after cell opening, (4) microstructural analysis of the electrodes via light microscopy and scanning electron microscopy, (5) chemical analysis of the electrode materials using energy‐dispersive X‐ray spectroscopy, and (6) mathematical analysis of the electrode balances. The combined results give a detailed and comparative insight into the cell characteristics, providing essential information needed for system integration. The study also provides complete and self‐consistent parameter sets for the use in cells models needed for performance prediction or state diagnosis.
Increasing global energy demand and the need to transition to sustainable energy sources to mitigate climate change, highlights the need for innovative approaches to improve the resilience and sustainability of power grids. This study focuses on addressing these challenges in the context of Morocco's evolving energy landscape, where increasing energy demand and efforts to integrate renewable energy require grid reinforcement strategies. Using renewable energy sources such as photovoltaic systems and energy storage technologies, this study aims to develop a methodology for strengthening rural community grids in Morocco.
Traditional reinforcement measures such as line and transformer upgrades will be investigated as well as the integration of power generation from photovoltaic systems, which offer a promising way to utilise Morocco's abundant solar resources. In addition, energy storage systems will be analysed as potential solutions to the challenges of grid stability and resilience. Using comprehensive data analysis, scenario planning and simulation methods with the open-source simulation software Panda Power, this study aims to assess the impact of different grid reinforcement measures, including conventional methods, photovoltaic integration, and the use of energy storage, on grid performance and sustainability. The results of this study provide valuable insights into the challenges and opportunities of transitioning to a more resilient and sustainable energy future in Morocco.
Based on a rural medium-voltage grid in Souihla, Morocco, three scenarios were carried out to assess the impact of demand growth in 2030 and 2040. The first scenario focuses on conventional grid reinforcement measures, while the second scenario incorporates energy from residential photovoltaic systems. The third scenario analyses the integration of storage systems and their impact on grid reinforcement in 2030.
The simulations with energy from photovoltaic systems show a reduction in grid reinforcement measures compared to the scenario without solar energy. In addition, the introduction of a storage system in 2030 led to a significant reduction in the required installed transformer capacity and fewer congested lines. Furthermore, the results emphasized the role of storage in stabilizing grid voltage levels.
In summary, the results highlighted the potential benefits of integrating energy from photovoltaics and storage into the grid. This integration not only reduces the need for transformers and overall grid infrastructure but also promotes a more efficient and sustainable energy system.
We present a two-dimensional (2D) planar chromatographic separation of estrogenic active compounds on RP-18 W (Merck, 1.14296) phase. A mixture of 8 substances was separated using a solvent mix consisting of hexane, ethyl acetate, acetone (55:15:10, v/v) in the first direction and of acetone and water (15:10, v/v) in the second direction. Separation was performed on an RP-18 W plate over a distance of 70 mm. This 2D-separation method can be used to quantify 17α-ethinylestradiol (EE2) in an effect-directed analysis, using the yeast strain Saccharomyces cerevisiae BJ3505. The test strain (according to McDonnell) contains the estrogen receptor. Its activation by estrogen active compounds is measured by inducing the reporter gene lacZ which encodes the enzyme β-galactosidase. This enzyme activity is determined on plate by using the fluorescent substrate MUG (4-methylumbelliferyl-β-d-galactopyranoside).
Footwear plays a critical role in our daily lives, affecting our performance, health and overall well-being. Well-designed footwear can provide protection, comfort and improved foot functionality, while poorly designed footwear can lead to mobility problems and declines in physical activity. The overall goal of footwear research is to provide a scientific basis for professionals in the field to provide an optimal footwear solution for a given person, for a given task, in a given environment, while using sustainable manufacturing processes. This article suggests potential directions for future research with a focus on athletic footwear biomechanics. Directions include the evidence-based individualisation of footwear, the interaction between design and prolonged use, and improving the sustainability of footwear. The authors also provide a speculative outlook on methodological developments that may provide greater insight into these areas. These developments may include: (1) the use of larger scale, real-world and representative data, (2) the use of 3D printing to create experimental footwear, (3) the advancement of in silico research methods, and (4) furthering multidisciplinary collaboration. If successfully applied in the future, footwear research will contribute to active and healthy lifestyles across the lifespan.
Treadmills are essential to the study of human and animal locomotion as well as for applied diagnostics in both sports and medicine. The quantification of relevant biomechanical and physiological variables requires a precise regulation of treadmill belt velocity (TBV). Here, we present a novel method for time-efficient tracking of TBV using standard 3D motion capture technology. Further, we analyzed TBV fluctuations of four different treadmills as seven participants walked and ran at target speeds ranging from 1.0 to 4.5 m/s. Using the novel method, we show that TBV regulation differs between treadmill types, and that certain features of TBV regulation are affected by the subjects’ body mass and their locomotion speed. With higher body mass, the TBV reductions in the braking phase of stance became higher, even though this relationship differed between locomotion speeds and treadmill type (significant body mass × speed × treadmill type interaction). Average belt speeds varied between about 98 and 103% of the target speed. For three of the four treadmills, TBV reduction during the stance phase of running was more intense (> 5% target speed) and occurred earlier (before 50% of stance phase) unlike the typical overground center of mass velocity patterns reported in the literature. Overall, the results of this study emphasize the importance of monitoring TBV during locomotor research and applied diagnostics. We provide a novel method that is freely accessible on Matlab’s file exchange server (“getBeltVelocity.m”) allowing TBV tracking to become standard practice in locomotion research.
High-tech running shoes and spikes ("super-footwear") are currently being debated in sports. There is direct evidence that distance running super shoes improve running economy; however, it is not well established to which extent world-class performances are affected over the range of track and road running events.
This study examined publicly available performance datasets of annual best track and road performances for evidence of potential systematic performance effects following the introduction of super footwear. The analysis was based on the 100 best performances per year for men and women in outdoor events from 2010 to 2022, provided by the world governing body of athletics (World Athletics).
We found evidence of progressing improvements in track and road running performances after the introduction of super distance running shoes in 2016 and super spike technology in 2019. This evidence is more pronounced for distances longer than 1500 m in women and longer than 5000 m in men. Women seem to benefit more from super footwear in distance running events than men.
While the observational study design limits causal inference, this study provides a database on potential systematic performance effects following the introduction of super shoes/spikes in track and road running events in world-class athletes. Further research is needed to examine the underlying mechanisms and, in particular, potential sex differences in the performance effects of super footwear.
Background: Running overuse injuries (ROIs) occur within a complex, partly injury-specific interplay between training loads and extrinsic and intrinsic risk factors. Biomechanical risk factors (BRFs) are related to the individual running style. While BRFs have been reviewed regarding general ROI risk, no systematic review has addressed BRFs for specific ROIs using a standardized methodology.
Objective: To identify and evaluate the evidence for the most relevant BRFs for ROIs determined during running and to
suggest future research directions.
Design: Systematic review considering prospective and retrospective studies. (PROSPERO_ID: 236,832).
Data Sources: PubMed. Connected Papers. The search was performed in February 2021.
Eligibility Criteria: English language. Studies on participants whose primary sport is running addressing the risk for the seven most common ROIs and at least one kinematic, kinetic (including pressure measurements), or electromyographic BRF. A BRF needed to be identified in at least one prospective or two independent retrospective studies. BRFs needed to be determined during running.
Results: Sixty-six articles fulfilled our eligibility criteria. Levels of evidence for specific ROIs ranged from conflicting to moderate evidence. Running populations and methods applied varied considerably between studies. While some BRFs appeared for several ROIs, most BRFs were specific for a particular ROI. Most BRFs derived from lower-extremity joint kinematics and kinetics were located in the frontal and transverse planes of motion. Further, plantar pressure, vertical ground reaction force loading rate and free moment-related parameters were identified as kinetic BRFs.
Conclusion: This study offers a comprehensive overview of BRFs for the most common ROIs, which might serve as a starting point to develop ROI-specific risk profiles of individual runners. We identified limited evidence for most ROI-specific risk factors, highlighting the need for performing further high-quality studies in the future. However, consensus on data collection standards (including the quantification of workload and stress tolerance variables and the reporting of injuries) is warranted.
Objective: To identify and evaluate the evidence of the most relevant running-related risk factors (RRRFs) for running-related overuse injuries (ROIs) and to suggest future research directions.
Design: Systematic review considering prospective and retrospective studies. (PROSPERO_ID: 236832)
Data sources: Pubmed. Connected Papers. The search was performed in February 2021.
Eligibility criteria: English language. Studies on participants whose primary sport is running addressing the risk for the seven most common ROIs and at least one kinematic, kinetic (including pressure measurements), or electromyographic RRRF. An RRRF needed to be identified in at least one prospective or two retrospective studies.
Results: Sixty-two articles fulfilled our eligibility criteria. Levels of evidence for specific ROIs ranged from conflicting to moderate evidence. Running populations and methods applied varied considerably between studies. While some RRRFs appeared for several ROIs, most RRRFs were specific for a particular ROI. The biomechanical measurements performed in many studies would have allowed for consideration of many more RRRFs than have been reported, highlighting a potential for more effective data usage in the future.
Conclusion: This study offers a comprehensive overview of RRRFs for the most common ROIs, which might serve as a starting point to develop ROI-specific risk profiles of individual runners. Future work should use macroscopic (big data) approaches involving long-term data collections in the real world and microscopic approaches involving precise stress calculations using recent developments in biomechanical modelling. However, consensus on data collection standards (including the quantification of workload and stress tolerance variables and the reporting of injuries) is warranted.
The purpose of this study was to describe the effects of running speed and slope on metatarsophalangeal (MTP) joint kinematics. 22 male and female runners underwent 3D motion analysis on an instrumented treadmill at three different speeds (2.5 m/s, 3.0 m/s, 3.5 m/s). At each speed, participants ran at seven slope conditions (downhill: -15%, -10%, -5%, level, and uphill: +5%, +10%, +15%). We found a significant main effect (p < 0.001) of running speed and slope on peak MTP dorsiflexion and a running speed by slope interaction effect (p < 0.001) for peak MTP dorsiflexion velocity. These findings highlight the need to consider running intensity and environmental factors like running surface inclination when considering MTP joint mechanics and technological aids to support runners.
Background: Many countries have restricted public life in order to contain the spread of the novel coronavirus (SARS-CoV2). As a side effect of related measures, physical activity (PA) levels may have decreased.
Objective: We aimed (1) to quantify changes in PA and (2) to identify variables potentially predicting PA reductions.
Methods: A systematic review with random-effects multilevel meta-analysis was performed, pooling the standardized mean differences in PA measures before and during public life restrictions.
Results: A total of 173 trials with moderate methodological quality (modified Downs and Black checklist) were identified. Compared to pre-pandemic, total PA (SMD − 0.65, 95% CI − 1.10 to − 0.21) and walking (SMD − 0.52, 95% CI − 0.29 to − 0.76) decreased while sedentary behavior increased (SMD 0.91, 95% CI: 0.17 to 1.65). Reductions in PA affected all intensities (light: SMD − 0.35, 95% CI − 0.09 to − 0.61, p = .013; moderate: SMD − 0.33, 95% CI − 0.02 to − 0.6; vigorous: SMD − 0.33, − 0.08 to − 0.58, 95% CI − 0.08 to − 0.58) to a similar degree. Moderator analyses revealed no influence of variables such as sex, age, body mass index, or health status. However, the only continent without a PA reduction was Australia and cross-sectional trials yielded higher effect sizes (p < .05).
Conclusion: Public life restrictions associated with the COVID-19 pandemic resulted in moderate reductions in PA levels and large increases in sedentary behavior. Health professionals and policy makers should therefore join forces to develop strategies counteracting the adverse effects of inactivity.
Governments have restricted public life during the COVID-19 pandemic, inter alia closing sports facilities and gyms. As regular exercise is essential for health, this study examined the effect of pandemic-related confinements on physical activity (PA) levels. A multinational survey was performed in 14 countries. Times spent in moderate-to-vigorous physical activity (MVPA) as well as in vigorous physical activity only (VPA) were assessed using the Nordic Physical Activity Questionnaire (short form). Data were obtained for leisure and occupational PA pre- and during restrictions. Compliance with PA guidelines was calculated based on the recommendations of the World Health Organization (WHO). In total, n = 13,503 respondents (39 ± 15 years, 59% females) were surveyed. Compared to pre-restrictions, overall self-reported PA declined by 41% (MVPA) and 42.2% (VPA). Reductions were higher for occupational vs. leisure time, young and old vs. middle-aged persons, previously more active vs. less active individuals, but similar between men and women. Compared to pre-pandemic, compliance with WHO guidelines decreased from 80.9% (95% CI: 80.3–81.7) to 62.5% (95% CI: 61.6–63.3). Results suggest PA levels have substantially decreased globally during the COVID-19 pandemic. Key stakeholders should consider strategies to mitigate loss in PA in order to preserve health during the pandemic.
Do you know that for each banana bunch the complete plant must be cut as well? Only in Brazil 440 million trees are planted annually. With an average weight of 30 kg per banana plant you can estimate about 13,5 million tons of banana residues per year. Although there exist some projects to use these residues for the production of valuable products (e.g fibers for textile and paper production) most of this organic waste material is unused and left for composting on the farmland.
The basic idea of this project is to evaluate this organic waste material for converting it to a renewable and CO2 neutral fuel. Therefore, the different parts of the banana plant (heart, leaves and pseudo stem) were analyzed regarding their biogas potential (specific biogas yield and biogas production kinetics). In further studies the effect of mechanical and enzymatic pretreatments of the different parts of the plants was investigated. This examination could then be the basis for an energetic usage of this organic residue.
The biogas batch experiments were performed according to the german guideline VDI 4630 in 2-L-Batch reactors at 37°C. As biogas substrates, the heart, the leaves and the pseudo stem of the banana plant residue with and without enzymatic/mechanical pretreatment were used.
The different parts of the banana plants result in a specific biogas production yield in the range of 260-470 norm liters per kg organic dry mass.
To determine the influence of the mechanical pretreatment (particle size 1-15 mm) on the biogas production kinetics, the kinetic constants were defined and calculated. The reduction of the particle size leads to an improved biogas production kinetics. Therefore experiments will demonstrate, if the results from the batch experiments can be converted in the continuous fed biogas reactor. The experiments of the enzymatic pretreatment are still under investigation.
The compliant nature of distal limb muscle-tendon units is traditionally considered suboptimal in explosive movements when positive joint work is required. However, during accelerative running, ankle joint net mechanical work is positive. Therefore, this study aims to investigate how plantar flexor muscle-tendon behavior is modulated during fast accelerations. Eleven female sprinters performed maximum sprint accelerations from starting blocks, while gastrocnemius muscle fascicle lengths were estimated using ultrasonography. We combined motion analysis and ground reaction force measurements to assess lower limb joint kinematics and kinetics, and to estimate gastrocnemius muscle-tendon unit length during the first two acceleration steps. Outcome variables were resampled to the stance phase and averaged across three to five trials. Relevant scalars were extracted and analyzed using one-sample and two-sample t-tests, and vector trajectories were compared using statistical parametric mapping. We found that an uncoupling of muscle fascicle behavior from muscle-tendon unit behavior is effectively used to produce net positive mechanical work at the joint during maximum sprint acceleration. Muscle fascicles shortened throughout the first and second steps, while shortening occurred earlier during the first step, where negative joint work was lower compared with the second step. Elastic strain energy may be stored during dorsiflexion after touchdown since fascicles did not lengthen at the same time to dissipate energy. Thus, net positive work generation is accommodated by the reuse of elastic strain energy along with positive gastrocnemius fascicle work. Our results show a mechanism of how muscles with high in-series compliance can contribute to net positive joint work.
Immunosorbent turnip vein clearing virus (TVCV) particles displaying the IgG-binding domains D and E of Staphylococcus aureus protein A (PA) on every coat protein (CP) subunit (TVCVPA) were purified from plants via optimized and new protocols. The latter used polyethylene glycol (PEG) raw precipitates, from which virions were selectively re-solubilized in reverse PEG concentration gradients. This procedure improved the integrity of both TVCVPA and the wild-type subgroup 3 tobamovirus. TVCVPA could be loaded with more than 500 IgGs per virion, which mediated the immunocapture of fluorescent dyes, GFP, and active enzymes. Bi-enzyme ensembles of cooperating glucose oxidase and horseradish peroxidase were tethered together on the TVCVPA carriers via a single antibody type, with one enzyme conjugated chemically to its Fc region, and the other one bound as a target, yielding synthetic multi-enzyme complexes. In microtiter plates, the TVCVPA-displayed sugar-sensing system possessed a considerably increased reusability upon repeated testing, compared to the IgG-bound enzyme pair in the absence of the virus. A high coverage of the viral adapters was also achieved on Ta2O5 sensor chip surfaces coated with a polyelectrolyte interlayer, as a prerequisite for durable TVCVPA-assisted electrochemical biosensing via modularly IgG-assembled sensor enzymes.
Battery degradation is a complex physicochemical process that strongly depends on operating conditions. We present a model-based analysis of lithium-ion battery degradation in a stationary photovoltaic battery system. We use a multi-scale multi-physics model of a graphite/lithium iron phosphate (LiFePO4, LFP) cell including solid electrolyte interphase (SEI) formation. The cell-level model is dynamically coupled to a system-level model consisting of photovoltaics (PV), inverter, load, grid interaction, and energy management system, fed with historic weather data. Simulations are carried out for two load scenarios, a single-family house and an office tract, over annual operation cycles with one-minute time resolution. As key result, we show that the charging process causes a peak in degradation rate due to electrochemical charge overpotentials. The main drivers for cell ageing are therefore not only a high state of charge (SOC), but the charging process leading towards high SOC. We also show that the load situation not only influences system parameters like self-sufficiency and self-consumption, but also has a significant impact on battery ageing. We assess reduced charge cut-off voltage as ageing mitigation strategy.
The efficiency of a chromatographic analytical method is determined by the selectivity of the chromatographic separation and the specificity of the detection method. In high-performance thin-layer chromatography (HPTLC) the separated components can be detected and quantified directly on the plate by physical and chemical methods. By coupling high-performance thin-layer chromatography with biological or biochemical inhibition tests it is possible to detect toxic substances in situ.
Introduction: The use of scaffolds in tissue engineering is becoming increasingly important as solutions need to be found to preserve human tissues such as bone or cartilage. Various factors, including cells, biomaterials, cell and tissue culture conditions, play a crucial role in tissue engineering. The in vivo environment of the cells exerts complex stimuli on the cells, thereby directly influencing cell behavior, including proliferation and differentiation. Therefore, to create suitable replacement or regeneration procedures for human tissues, the conditions of the cells’ natural environment should be well mimicked. Therefore, current research is trying to develop 3-dimensional scaffolds (scaffolds) that can elicit appropriate cellular responses and thus help the body regenerate or replace tissues. In this work, scaffolds were printed from the biomaterial polycaprolactone (PCL) on a 3D bioplotter. Biocompatibility testing was used to determine whether the printed scaffolds were suitable for use in tissue engineering.
Material and Methods: An Envisiontec 3D bioplotter was used to fabricate the scaffolds. For better cell-scaffold interaction, the printed polycaprolactone scaffolds were coated with type-I collagen. Three different cell types were then cultured on the scaffolds and various tests were used to investigate the biocompatibility of the scaffolds.
Results: Reproducible scaffolds could be printed from polycaprolactone. In addition, a coating process with collagen was developed, which significantly improved the cell-scaffold interaction. Biocompatibility tests showed that the PCL-collagen scaffolds are suitable for use with cells. The cells adhered to the surface of the scaffolds and as a result extensive cell growth was observed on the scaffolds. The inner part of the scaffolds, however, remained largely uninhabited. In the cytotoxicity studies, it was found that toxicity below 20% was present in some experimental runs. The determination of the compressive strength by means of the universal testing machine Z005 by ZWICK according to DIN EN ISO 604 of the scaffolds resulted in a value of 68.49 ± 0.47 MPa.
Power systems are increasingly built from distributed generation units and smart consumers that are able to react to grid conditions. Managing this large number of decentralized electricity sources and flexible loads represent a very huge optimization problem. Both from the regulatory and the computational perspective, no one central coordinator can optimize this overall system. Decentralized control mechanisms can, however, distribute the optimization task through price signals or market-based mechanisms. This chapter presents the concepts that enable a decentralized control of demand and supply while enhancing overall efficiency of the electricity system. It highlights both technological and business challenges that result from the realization of these concepts, and presents the state-of-the-art in the respective domains.
Short-term load forecasting (STLF) has been playing a key role in the electricity sector for several decades, due to the need for aligning energy generation with the demand and the financial risk connected with forecasting errors. Following the top-down approach, forecasts are calculated for aggregated load profiles, meaning the sum of singular loads from consumers belonging to a balancing group. Due to the emerging flexible loads, there is an increasing relevance for STLF of individual factories. These load profiles are typically more stochastic compared to aggregated ones, which imposes new requirements to forecasting methods and tools with a bottom-up approach. The increasing digitalization in industry with enhanced data availability as well as smart metering are enablers for improved load forecasts. There is a need for STLF tools processing live data with a high temporal resolution in the minute range. Furthermore, behin-the-meter (BTM) data from various sources like submetering and production planning data should be integrated in the models. In this case, STLF is becoming a big data problem so that machine learning (ML) methods are required. The research project “GaIN” investigates the improvement of the STLF quality of an energy utility using BTM data and innovative ML models. This paper describes the project scope, proposes a detailed definition for a benchmark and evaluates the readiness of existing STLF methods to fulfil the described requirements as a reviewing paper.
The review highlights that recent STLF investigations focus on ML methods. Especially hybrid models gain more and more importance. ML can outperform classical methods in terms of automation degree and forecasting accuracy. Nevertheless, the potential for improving forecasting accuracy by the use of ML models depends on the underlying data and the types of input variables. The described methods in the analyzed publications only partially fulfil the tool requirements for STLF on company level. There is still a need to develop suitable ML methods to integrate the expanded data base in order to improve load forecasts on company level.
Colored glass products with various printing technologies are becoming more important in industry. The aim is to achieve individual solution in a very short delivery time. Conventional thermal treatment of burning glasses in oven for tempered color printing has predominant issues with high time consumption, energy consumption and manufacturing cost. It requires alternative process development.
This paper proposes laser process to overcome issues in conventional treatment with the latest results of tempering colored glass. Samples have been analyzed with the scanning electron microscope (SEM). Two different laser systems have been applied and the glass has been printed with black paste.
Combined heat and power production (CHP) based on solid oxide fuel cells (SOFC) is a very promising technology to achieve high electrical efficiency to cover power demand by decentralized production. This paper presents a dynamic quasi 2D model of an SOFC system which consists of stack and balance of plant and includes thermal coupling between the single components. The model is implemented in Modelica® and validated with experimental data for the stack UI-characteristic and the thermal behavior. The good agreement between experimental and simulation results demonstrates the validity of the model. Different operating conditions and system configurations are tested, increasing the net electrical efficiency to 57% by implementing an anode offgas recycle rate of 65%. A sensitivity analysis of characteristic values of the system like fuel utilization, oxygen-to-carbon ratio and electrical efficiency for different natural gas compositions is carried out. The result shows that a control strategy adapted to variable natural gas composition and its energy content should be developed in order to optimize the operation of the system.
HiSiMo cast irons are frequently used as material for high temperature components in engines as e.g. exhaust manifolds and turbo chargers. These components must withstand severe cyclic mechanical and thermal loads throughout their service life. The combination of thermal transients with mechanical load cycles results in a complex evolution of damage, leading to thermomechanical fatigue (TMF) of the material and, after a certain number of loading cycles, to failure of the component. In this paper (Part I), the low-cycle fatigue (LCF) and TMF properties of HiSiMo are investigated in uniaxial tests and the damage mechanisms are addressed. On the basis of the experimental results a fatigue life model is developed which is based on elastic, plastic and creep fracture mechanics results of short cracks, so that time and temperature dependent effects on damage are taken into account. The model can be used to estimate the fatigue life of components by means of finite-element calculations (Part II of the paper).
Optimization of energetic refurbishment roadmaps for multi-family buildings utilizing heat pumps
(2023)
A novel methodology for calculating optimized refurbishment roadmaps is developed in this paper. The aim of the roadmaps is to determine when and how should which component of the building envelope and heat generation system be refurbished to achieve the lowest net present value. The integrated optimization approach couples a particle swarm optimization algorithm with a dynamic building simulation of the building envelope and the heat supply system. Due to a free selection of implementation times and refurbishment depth, the optimization method achieves the lowest net present value and high CO2 reduction and is therefore an important contribution to achieve climate neutrality in the building stock.
The method is exemplarily applied to a multi-family house built in 1970. In comparison to a standard refurbishment roadmap, cost savings of 6–16 % and CO2 savings of 6–59 % are possible. The sensitivity of the refurbishment roadmap measures is analyzed on the basis of a parametric analysis. Robust optimization results are obtained with a mean refurbishment level of approx. 50 kWh/m2/a of the building envelope. The preferred heat generation system is a bivalent brine-heat pump system with a share of 70 % of the heat load being covered by the electric heat pump.
Predictive control has great potential in the home energy management domain. However, such controls need reliable predictions of the system dynamics as well as energy consumption and generation, and the actual implementation in the real system is associated with many challenges. This paper presents the implementation of predictive controls for a heat pump with thermal storage in a real single-family house with a photovoltaic rooftop system. The predictive controls make use of a novel cloud camera-based short-term solar energy prediction and an intraday prediction system that includes additional data sources. In addition, machine learning methods were used to model the dynamics of the heating system and predict loads using extensive measured data. The results of the real and simulated operation will be presented.
During the coronavirus crisis, labs had to be offered in digital form in mechanical engineering at short notice. For this purpose, digital twins of more complex test benches in the field of fluid energy machines were used in the mechanical engineering course, with which the students were able to interact remotely to obtain measurement data. The concept of the respective lab was revised with regard to its implementation as a remote laboratory. Fortunately, real-world labs were able to be fully replaced by remote labs. Student perceptions of remote labs were mostly positive. This paper explains the concept and design of the digital twins and the lab as well as the layout, procedure, and finally the results of the accompanying evaluation. However, the implementation of the digital twins to date does not yet include features which address the tactile experience of working in real-world labs.
Crystal structures of two metal–organic frameworks (MFU‐1 and MFU‐2) are presented, both of which contain redox‐active CoII centres coordinated by linear 1,4‐bis[(3,5‐dimethyl)pyrazol‐4‐yl] ligands. In contrast to many MOFs reported previously, these compounds show excellent stability against hydrolytic decomposition. Catalytic turnover is achieved in oxidation reactions by employing tert‐butyl hydroperoxide and the solid catalysts are easily recovered from the reaction mixture. Whereas heterogeneous catalysis is unambiguously demonstrated for MFU‐1, MFU‐2 shows catalytic activity due to slow metal leaching, emphasising the need for a deeper understanding of structure–reactivity relationships in the future design of redox‐active metal–organic frameworks. Mechanistic details for oxidation reactions employing tert‐butyl hydroperoxide are studied by UV/Vis and IR spectroscopy and XRPD measurements. The catalytic process accompanying changes of redox states and structural changes were investigated by means of cobalt K‐edge X‐ray absorption spectroscopy. To probe the putative binding modes of molecular oxygen, the isosteric heats of adsorption of O2 were determined and compared with models from DFT calculations. The stabilities of the frameworks in an oxygen atmosphere as a reactive gas were examined by temperature‐programmed oxidation (TPO). Solution impregnation of MFU‐1 with a co‐catalyst (N‐hydroxyphthalimide) led to NHPI@MFU‐1, which oxidised a range of organic substrates under ambient conditions by employing molecular oxygen from air. The catalytic reaction involved a biomimetic reaction cascade based on free radicals. The concept of an entatic state of the cobalt centres is proposed and its relevance for sustained catalytic activity is briefly discussed.
Silicon (Si) has turned out to be a promising active material for next‐generation lithium‐ion battery anodes. Nevertheless, the issues known from Si as electrode material (pulverization effects, volume change etc.) are impeding the development of Si anodes to reach market maturity. In this study, we are investigating a possible application of Si anodes in low‐power printed electronic applications. Tailored Si inks are produced and the impact of carbon coating on the printability and their electrochemical behavior as printed Si anodes is investigated. The printed Si anodes contain active material loadings that are practical for powering printed electronic devices, like electrolyte gated transistors, and are able to show high capacity retentions. A capacity of 1754 mAh/gSi is achieved for a printed Si anode after 100 cycles. Additionally, the direct applicability of the printed Si anodes is shown by successfully powering an ink‐jet printed transistor.
The use of a TLC scanner can be regarded as a key step in high performance thin layer chromatography (HPTLC). Densitometric measurements transform the substance distribution on a TLC plate into digital computer data. Systems that allow quantitative measurements have been available for many years for either fluorescence or ultraviolet absorption measurements, while lately the reflection analysis mode for both types is the most common application. New scanning approaches are designed to aid the analyst who has common demands for TLC-densitometry without using special data, such as scanned images. Two examples that have been developed lately in the laboratories of the authors are described in this paper. These approaches were developed on the basis of current needs for analysts who employ TLC as a tool in research, as well as in routine analysis. One approach is aimed to support analysts in economically disadvantaged areas, where cost intensive apparatus is unsuitable but trace analysis by simple means is required. The other system, allows the spectral determination of chromatographic spots on TLC plates covering the ultraviolet and visible range, thus, revealing highly desired information for the analyst.
An interlaboratory comparison was carried out to evaluate the effectiveness of a method based on HPTLC in which reagent-free derivatization is followed by UV/fluorescence detection. The method was tested for the determination of sucralose (C12H19C13O8; (2R,3R,4R,5S,6R)-2-[(2R,3S,4S,5S)-2,5-bis(chloromethyl)-3,4-dihydroxyoxolan-2-yl]oxy-5-chloro-6-hydroxymethyl)oxane-3, 4-diol; CAS Registry No. 56038-13-2) in carbonated and still beverages at the proposed European regulatory limits. For still beverages, a portion of the sample was diluted with methanol-water. For carbonated beverages, a portion of the sample was degassed in an ultrasonic bath before dilution. Turbid beverages were filtered after dilution through an HPLC syringe filter. The separation of sucralose was performed by direct application on amino-bonded (NH2) silica gel HPTLC plates (no cleanup needed) with the mobile phase acetonitrile-water. Sucralose was determined after reagent-free derivatization at 190 degrees C; it was quantified by measurements of both UV absorption and fluorescence. The samples, both spiked and containing sucralose, were sent to 14 laboratories in five different countries. Test portions of a sample found to contain no sucralose were spiked at levels of 30.5, 100.7, and 299 mg/L. Recoveries ranged from 104.3 to 124.6% and averaged 112% for determination by UV detection; recoveries ranged from 98.4 to 101.3% and averaged 99.9% for determination by fluorescence detection. On the basis of the results for spiked samples (blind duplicates at three levels), as well as sucralose-containing samples (blind duplicates at three levels and one split level), the values for the RSDr ranged from 10.3 to 31.4% for determinations by UV detection and from 8.9 to 15.9% for determinations by fluorescence detection. The values for the RSDR values ranged from 13.5 to 31.4% for determinations by UV detection and from 8.9 to 20.7% for determinations by fluorescence detection.
The production of potable water in dry areas nowadays is mainly done by the desalination of seawater. State of the art desalination plants usually are built with high production capacities and consume a lot of electrical energy or energy from primary resources such as oil. This causes difficulties in rural areas, where no infrastructure is available neither for the plants’ energy supply nor the distribution of the produced potable water. To address this need, small, self-sustaining and locally operated desalination plants came into the focus of research. In this work, a novel flash evaporator design is proposed which can be driven either by solar power or by low temperature waste heat. It offers low operation costs as well as easy maintenance. The results of an experimental setup operated with water at a feed flow rate of up to 1,600 l/h are presented. It is shown that the proof of concept regarding efficient evaporation as well as efficient gas-liquid separation is provided successfully. The experimental evaporation yield counts for 98 % of the vapor content that is expected from the vapor pressure curve of water. Neither measurements of the electrical conductivity of the gained condensate, nor the analysis of the vapor flow by optical methods show significant droplet entrainment, so there are no concerns regarding the purity of the produced condensate for the use as drinking water.
The growing threat posed by multidrug-resistant (MDR) pathogens, such as Klebsiella pneumoniae (Kp), represents a significant challenge in modern medicine. Traditional antibiotic therapies are often ineffective against these pathogens, leading to high mortality rates. MDR Kp infections pose a novel challenge in military medical contexts, particularly in Medical Biodefense, as they can be deliberately spread, leading to resource-intensive care in military centres. Recognizing this issue, the European Defence Agency initiated a prioritised research project in 2023 (EDF Resilience PHAGE- SGA 2023). To address this challenge, the Bundeswehr Institute of Microbiology (IMB) leads BMBF- (Federal Ministry of Education and Research) and EU-funded projects on the use of bacteriophages as adjuvant therapy alongside antibiotics. Since 2017, the IMB has isolated and characterised Kp phages, collecting over 600 isolates and optimizing their production for therapy, in compliance with the EMA (European Medicine Agency) guidelines. This involves in vitro phage genome packaging to minimize endotoxin load, reduce manufacturing costs, and shorten production times. The goal of this work was to establish MinION sequencing (Oxford Nanopore Technology) as a quick and reliable way for initial identification and characterisation of phage genomes. Especially as a quick screening method for isolated on Kp, prior to more precise but also more expensive and time consuming sequencing methods like Illumina. This characterisation is crucial for developing a personalized pipeline aimed at producing magistral or Good Manufacturing Practice (GMP) quality medicinal phage solutions tailored individually for each patient. DNA extraction methods were compared to identify suitable input DNA for sequencing purposes. Additionally, the quality of this DNA was as- sessed to determine its suitability for in vitro phage packaging, which was successfully done achieving a phage titer of 103, confirming that the DNA used for MinION sequencing could indeed be used for acellular packaging. The created genomes were annotated and compared with Illumina sequencing, revealing high similarity in all five individually tested cases. Between the generated sequences only a 4% maximal percentual difference in genome size was observed, while simultaneously showing high similarity in the actual sequence. Throughout the course of this study, a total of 645.15 GB of sequencing data were generated. In total, 38 phages were successfully characterised, with 21 phage genomes assembled and annotated, and saved in the IMB database.
A new formula is presented for transforming fluorescence measurements in accordance with Kubelka-Munk theory. The fluorescence signals, the absorption signals, and data from a selected reference are combined in one expression. Only diode-array techniques can measure all the required data simultaneously to linearize fluorescence data correctly. To prove the new theory HPTLC quantification of the analgesic flupirtine was performed over the mass range 300 to 5000 ng per spot. The fluorescence calibration curve was linear over the whole range. The transformation of fluorescence measurements into linear mass-dependent data extends the technique of in-situ fluorescence analysis to the high concentration range. It also extends Kubelka-Munk theory from absorption to fluorescence analysis. The results presented also emphasize the importance of Kubelka-Munk theory for in-situ measurements in scattering media, especially in planar chromatography.
We present a videodensitometric quantification method for methadone in syrup, separated by thin-layer chromatography (TLC). The quantification is based on a derivation reaction with Dragendorf reagent. Measurements were carried out using a 16-bit flatbed scanner. The range of linearity covers two magnitudes of power using the Kubelka-Munk expression for data transformation. The separation method is inexpensive, fast, and reliable.
A Simple and Reliable HPTLC Method for the Quantification of the Intense Sweetener Sucralose®
(2003)
This paper describes a simple and fast thin layer chromatography (TLC) method for the monitoring of the relatively new intense sweetener Sucralose® in various food matrices. The method requires little or no sample preparation to isolate or concentrate the analyte. The Sucralose® extract is separated on amino‐TLC‐plates, and the analyte is derivatized “reagent‐free” by heating the developed plate for 20 min at 190°C. Spots can be measured either in the absorption or fluorescence mode. The method allows the determination of Sucralose® at the levels of interest regarding foreseen European legislation (>50 mg/kg) with excellent repeatability (RSD = 3.4%) and recovery data (95%).
Diode-array planar chromatography is a versatile tool for identification of pharmaceutical substances In this paper thirty-three compounds with benzodiazepine properties were investigated and the separating conditions for silica gel HPTLC plates and three mobile phases were optimized. Diode-array HPTLC makes it possible to identify all the compounds with high certainty down to a level of 20 ng. An algorithm for spectral recognition which is combined with R F values from the three separation steps into one fit factor is presented. This set of data is unique for each of the compounds investigated and enables unequivocal identification. The method is rapid, inexpensive, and sensitive down to a level of 20 ng mL −1.
High-performance thin-layer chromatography (HPTLC), as the modern form of TLC (thin-layer chromatography), is suitable for detecting pharmaceutically active compounds over a wide polarity range using the gradient multiple development (GMD) technique. Diode-array detection (DAD) in conjunction with HPTLC can simultaneously acquire ultraviolet‒visible (UV‒VIS) and fluorescence spectra directly from the plate. Visualization as a contour plot helps to identify separated zones. An orange peel extract is used as an example to show how GMD‒DAD‒HPTLC in seven different developments with seven different solvents can provide an overview of the entire sample. More than 50 compounds in the extract can be separated on a 6-cm HPTLC plate. Such separations take place in the biologically inert stationary phase of HPTLC, making it a suitable method for effect-directed analysis (EDA). HPTLC‒EDA can even be performed with living organism, as confirmed by the use of Aliivibrio fischeri bacteria to detect bioluminescence as a measure of toxicity. The combining of gradient multiple development planar chromatography with diode-array detection and effect-directed analysis (GMD‒DAD‒HPTLC‒EDA) in conjunction with specific staining methods and time-of-flight mass spectrometry (TOF‒MS) will be the method of choice to find new chemical structures from plant extracts that can serve as the basic structure for new pharmaceutically active compounds.
High performance thin layer chromatography (HPTLC) is a frequently used separation technique which works well for quantification of caffeine and quinine in beverages. Competing separation techniques, e.g. high-performance liquid chromatography (HPLC) or gas chromatography (GC), are not suitable for sugar-containing samples, because these methods need special pretreatment by the analyst. In HPTLC, however, it is possible to separate ‘dirty’ samples without time-consuming pretreatment, because disposable HPTLC plates are used. A convenient method for quantification of caffeine and quinine in beverages, without sample pretreatment, is presented below. The basic theory of in-situ quantification in HPTLC by use of remitted light is introduced and discussed. Several linearization models are discussed.
A home-made diode-array scanner has been used for quantification; this, for the first time, enables simultaneous measurements at different wavelengths. The new scanner also enables fluorescence evaluation without further equipment. Simultaneous recording at different wavelengths improves the accuracy and reliability of HPTLC analysis. These aspects result in substantial improvement of in-situ quantitative densitometric analysis and enable quantification of compounds in beverages.
Fluorescence Enhancement of Pyrene Measured by Thin-Layer Chromatography with Diode-Array Detection
(2003)
In-situ densitometry for qualitative or quantitative purposes is a key step in thin-layer chromatography. It offers a simple way of quantifying by measuring the optical density of the separated spots directly on the plate. A new TLC scanner has been developed which is able to measure TLC plates or HPTLC plates, at different wavelengths simultaneously, without destroying the plate surface. The system enables absorbance and fluorescence measurements in one run. Fluorescence measurements are possible without filters or other adjustments.
The measurement of fluorescence from a TLC plate is a versatile means of making TLC analysis more sensitive. Fluorescence measurements with the new scanner are possible without filters or special lamps. Improvement of the signal-to-noise ratio is achieved by wavelength bundling. During plate scanning the scattered light and the fluorescence are both emitted from the surface of the TLC plate and this emitted light provides the desired spectral information from substances on the TLC plate. The measurement of fluorescence spectra and absorbance spectra directly from a TLC plate is based on differential measurement of light emerging from sample-free and sample-containing zones.
The literature recommends dipping TLC plates in viscous liquids to enhance fluorescence. Measurement of the fluorescence and absorbance spectra of pyrene spots reveals the mechanism of enhancement of plate dipping in viscous liquids—blocked contact of the fluorescent molecules with the stationary phase or other sample molecules is responsible for the enhanced fluorescence at lower concentrations.
In conclusion, dipping in TLC analysis is no miracle. It is based on similar mechanisms observable in liquids. The measured TLC spectra are also very similar to liquid spectra and this makes TLC spec-troscopy an important tool in separation analysis.
A new diode-array scanner in combination with a computer-controlled application system meets all the demands of modern HPTLC measurement. Automatic application, simultaneous measurements at different wavelengths, and different linearization models enable appropriate evaluation of all analytical questions. The theory of error propagation recommends quantification at reflectance values smaller than 0.8; this can be verified only by use of diode-array scanning. The same theory also recommends quantification by use of peak height data, because the theory predicts best precision only for peak height evaluation. Diode-array scanning with reflectance monitoring enables appropriate validation in TLC and HPTLC analysis. All these aspects result in substantial improvement of in-situ quantitative densitometric analysis, and simultaneous recording at different wavelengths opens the way for chemometric evaluation, e.g. peak purity monitoring, which improves the accuracy and reliability of HPTLC analysis.
HPTLC (High Performance Thin Layer Chromatography) is a well known and versatile separation method which shows a lot of advantages and options in comparison to other separation techniques. The method is fast and inexpensive and does not need time-consuming pretreatments. Using fiber-optic elements for controlled light-guiding, the TLC-method was significantly improved: the new HPTLC-system is able to measure simultaneously at different wavelengths without destroying the plate surface or the analytes on the surface. For registration of the sample distribution on a HPTLC-plate we developed a new and sturdy diode-array HPTLC- scanner which allows registration of spectra on the TLC- plates in the range of 198 nm to 610 nm with a spectral resolution better than 1.2 nm. The spatial resolution on plate is better than 160 micrometers . In the spectral mode, the new HPTLC-scanner delivers much more information than the commonly used TLC-scanner. The measurement of 450 spectra of one separation track does not need more than three minutes. However, in the fixed wavelength mode the contour plot can be measured within 15 seconds. In this case, the signal will be summarized and averaged over a spectral range having FWHM from 10 nm to 25 nm depending on the substance under test. The new diode-array HPTLC-scanner makes various chemometric applications possible. The new method can be used easily in clinical diagnostic systems easily, e.g. for blood and uring investigations. In addition, new applications are possible. For example, the rich structured PAHs were studied. Although the separation is incomplete the 16 compounds can be quantified using suitable wavelengths.
In-situ densitometry for qualitative or quantitative purposes is a key step in thin-layer chromatography (TLC). It is a simple means of quantification by measurement of the optical density of the separated spots directly on the plate. A new scanner has been developed which is capable of measuring TLC or HPTLC (high-performance thin-layer chromatography) plates simultaneously at different wavelengths without damaging the plate surface. Fiber optics and special fiber interfaces are used in combination with a diode-array detector. With this new scanner sophisticated plate evaluation is now possible, which enables use of chemometric methods in HPTLC. Different regression models have been introduced which enable appropriate evaluation of all analytical questions. Fluorescent measurements are possible without filters or special lamps and signal-to-noise ratios can be improved by wavelength bundling. Because of the richly structured spectra obtained from PAH, diode-array HPTLC enables quantification of all 16 EPA PAH on one track. Although the separation is incomplete all 16 compounds can be quantified by use of suitable wavelengths. All these aspects are enable substantial improvement of in-situ quantitative densitometric analysis.
In this paper a high-performance thin-layer chromatography (HPTLC) scanner is presented in which a special fibre arrangement is used as HPTLC plate scanning interface. Measurements are taken with a set of 50 fibres at a distance of 400 to 500 μm above the HPTLC plate. Spatial resolutions on the HPTLC plate of better than 160 μm are possible. It takes less than 2 min to scan 450 spectra simultaneously in a range of 198 to 610 nm. The basic improvement of the item is the use of highly transparent glass fibres which provide excellent transmission at 200 nm and the use of a special fibre arrangement for plate illumination and detection.
We present a video-densitometric high-performance thin-layer chromatography (HPTLC) quantification method for patulin in apple juice, developed in a vertical chamber from the starting point to a distance of 50 mm, using MTBE, n-pentane (9 + 5, v/v) as mobile phase. After separation the plate is sprayed with methyl-benzothiazolinone hydrazone hydrochloride monohydrate (MBTH) solution (40 mg in 20 mL methanol) and heated at 105 °C for 15 min. Patulin zones are transformed into yellow spots. The quantification is based on direct measurements using an inexpensive 48-bit flatbed scanner for color measurements (in red, green, and blue). Evaluation of the blue channel makes the measurements very specific. Quantification in fluorescence was also done by use of a 16-bit CCD-camera and UV-366 nm illumination as well as using a HPTLC DAD-scanner. For linearization the extended Kubelka–Munk expression for data transformation was used. The range of linearity covers more than two magnitudes and lies between 5 and 800 ng patulin. The extraction of 20 g apple juice and an extract application on plate up to 50 µL allows statistically defined checking the limit of detection (LOD) of 50 ng patulin per track, which is equivalent to 50 µg patulin per kg apple juice.
The NaSiO Institute (Institute for Sustainable Silicate Research in Offenburg, https://inasio.hs-offenburg.de/) has been working for years on climate-friendly alternatives to insulation materials and inorganic binders, as well as the reasonable use of construction waste in the building industry. The aim of research is to realize the enormous CO 2 saving potential of the construction sector worldwide. A stopping of climate heating will only succeed if these climate-friendly alternatives are used in the construction industry. This is the only way to realize the enormous CO2 savings that will be needed in future to comply with the Paris Agreement.
An Extraction Method for 17α-Ethinylestradiol from Water using a new kind of monolithic Stir-bar
(2015)
Described is a solid body formed with Si, Al, Ca, O and at least one of Na and K, said body exhibiting in the 27Al MAS NMR spectrum a signal additional to the 27Al MAS NMR spectrum of pure calcium aluminate, with a chemical shift sited between that of the main peak of calcium aluminate and the peak next upfield to the main peak of calcium aluminate. Possible uses of the solid body include use as a building material with aggregates, as a coating, as an adhesive for joining two components for sanitary ceramic units, for high-temperature applications, for renovating existing edifices, especially for underwater renovation, for the erection and/or repair of built structures, particularly when high compressive strengths are needed or chemically aggressive conditions arise. It can be produced by bringing waterglass, sodium hydroxide and/or potassium hydroxide, calcium aluminate, one or more aggregates and optionally water, especially sea water, into contact, even at temperatures below 0°C without heating.
A simple Method for quantifying Triazine Herbicides using Thin-Layer Chromatography and a CCD-Camera
(2010)
We present a video-densitometric quantification method for the triazine herbicides atraton, terbumeton, simazine, atrazine, and terbutylazine. Triazine herbicides were separated on silica gel using methyl-t-butyl ether, cyclohexane (1 + 1, v/v) as mobile phase. The quantification is based on a derivation reaction using chlorine and starch-iodine which forms red-brown triazine zones. Measurements were carried out using a 16 bit ST-1603ME CCD camera with 1.56 megapixel from Santa Barbara Instrument Group, Inc., Santa Barbara, USA. A white LED was used for illumination purposes. The range of linearity covers two magnitudes using the (1/R-1) expression data transformation. The signal-to-noise ratio increases directly linearly with the measurement time. The separation method is cheap, fast and reliable.
Melamine (1,3,5-triazine-2,4,6-triamine or cyanuramide, C3H6N6) is a trimer of cyanamide, with a 1,3,5-triazine skeleton (Figure 3.5-1). The molecule contains 66% nitrogen by mass and, if mixed with resins, has fire retardant properties due to its release of nitrogen gas when burned or charred. The word melamine (from German) is a combination of the word melam (which is a distillation derivative of ammonium thiocyanate) and amine [1]. Melamine is also a metabolite of cyromazine, an insecticide in which the proton of an NH2-group is substituted by a cyclopropyl group.
We present a densitometric quantification method for triclosan in toothpaste, separated by high-performance thin-layer chromatography (HPTLC) and using a 48-bit flatbed scanner as the detection system. The sample was band-wise applied to HPTLC plates (10 × 20 cm), with fluorescent dye, Merck, Germany (1.05554). The plates were developed in a vertical developing chamber with 20 min of chamber saturation over 70 mm, using n-heptane–methyl tert-butyl ether–acetic acid (92:8:0.1, V/V) as solvent. The RF value of triclosan is hRF = 22.4, and quantification is based on direct measurements using an inexpensive 48-bit flatbed scanner for color measurements (in red, green, and blue) after plate staining with 2,6-dichloroquinone-4-chloroimide (Gibbs' reagent). Evaluation of the red channel makes the measurements of triclosan very specific. For linearization, an extended Kubelka–Munk expression was used for data transformation. The range of linearity covers more than two orders of magnitude and is between 91 and 1000 ng. The separation method is inexpensive, fast and reliable.
HPTLC (High Performance Thin Layer Chromatography) is a well known and versatile separation method which shows many advantages when compared to other separation techniques. The method is fast and inexpensive and does not need time-consuming pretreatments. For visualisation of the sample distribution on a HPTLC-plate we developed a new and sturdy HPTLC-scanner. The scanner allows simultaneous registrations of spectra in a range from 198 nm to 612 nm with a spectral resolution of better than 0.8 nm. The on-plate spatial resolution is better than 160 μm. The measurement of 450 spectra in one separation track does not need more than two minutes. The new diode-array scanner offers a fast survey over a TLC-separation and makes various chemometric applications possible. For compound identification a cross-correlation function is described to compare UV sample spectra with appropriate library data. The cross-correlation function herein described can also be used for purity testing. Unresolved peaks can be virtually separated by use of a least squares fit algorithm. In summary, the diode arry system delivers much more information than the commonly used TLC-scanner.
Rudolf E. Kaiser
(2020)
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In thin-layer chromatography the development step distributes the sample throughout the layer, a process which strongly affects the reflection signals. The essential requirement for quantitative thinlayer chromatography is not a constant sample concentration but constant sample distribution in each sample spot. This makes evaporation of the mobile phase extremely important, because all tracks of a TLC plate must be dried uniformly. This paper shows that quantitative TLC is possible even if the concentration of the sample is not constant throughout the layer or if the distribution of the sample is not known. With uniform sample distribution, classical Kubelka-Munk theory is valid for isotropic scattering only. In the absence of this constraint classical Kubelka-Munk theory must be extended to situations where scattering is asymmetric. This can be achieved by modification of the original Kubelka-Munk equation. Extended theory is presented which is not only capable of describing asymmetrical scattering in TLC layers but also includes a formula for absorption and fluorescence in diode-array TLC. With this new theory all different formulas for diode-array thin-layer chromatographic evaluation are combined in one expression.
Thin-layer chromatography (TLC) is a well-established and widely used separation technique. Most undergraduate students of chemistry or food science used TLC as a primitive separation tool, which does not need more than small pieces of TLC plates, a glass jar and some solvents. TLC has evolved from a simple separation method of the past into an instrumental technique that offers automation, reproducibility and accurate quantification for a wide variety of applications [1]. The use of modern 10*10 cm TLC plates with narrow particle size distribution is called high performance thin layer chromatography (HPTLC), to distinguish the method from the use of traditional 20 20 cm TLC plates.
A 2D-separation of 16 polyaromatic hydrocarbons (PAHs) according to the Environmental Protecting Agency (EPA) standard was introduced. Separation took place on a TLC RP-18 plate (Merck, 1.05559). In the first direction, the plate was developed twice using n-pentane at −20°C as the mobile phase. The mixture acetonitrile-methanol-acetone-water (12:8:3:3, v/v) was used for developing the plate in the second direction. Both developments were carried out over a distance of 43 mm. Further on in this publication, a specific and very sensitive indication method for benzo[a]pyrene and perylene was presented. The method can detect these hazardous compounds even in complicated PAH mixtures. These compounds can be quantified by a simple chemiluminescent reaction with a limit of detection (LOD) of 48 pg per band for perylene and 95 pg per band for benzo[a]pyrene. Although these compounds were separated from all other PAHs in the standard, a separation of both compounds was not possible from one another. The method is suitable for tracing benzo[a]pyrene and/or perylene. The proposed chemiluminescence screening test on PAHs is extremely sensitive but may indicate a false positive result for benzo[a]pyrene.
The main focus of this chapter is the theoretical and instrumental processes that underpin densitometric methods widely used in thin-layer chromatography (TLC). Densitometric methods include UV–vis, luminescence, and fluorescence optical measurements as well as infrared and Raman spectroscopic measurements. The chapter is divided in two general parts: a theoretical part and a practical part. The systems for direct radioactivity measurements and the combination of TLC with mass spectrometry are also discussed. All these systems allow measuring an intensity distribution directly on a TLC plate. We call this “in situ detection” because no analyte is removed from the plate.
The main focus of this chapter is the theoretical and instrumental processes that underpin densitometric methods widely used in thin-layer chromatography (TLC). Densitometric methods include UV–vis, luminescence and fluorescence optical measurements as well as infrared and Raman spectroscopic measurements. The chapter is divided in two general parts: a theoretical part and a practical part. The systems for direct radioactivity measurements and the combination of TLC with mass spectrometry are also discussed. All these systems allow measuring an intensity distribution directly on a TLC plate. We call this “in situ detection” because no analyte is removed from the plate.