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Subject: Dissolution ×

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Now showing 1 - 6 of 6
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    Dissolution and precipitation of copper-rich phases during heating and cooling of precipitation-hardening steel X5CrNiCuNb16-4 (17-4 PH)
    (Dordrecht [u.a.] : Springer Science + Business Media B.V, 2020) Rowolt, Christian; Milkereit, Benjamin; Springer, Armin; Kreyenschulte, Carsten; Kessler, Olaf
    Continuous heating transformation (CHT) diagrams and continuous cooling transformation (CCT) diagrams of precipitation-hardening steels have the drawback that important information on the dissolution and precipitation of Cu-rich phases during continuous heating and cooling are missing. This work uses a comparison of different techniques, namely dilatometry and differential scanning calorimetry for the in situ analysis of the so far neglected dissolution and precipitation of Cu-rich phases during continuous heating and cooling to overcome these drawbacks. Compared to dilatometry, DSC is much more sensitive to phase transformation affecting small volume fractions, like precipitation. Thus, the important solvus temperature for the dissolution of Cu-rich phases was revealed from DSC and integrated into the CHT diagram. Moreover, DSC reveals that during continuous cooling from solution treatment, premature Cu-rich phases may form depending on cooling rate. Those quench-induced precipitates were analysed for a broad range of cooling rates and imaged for microstructural analysis using optical microscopy, scanning electron microscopy and transmission electron microscopy. This information substantially improves the CCT diagram.
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    Polysulfide driven degradation in lithium–sulfur batteries during cycling – quantitative and high time-resolution operando X-ray absorption study for dissolved polysulfides probed at both electrode sides
    (London [u.a.] : RSC, 2021) Zech, Claudia; Hönicke, Philipp; Kayser, Yves; Risse, Sebastian; Grätz, Olga; Stamm, Manfred; Beckhoff, Burkhard
    The development of operando characterization techniques on realistic batteries is essential for an advanced mechanistic understanding in battery chemistry and, therefore, contributes to their further performance improvement. This manuscript presents operando Near-Edge X-ray Absorption Spectroscopy (NEXAFS) traceable to the SI units (SI is the abbreviation for the International System of Units) during multiple charge–discharge cycles on both electrodes of lithium–sulfur (Li/S) coin cells which enables an absolute quantification of dissolved polysulfides with no need for calibration samples or reference material. We could reveal that during the charging process, polysulfide (PS) movement from the negative to the positive electrode is inhibited. This leads to a steady increase of dissolved polysulfides at the anode side and, therefore, is one of the key points for capacity fading. We quantitatively track the polysulfides dissolved in the electrolyte and correlate for the first time their evolution with the capacity fading of the cell. We analyze the appearance of PS during cell operation at the cathode and anode side to characterize the transport mechanisms of the polysulfide shuttle phenomena and to reveal quantitative information about their evolution at different states of charge and states of health. Our cell design suppresses the contribution of cathodic sulfur, which is mandatory for reference-sample-free quantification in X-ray spectrometry and allows us to use only slightly modified standard coin cell batteries.
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    Reliable release testing for nanoparticles with the NanoDis System, an innovative sample and separate technique
    (New York, NY [u.a.] : Elsevier, 2021) Lombardo, Sonia M.; Türeli, Nazende Günday; Koch, Marcus; Schneider, Marc; Türeli, Akif E.
    One of the critical quality attributes of nanoparticle formulations is drug release. Their release properties should therefore be well characterized with predictive and discriminative methods. However, there is presently still no standard method for the release testing of extended release nanoformulations. Dialysis techniques are widely used in the literature but suffer from severe drawbacks. Burst release of formulations can be masked by slow permeation kinetics of the free drug through the dialysis membrane, saturation in the membrane, and absence of agitation in the membrane. In this study, the release profile of poly(lactic co-glycolic) (PLGA) nanocapsules loaded with all-trans retinoic acid was characterized using an innovative sample and separate set-up, the NanoDis System, and compared to the release profile measured with a dialysis technique. The NanoDis System showed clear superiority over the dialysis method and was able to accurately characterize the burst release from the capsules and furthermore discriminate between different all-trans retinoic acid nanoparticle formulations.
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    Poly(ethylene oxide)-based block copolymers with very high molecular weights for biomimetic calcium phosphate mineralization
    (London : RSC Publishing, 2015) Mai, Tobias; Boye, Susanne; Yuan, Jiayin; Völkel, Antje; Gräwert, Marlies; Günter, Christina; Lederer, Albena; Taubert, Andreas
    The present article is among the first reports on the effects of poly(ampholyte)s and poly(betaine)s on the biomimetic formation of calcium phosphate. We have synthesized a series of di- and triblock copolymers based on a non-ionic poly(ethylene oxide) block and several charged methacrylate monomers, 2-(trimethylammonium)ethyl methacrylate chloride, 2-((3-cyanopropyl)-dimethylammonium)ethyl methacrylate chloride, 3-sulfopropyl methacrylate potassium salt, and [2-(methacryloyloxy)ethyl]dimethyl-(3-sulfopropyl)ammonium hydroxide. The resulting copolymers are either positively charged, ampholytic, or betaine block copolymers. All the polymers have very high molecular weights of over 106 g mol−1. All polymers are water-soluble and show a strong effect on the precipitation and dissolution of calcium phosphate. The strongest effects are observed with triblock copolymers based on a large poly(ethylene oxide) middle block (nominal Mn = 100 000 g mol−1). Surprisingly, the data show that there is a need for positive charges in the polymers to exert tight control over mineralization and dissolution, but that the exact position of the charge in the polymer is of minor importance for both calcium phosphate precipitation and dissolution.
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    Shear wave reflection seismic yields subsurface dissolution and subrosion patterns: application to the Ghor Al-Haditha sinkhole site, Dead Sea, Jordan
    (Göttingen : Copernicus Publ., 2018) Polom, Ulrich; Alrshdan, Hussam; Al-Halbouni, Djamil; Holohan, Eoghan P.; Dahm, Torsten; Sawarieh, Ali; Atallah, Mohamad Y.; Krawczyk, Charlotte M.
    Near-surface geophysical imaging of alluvial fan settings is a challenging task but crucial for understating geological processes in such settings. The alluvial fan of Ghor Al-Haditha at the southeast shore of the Dead Sea is strongly affected by localized subsidence and destructive sinkhole collapses, with a significantly increasing sinkhole formation rate since ca. 1983. A similar increase is observed also on the western shore of the Dead Sea, in correlation with an ongoing decline in the Dead Sea level. Since different structural models of the upper 50 m of the alluvial fan and varying hypothetical sinkhole processes have been suggested for the Ghor Al-Haditha area in the past, this study aimed to clarify the subsurface characteristics responsible for sinkhole development. For this purpose, high-frequency shear wave reflection vibratory seismic surveys were carried out in the Ghor Al-Haditha area along several crossing and parallel profiles with a total length of 1.8 and 2.1 km in 2013 and 2014, respectively. The sedimentary architecture of the alluvial fan at Ghor Al-Haditha is resolved down to a depth of nearly 200 m at a high resolution and is calibrated with the stratigraphic profiles of two boreholes located inside the survey area. The most surprising result of the survey is the absence of evidence of a thick (> 2–10 m) compacted salt layer formerly suggested to lie at ca. 35–40 m depth. Instead, seismic reflection amplitudes and velocities image with good continuity a complex interlocking of alluvial fan deposits and lacustrine sediments of the Dead Sea between 0 and 200 m depth. Furthermore, the underground section of areas affected by sinkholes is characterized by highly scattering wave fields and reduced seismic interval velocities. We propose that the Dead Sea mud layers, which comprise distributed inclusions or lenses of evaporitic chloride, sulfate, and carbonate minerals as well as clay silicates, become increasingly exposed to unsaturated water as the sea level declines and are consequently destabilized and mobilized by both dissolution and physical erosion in the subsurface. This new interpretation of the underlying cause of sinkhole development is supported by surface observations in nearby channel systems. Overall, this study shows that shear wave seismic reflection technique is a promising method for enhanced near-surface imaging in such challenging alluvial fan settings.
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    Time-lapse gravity and levelling surveys reveal mass loss and ongoing subsidence in the urban subrosion-prone area of Bad Frankenhausen, Germany
    (Göttingen : Copernicus Publ., 2019) Kobe, Martin; Gabriel, Gerald; Weise, Adelheid; Vogel, Detlef
    We present results of sophisticated, high-precision time-lapse gravity monitoring that was conducted over 4 years in Bad Frankenhausen (Germany). To our knowledge, this is the first successful attempt to monitor subrosion-induced mass changes in urban areas with repeated gravimetry. The method provides an approach to estimate the mass of dissolved rocks in the subsurface. Subrosion, i.e. leaching and transfer of soluble rocks, occurs worldwide. Mainly in urban areas, any resulting ground subsidence can cause severe damage, especially if catastrophic events, i.e. collapse sinkholes, occur. Monitoring strategies typically make use of established geodetic methods, such as levelling, and therefore focus on the associated deformation processes. In this study, we combine levelling and highly precise time-lapse gravity observations. Our investigation area is the urban area of Bad Frankenhausen in central Germany, which is prone to subrosion, as many subsidence and sinkhole features on the surface reveal. The city and the surrounding areas are underlain by soluble Permian deposits, which are continuously dissolved by meteoric water and groundwater in a strongly fractured environment. Between 2014 and 2018, a total of 17 high-precision time-lapse gravimetry and 18 levelling campaigns were carried out in quarterly intervals within a local monitoring network. This network covers historical sinkhole areas but also areas that are considered to be stable. Our results reveal ongoing subsidence of up to 30.4 mm a−1 locally, with distinct spatiotemporal variations. Furthermore, we observe a significant time-variable gravity decrease on the order of 8 µGal over 4 years at several measurement points. In the processing workflow, after the application of all required corrections and least squares adjustment to our gravity observations, a significant effect of varying soil water content on the adjusted gravity differences was figured out. Therefore, we place special focus on the correlation of these observations and the correction of the adjusted gravity differences for soil water variations using the Global Land Data Assimilation System (GLDAS) Noah model to separate these effects from subrosion-induced gravity changes. Our investigations demonstrate the feasibility of high-precision time-lapse gravity monitoring in urban areas for sinkhole investigations. Although the observed rates of gravity decrease of 1–2 µGal a−1 are small, we suggest that it is significantly associated with subterranean mass loss due to subrosion processes. We discuss limitations and implications of our approach, as well as give a first quantitative estimation of mass transfer at different depths and for different densities of dissolved rocks.