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Sequence-defined poly(amino phosphodiester)s containing main-chain tertiary amines were synthesized by automated solid-phase phosphoramidite chemistry. These polymers were prepared using four monomers with different substituents. The formed polymers were characterized by HPLC and mass spectrometry. These methods evidenced preparation of molecularly-defined polymers. Furthermore, the presence of tertiary amines in the polymer backbones facilitates sequencing by tandem mass spectrometry.
The reliability in measurement results obtained during environmental monitoring is crucial for the assessment and further planning of remediation efforts on the respective contaminated sites by the responsible authorities. A case study concerned with groundwater contaminated with perchloroethylene, trichloroethylene and 1,1,2-trichlorotrifluoroethane including their degradation products which involves private contract laboratories and an independent provider of quality assurance (QA) is presented. The experience gained with biannual monitoring campaigns over 14 years indicates that the selection of contractors on basis of accreditation status and successful performance in interlaboratory comparisons are not sufficient. Rather the auditing of the contractors by the QA provider prior to each campaign and the crosschecking of selected monitoring samples by the QA provider led to a lasting improvement of reliability in the contractors' measurement results. A mean deviation of 20% from the reference value determined by the QA provider for the crosschecked samples was reached.
The vanadium redox flow battery (VRFB) is currently a potential candidate for stationary energy storage. A major challenge is the unintended vanadium transport through the separator, which results in a fade of capacity. To overcome this issue, it is necessary to understand the transport processes in the membrane on a more fundamental level. In this work, the vanadium species distribution in Nafion™ 117 after cyclization was investigated. Two membranes, one from a charged VRFB and another from a discharged VRFB, were analyzed using ultraviolet–visible spectroscopy (UV/VIS) and X-ray absorption near edge structure spectroscopy (XANES). Little difference between the two membranes was recognizable according to the UV/VIS results. In comparison, the XANES results showed that the membrane from the charged VRFB contains more V3+ than VO2+, whereas for the discharged case, more VO2+ is present in the membrane.
A core component of energy storage systems like vanadium redox flow batteries (VRFB) is the polymer electrolyte membrane (PEM). In this work, the frequently used perfluorosulfonic-acid (PFSA) membrane Nafion™ 117 and a novel poly (vinylidene difluoride) (PVDF)-based Membrane are investigated. A well-known problem in VRFBs is the vanadium permeation through the membrane. The consequence of this so-called vanadium crossover is a severe loss of capacity. For a
better understanding of vanadium transport in membranes, the uptake of vanadium ions from electrolytes containing Vdimer(IV–V) and for comparison also V(II), V(III), V(IV), and V(V) by both membranes was studied. UV/VIS spectroscopy, X-ray absorption near edge structure spectroscopy (XANES), total reflection X-ray fluorescence spectroscopy (TXRF), inductively coupled plasma optical emission spectrometry (ICP-OES), and micro X-ray fluorescence spectroscopy (microXRF) were used to determine the vanadium concentrations and the species inside the membrane. The results strongly support that Vdimer(IV–V), a dimer formed from V(IV) and V(V), enters the nanoscopic water-body of Nafion™ 117 as such. This is interesting, because as of now, only the individual ions V(IV) and V(V) were considered to be transported through the membrane. Additionally, it was found that the Vdimer(IV–V) dimer partly dissociates to the individual ions in the novel PVDF-based membrane.
The Vdimer(IV–V) dimer concentration in Nafion™ was determined and compared to those of the other species. After three days of equilibration time, the concentration of the dimer is the lowest compared to the monomeric vanadium species. The concentration of vanadium in terms of the relative uptake λ = n(V)/n(SO3
) are as follows: V(II) [λ = 0.155] > V(III) [λ = 0.137] > V(IV) [λ = 0.124] > V(V) [λ = 0.053] > Vdimer(IV–V) [λ = 0.039]. The results show that the Vdimer(IV–V) dimer Needs to be considered in addition to the other monomeric species to properly describe the transport of vanadium through Nafion™ in VRFBs.
En este artículo se presentan 2 metodologías basadas en las formulaciones del Método de los Elementos de Contorno y del Método de los Elementos Finitos para estudiar el efecto de la interacción suelo-estructura en el comportamiento dinámico de edificaciones. Se ha estudiado la respuesta de un edificio de 3 plantas producida por un campo de ondas incidente con los 2 métodos propuestos. Los resultados obtenidos presentan un buen grado de acuerdo entre ellos. A partir de estos resultados se ha validado un modelo aproximado para estudiar este tipo de problemas y se han examinado diferentes tipologías de edificaciones. Las conclusiones alcanzadas muestran que la respuesta global de las estructuras se debe a la deformación de los forjados y depende de su superficie, de las condiciones de apoyo y del acoplamiento con los forjados de la misma planta. Del mismo modo, se ha observado un acoplamiento del comportamiento de pilares y forjados cuando las rigideces de ambos son similares.----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------- This paper presents 2 methodologies based on the Boundary Element Method and the Finite Element Method to study soil-structure interaction effect on building behaviour. A 3-story building response induced by an incident wave field is studied using both methods. The results obtained show a good agreement. Then, a simplified model is validated from these methods and several buildings are analysed. Conclusions show that structural responses are due to floor deformation, and depend on their area, support conditions and coupling. A coupling between floors and columns when both elements have similar stiffness is also observed.
A liver biopsy specimen from a Wilson’s disease (WD) patient was analyzed by means of micro-X-ray fluorescence (mXRF) spectroscopy to determine the elemental distribution. First, bench-top mXRF was utilized for a coarse scan of the sample under laboratory conditions. The resulting distribution maps of copper and iron enabled the determination of a region of interest (ROI) for further analysis. In order to obtain more detailed elemental information, this ROI was analyzed by synchrotron radiation (SR)-based mXRF with a beam size of 4 mm offering a resolution at the cellular level. Distribution maps of additional elements to copper and iron like zinc and manganese were obtained due to a higher sensitivity of SR-mXRF. In addition to this, X-ray absorption near edge structure spectroscopy (XANES) was performed to identify the oxidation states of copper in WD. This speciation analysis indicated a mixture of copper(I) and copper(II) within the WD liver tissue.
Im Rahmen des Ökologischen Großprojekts "Industriegebiet Spree" der Senatsverwaltung für Umwelt, Verkehr und Klimaschutz (SenUVK), Berlin, wurde als Überwachungssystem für laufende Gefahrenabwehr- und Sanierungsmaßnahmen ein Grundwasser-Monitoring eingerichtet. Die Maßnahmen zur externen Qualitätssicherung der Laborarbeiten im Monitoring werden zusammenfassend dargestellt.
Um einen vergleichbaren und hohen Qualitätsstandard der Analytik zu gewährleisten, ist die Ausschreibung der analytischen Leistungen in diesem Projekt direkt an die Teilnahme an einem Ringversuch zur Bestimmung von Anilin und Anilinderivaten in Wasser gekoppelt. Die Ergebnisse des Ringversuchs werden im Einzelnen vorgestellt.