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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.
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.
Bewegungsanalysesysteme in der Forschung und für niedergelassene Orthopädinnen und Orthopäden
(2023)
Hintergrund
Komplexe biomechanische Bewegungsanalysen können für eine Vielzahl orthopädischer Fragestellungen wichtige Informationen liefern. Bei der Beschaffung von Bewegungsanalysesystemen sind neben den klassischen Messgütekriterien (Validität, Reliabilität, Objektivität) auch räumliche und zeitliche Rahmenbedingungen sowie Anforderungen an die Qualifikation des Messpersonals zu berücksichtigen.
Anwendung
In der komplexen Bewegungsanalyse werden Systeme zur Bestimmung der Kinematik, der Kinetik und der Muskelaktivität (Elektromyographie) eingesetzt. Der vorliegende Artikel gibt einen Überblick über Methoden der komplexen biomechanischen Bewegungsanalyse für den Einsatz in der orthopädischen Forschung oder in der individuellen Patientenversorgung. Neben dem Einsatz zur reinen Bewegungsanalyse wird auch der Einsatz von Bewegungsanalyseverfahren im Bereich des Biofeedbacktrainings diskutiert.
Beschaffung
Für die konkrete Anschaffung von Bewegungsanalysesystemen empfiehlt sich die Kontaktaufnahme mit Fachgesellschaften (z. B. Deutsche Gesellschaft für Biomechanik), Hochschulen und Universitäten mit vorhandenen Bewegungsanalyseeinrichtungen oder Vertriebsfirmen im Bereich der Biomechanik.
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.
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.
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.
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.
Der Einbau von Smart Metern und deren intelligente Vernetzung in Richtung eines Smart Grid wird Stromverbrauchsmuster bis in die Haushalte hinein verändern. Über die technisch geprägte Diskussion um die Komponenten dafür darf deshalb keinesfalls die Einbeziehung der Gesellschaft in den anstehenden Wandel vergessen werden. Transparenz bei den Kosten, die Förderung von Vertrauen insbesondere in die Datenschutzstandards und eine verständliche Aufklärungsarbeit sind Schlüssel für den notwendigen Dialog zwischen Energieversorgern, Politik und Bürgern.
Im Eurocode 3 wird im Gegensatz zu DIN 18800 die Bemessung von Verbindungen nicht in der Grundnorm DIN EN 1993‐1‐1, sondern in anderen Normenteilen geregelt. Dieser Beitrag behandelt die Bemessung geschweißter Verbindungen nach DIN EN 1993‐1‐8, die auch Hohlprofile, aber weder dünnwandige Bauteile noch Stähle höherer Festigkeit als S460 einschließt, vergleicht diese Bemessung mit der nach DIN 18800‐1, erläutert sie an Beispielen und hebt die wesentlichen Änderungen hervor. Da diese Änderungen auch die im Vergleich zu DIN 18800 viel stärkere Verknüpfung der in der Tragwerksplanung ansetzbaren Beanspruchbarkeiten mit dem Aufwand der Prüfung und Qualitätsüberwachung bei der Herstellung betreffen, werden abschließend wichtige Regelungen der DIN EN 1090‐2 zur Ausführung und Prüfung von Schweißnähten beschrieben, die auch der Tragwerksplaner kennen muss.
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.
Hintergrund
In diesem Artikel wird ein Überblick und Vergleich der am häufigsten verwendeten zementierten Hüftschäfte, gruppiert in die verschiedenen Schafttypen und Zementmanteldicken, gegeben, um zu sehen, welche Kombination gut abschneidet.
Methodik
Aus dem Endoprothesenregister Deutschland wurden die Revisionsraten zementierter Schaftarten kategorisiert und die Revisionsraten von 3 und 5 Jahren erfasst und analysiert. Für die Recherche lag die Konzentration auf den Schäften Exeter, C‑Stem, MS-30, Excia, Bicontact, Charnley, Müller Geradschaft, Twinsys, Corail, Avenir, Quadra und dem Lubinus SP II. Ein wichtiger Aspekt lag darin, welcher Schaft favorisiert implantiert wird und welche Zementiertechnik in Hinblick auf die geplante Zementmanteldicke angewendet wird. Um einen Trend in der zementierten Hüftendoprothetik herauszufinden, wurden zusätzlich die Daten des dänischen, schwedischen, norwegischen, schweizerischen, neuseeländischen, englischen und australischen Endoprothesenregister verglichen.
Ergebnisse und Schlussfolgerung
Die meisten Länder nutzen zementierte Prothesen nach dem Kraftschlussprinzip (Exeter, MS30, C‑Stem etc.) oder dem Formschlussprinzip (Charnley, Excia, Bicontact), welche mit einer Zementmanteldicke von 2–4 mm implantiert werden. Jedoch hat sich in Deutschland und der Schweiz ein Trend zur Line-to-Line-Technik, mit einer geplanten Zementmanteldicke von 1 mm (Twinsys, Corail, Avenir, Quadra) aufgezeigt, dem Prinzip der Müller-Geradschaft-Prothese und der Kerboul-Charnley-Prothese folgend, auch wenn diese an sich als „french paradoxon“ postuliert werden. In den EPRD-5-Jahres-Ergebnissen scheinen die neueren Line-to-Line-Prothesen etwas schlechter abzuschneiden. Die besten Ergebnisse erzielt der „MS 30“ in Deutschland und der „Exeter“ in England. Hierbei handelt es sich um polierte Geradschäfte mit Zentraliser und Subsidence-Raum an der Spitze mit einem 2–4 mm Zementmantel in guter Zementiertechnik.
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.
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.
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.
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%).
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.
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.
An Extraction Method for 17α-Ethinylestradiol from Water using a new kind of monolithic Stir-bar
(2015)
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.
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.
Two solvent mixtures for high-performance thin-layer chromatographic (HPTLC) separation of some compounds showing estrogenic activity in the yeast estrogen screen (YES) assay are presented. The new method, planar yeast estrogen screen (pYES) combines the YES assay and a chromatographic separation on silica gel HPTLC plates with the performance of the YES assay. For separation, the analytes were applied bandwise to HPTLC plates (10 × 20 cm) with fluorescent dye (Merck, Germany). The plates were developed in a vertical developing chamber after 30 min of chamber saturation over a separation distance of 70 mm, using cyclohexane‒methyl-ethyl ketone (2:1, V/V) or cyclohexane‒CPME (3:2, V/V) as solvents. Both solvents allow separation of estriol, daidzein, genistein, 17β-estradiol, 17α-ethinyl estradiol, estrone, 4-nonylphenol and bis(2-ethylhexyl) phthalate.
An algorithm is presented that has successfully been utilized in practice for several years. It improves data analysis in chromatography. The program runs in an extremely reliable way and evaluates chromatographic raw data with an acceptable error. The algorithm requires a minimum of preliminaries and integrates even unsmoothed noisy data correctly.
Improved separation of highly toxic contact herbicides paraquat (1,1′-dimethyl-4-4′-bipyridinium), diquat (6,7-dihydrodipyridol[ 1,2-a:2′,1′-c]pyrazine-5,8-di-ium), difenzoquat (1,2-dimethyl-3,5-diphenyl-1H-pyrazolium-methyl sulfate), mepiquat (1,1-dimethyl-piperidinium), and chloromequat (2-chloroethyltrimethylammonium) were presented by high-performance thin-layer chromatography (HPTLC). The quantification is based on a derivatization reaction, using sodium tetraphenylborate. Measurements were made in the wavelength range from 500 to 535 nm, using a light-emitting diode (LED) for excitation purposes, which emits very dense light at 365 nm. For calculations, a new theory of standard addition method was used, thus leading to a minimal error if exactly the same amount of sample content is added as a standard. The method provides a fast and inexpensive approach to quantification of the five most important quats used for plant protection purposes. The method works reliably because it takes into account losses during pre-treatment procedure. The method meets the European legislation limits for paraquat and diquat in drinking water according to United States Environmental Protection Agency (US EPA) method 549.2 which are 680 ng L−1 for paraquat and 720 ng L−1 for diquat. The method of standard addition in planar chromatography can be beneficially used to reduce systematic errors. Although recovery rates of 33.7% to 65.2% are observed, calculated contents according to the method of standard addition lie between 69% and 127% of the theoretical amounts.
Selective separation of CO2-CH4 mixed gases via magnesium aminoethylphosphonate nanoparticles
(2016)
The CO2 uptake on nanoscale AlO(OH) hollow spheres (260 mg g−1) as a new material is comparable to that on many metal–organic frameworks although their specific surface area is much lower (530 m2 g¬1versus 1500–6000 m2g¬1). Suited temperature–pressure cycles allow for reversible storage and separation of CO2 while the CO2 uptake is 4.3-times higher as compared to N2.
Mass transfer phenomena in membrane fuel cells are complex and diversified because of the presence of complex transport pathways including porous media of very different pore sizes and possible formation of liquid water. Electrochemical impedance spectroscopy, although allowing valuable information on ohmic phenomena, charge transfer and mass transfer phenomena, may nevertheless appear insufficient below 1 Hz. Use of another variable, that is, back pressure, as an excitation variable for electrochemical pressure impedance spectroscopy is shown here a promising tool for investigations and diagnosis of fuel cells.
Pure orbital blowout fractures occur within the confines of the internal orbital wall. Restoration of orbital form and volume is paramount to prevent functional and esthetic impairment. The anatomical peculiarity of the orbit has encouraged surgeons to develop implants with customized features to restore its architecture. This has resulted in worldwide clinical demand for patient-specific implants (PSIs) designed to fit precisely in the patient’s unique anatomy. Material extrusion or Fused filament fabrication (FFF) three-dimensional (3D) printing technology has enabled the fabrication of implant-grade polymers such as Polyetheretherketone (PEEK), paving the way for a more sophisticated generation of biomaterials. This study evaluates the FFF 3D printed PEEK orbital mesh customized implants with a metric considering the relevant design, biomechanical, and morphological parameters. The performance of the implants is studied as a function of varying thicknesses and porous design constructs through a finite element (FE) based computational model and a decision matrix based statistical approach. The maximum stress values achieved in our results predict the high durability of the implants, and the maximum deformation values were under one-tenth of a millimeter (mm) domain in all the implant profile configurations. The circular patterned implant (0.9 mm) had the best performance score. The study demonstrates that compounding multi-design computational analysis with 3D printing can be beneficial for the optimal restoration of the orbital floor.
We present a video-densitometric quantification method for the pain killer known as diclofenac and ibuprofen. These non-steroidal anti-inflammatory drugs were separated on cyanopropyl bonded plates using CH2Cl2, methanol, cyclohexane (95 + 5 + 40, v/v) as mobile phase. The quantification is based on a bio-effective-linked analysis using Vibrio fisheri bacteria. Within 10 min a CCD-camera registered the white light of the light-emitting bacteria. Diclofenac and ibuprofen effectively suppressed the bacterial light emission which can be used for quantification within a linear range of 10 to 2000 ng. The detection limit for ibuprofen is 20 ng and the limit of quantification 26 ng per zone. Measurements were carried out using a 16-bit ST-1603ME CCD camera with 1.56 megapixels (from Santa Barbara Instrument Group, Inc., Santa Barbara, USA). The range of linearity covers more than two magnitudes because the extended Kubelka-Munk expression is used for data transformation. The separation method is inexpensive, fast, and reliable.
We present a video-densitometric quantification method in combination with diode-array quantification for the methyl-, ethyl-, propyl-, and butylparaben in cosmetics. These parabens were separated on cyanopropyl bonded plates using water-acetonitrile-dioxane-ethanol-NH3 (25%) (8:2:1:1:0.05, v/v) as mobile phase. The quantification is based on UV-measurements at 255 nm and a bioeffectively-linked analysis using Vibrio fischeri bacteria. Within 5 min, a Tidas S 700 diode-array scanner (J&M, Aalen, Germany) scans 8 tracks and thus measures in total 5600 spectra in the wavelengths range from 190 to 1000 nm. The quantification range for all these parabens is from 20 to 400 ng per band, measured at 255 nm. In the V. fischeri assay a CCD-camera registers the white light of the light-emitting bacteria within 10 min. All parabens effectively suppress the bacterial light emission which can be used for quantifying within a linear range from 100 to 400 ng. Measurements were carried out using a 16-bit MicroChemi chemiluminescence system (biostep GmbH, Jahnsdorf, Germany), using a CCD camera with 4.19 megapixels. The range of linearity is achieved because the extended Kubelka-Munk expression was used for data transformation. The separation method is inexpensive, fast, and reliable.
Cast iron materials are used as materials for cylinder heads for heavy duty internal combustion engines. These components must withstand severe cyclic mechanical and thermal loads throughout their service life. While high-cycle fatigue (HCF) is dominant for the material in the water jacket region, the combination of thermal transients with mechanical load cycles results in thermomechanical fatigue (TMF) of the material in the fire deck region, even including superimposed TMF and HCF loads. Increasing the efficiency of the engines directly leads to increasing combustion pressure and temperature and, thus, lower safety margins for the currently used cast iron materials or alternatively the need for superior cast iron materials. In this paper (Part I), the TMF properties of the lamellar graphite cast iron GJL250 and the vermicular graphite cast iron GJV450 are characterized in uniaxial tests and a mechanism-based model for TMF life prediction is developed for both materials. The model can be used to estimate the fatigue life of components by means of finite-element calculations (Part II of the paper) and supports engineers in finding the appropriate material and design. Furthermore, the effect of the elastic, plastic and creep properties of the materials on the fatigue life can be evaluated with the model. However, for a material selection also the thermophysical properties, controlling to a high level the thermal stresses in the component, must be considered. Hence, the need for integral concepts for material characterization and selection from a multitude of existing and soon-to-be developed cast iron materials is discussed.