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Nuclear magnetic resonance (NMR) spectrometric methods for the quantitative analysis of pure heparin in crude heparin is proposed. For quantification, a two-step routine was developed using a USP heparin reference sample for calibration and benzoic acid as an internal standard. The method was successfully validated for its accuracy, reproducibility, and precision. The methodology was used to analyze 20 authentic porcine heparinoid samples having heparin content between 4.25 w/w % and 64.4 w/w %. The characterization of crude heparin products was further extended to a simultaneous analysis of these common ions: sodium, calcium, acetate and chloride. A significant, linear dependence was found between anticoagulant activity and assayed heparin content for thirteen heparinoids samples, for which reference data were available. A Diffused-ordered NMR experiment (DOSY) can be used for qualitative analysis of specific glycosaminoglycans (GAGs) in heparinoid matrices and, potentially, for quantitative prediction of molecular weight of GAGs. NMR spectrometry therefore represents a unique analytical method suitable for the simultaneous quantitative control of organic and inorganic composition of crude heparin samples (especially heparin content) as well as an estimation of other physical and quality parameters (molecular weight, animal origin and activity).
Lignin is a promising renewable biopolymer being investigated worldwide as an environmentally benign substitute of fossil-based aromatic compounds, e.g. for the use as an excipient with antioxidant and antimicrobial properties in drug delivery or even as active compound. For its successful implementation into process streams, a quick, easy, and reliable method is needed for its molecular weight determination. Here we present a method using 1H spectra of benchtop as well as conventional NMR systems in combination with multivariate data analysis, to determine lignin’s molecular weight (Mw and Mn) and polydispersity index (PDI). A set of 36 organosolv lignin samples (from Miscanthus x giganteus, Paulownia tomentosa and Silphium perfoliatum) was used for the calibration and cross validation, and 17 samples were used as external validation set. Validation errors between 5.6% and 12.9% were achieved for all parameters on all NMR devices (43, 60, 500 and 600 MHz). Surprisingly, no significant difference in the performance of the benchtop and high-field devices was found. This facilitates the application of this method for determining lignin’s molecular weight in an industrial environment because of the low maintenance expenditure, small footprint, ruggedness, and low cost of permanent magnet benchtop NMR systems.
Heparin is a natural polysaccharide, which plays essential role in many biological processes. Alterations in building blocks can modify biological roles of commercial heparin products, due to significant changes in the conformation of the polymer chain. The variability structure of heparin leads to difficulty in quality control using different analytical methods, including infrared (IR) spectroscopy. In this paper molecular modelling of heparin disaccharide subunits was performed using quantum chemistry. The structural and spectral parameters of these disaccharides have been calculated using RHF/6-311G. In addition, over-sulphated chondroitin sulphate disaccharide was studied as one of the most widespread contaminants of heparin. Calculated IR spectra were analyzed with respect to specific structure parameters. IR spectroscopic fingerprint was found to be sensitive to substitution pattern of disaccharide subunits. Vibrational assignments of calculated spectra were correlated with experimental IR spectral bands of native heparin. Chemometrics was used to perform multivariate analysis of simulated spectral data.
Alte, geschichtsrelevante und thematisch angeordnete Objekte, welche man in den Vitrinen der Museen betrachten kann, das kennt sicher jeder. Doch wie kommen diese Artefakte eigentlich in die Vitrinen? Welche Menschen sind dafür verantwortlich, dass wir diese Kulturgüter bestaunen können? In diesem temporären Ausstellungskonzept für das Römisch-Germanische Museum Köln geht es darum, die sonst verborgene Arbeit der Restauratoren des Museums für die Besucher:innen sichtbar zu machen, ihnen genauere Einblicke in die Arbeit mit ihren Anforderungen zu geben und Restaurierungsprozesse auf zu zeigen. Diese Arbeit demonstriert, wie es abseits der Öffentlichkeit aussieht und wer dafür verantwortlich ist, dass wir einen Einblick in die vergangenen Zeit erhalten können. Das Projekt zeigt eine mögliche Bespielung des Museums, wie das Berufsbild der Restauratoren in die Dauerausstellung integriert werden könnte.
Nur ein Freitag : Ein Kurzfilm über Verlust und Freundschaft im Schatten
des Zweiten Weltkrieges.
(2022)
Der Film zeigt die wahre Geschichte des 15-jährigen Hans Jokisch, welche auf den Erzählungen seiner jüngeren Schwester, der Zeitzeugin Maria Theis (geb. Jokisch), beruhen.
Der Fokus liegt auf der Sichtweise von Kindern und Jugendlichen, einer Generation, die mit dem und im Zweiten Weltkrieg aufgewachsen ist und die gleichzeitig die letzte Generation ist, die uns das Erlebte noch aus erster Hand berichten kann. Hans gelangt mit seiner Familie nach einer harten Flucht vor der Frontlinie zurück in seine Heimat in Schlesien. Doch ihr geliebtes Heim ist besetzt von Familie Schöppe. Sie haben keine Wahl, die beiden Familien müssen sich das Haus von nun an teilen. Im Laufe der Zeit wird das Jokisch Haus auch für Familie Schöppe ein Zuhause und Hans freundet sich mit dem Jungen Bruno Schöppe an. Als Deutschland 1945 kapituliert und Schlesien nun zu Polen gehört, müssen plötzlich beide Familien endgültig das Haus und all ihren Besitz zurücklassen. Hans und Bruno beschließen, die Zwangsenteignung nicht hinzunehmen, doch ihr naiver Plan wird ihnen fast zum Verhängnis.
An improved and convenient ninhydrin assay for aminoacylase activity measurements was developed using the commercial EZ Nin™ reagent. Alternative reagents from literature were also evaluated and compared. The addition of DMSO to the reagent enhanced the solubility of Ruhemann's purple (RP). Furthermore, we found that the use of a basic, aqueous buffer enhances stability of RP. An acidic protocol for the quantification of lysine was developed by addition of glacial acetic acid. The assay allows for parallel processing in a 96-well format with measurements microtiter plates.
The replacement of existing spillway crests or gates with labyrinth weirs is a proven techno-economical means to increase the discharge capacity when rehabilitating existing structures. However, additional information is needed regarding energy dissipation of such weirs, since due to the folded weir crest, a three-dimensional flow field is generated, yielding more complex overflow and energy dissipation processes. In this study, CFD simulations of labyrinth weirs were conducted 1) to analyze the discharge coefficients for different discharges to compare the Cd values to literature data and 2) to analyze and improve energy dissipation downstream of the structure. All tests were performed for a structure at laboratory scale with a height of approx. P = 30.5 cm, a ratio of the total crest length to the total width of 4.7, a sidewall angle of 10° and a quarter-round weir crest shape. Tested headwater ratios were 0.089 ≤ HT/P ≤ 0.817. For numerical simulations, FLOW-3D Hydro was employed, solving the RANS equations with use of finite-volume method and RNG k-ε turbulence closure. In terms of discharge capacity, results were compared to data from physical model tests performed at the Utah Water Research Laboratory (Utah State University), emphasizing higher discharge coefficients from CFD than from the physical model. For upstream heads, some discrepancy in the range of ± 1 cm between literature, CFD and physical model tests was identified with a discussion regarding differences included in the manuscript. For downstream energy dissipation, variable tailwater depths were considered to analyze the formation and sweep-out of a hydraulic jump. It was found that even for high discharges, relatively low downstream Froude numbers were obtained due to high energy dissipation involved by the three-dimensional flow between the sidewalls. The effects of some additional energy dissipation devices, e.g. baffle blocks or end sills, were also analyzed. End sills were found to be non-effective. However, baffle blocks with different locations may improve energy dissipation downstream of labyrinth weirs.
Non-intrusive measuring techniques have attained a lot of interest in relation to both hydraulic modeling and prototype applications. Complimenting acoustic techniques, significant progress has been made for the development of new optical methods. Computer vision techniques can help to extract new information, e. g. high-resolution velocity and depth data, from videos captured with relatively inexpensive, consumer-grade cameras. Depth cameras are sensors providing information on the distance between the camera and observed features. Currently, sensors with different working principles are available. Stereoscopic systems reference physical image features (passive system) from two perspectives; in order to enhance the number of features and improve the results, a sensor may also estimate the disparity from a detected light to its original projection (active stereo system). In the current study, the RGB-D camera Intel RealSense D435, working on such stereo vision principle, is used in different, typical hydraulic modeling applications. All tests have been conducted at the Utah Water Research Laboratory. This paper will demonstrate the performance and limitations of the RGB-D sensor, installed as a single camera and as camera arrays, applied to 1) detect the free surface for highly turbulent, aerated hydraulic jumps, for free-falling jets and for an energy dissipation basin downstream of a labyrinth weir and 2) to monitor local scours upstream and downstream of a Piano Key Weir. It is intended to share the authors’ experiences with respect to camera settings, calibration, lightning conditions and other requirements in order to promote this useful, easily accessible device. Results will be compared to data from classical instrumentation and the literature. It will be shown that even in difficult application, e. g. the detection of a highly turbulent, fluctuating free-surface, the RGB-D sensor may yield similar accuracy as classical, intrusive probes.
Direct methods comprising limit and shakedown analysis is a branch of computational mechanics. It plays a significant role in mechanical and civil engineering design. The concept of direct method aims to determinate the ultimate load bearing capacity of structures beyond the elastic range. For practical problems, the direct methods lead to nonlinear convex optimization problems with a large number of variables and onstraints. If strength and loading are random quantities, the problem of shakedown analysis is considered as stochastic programming. This paper presents a method so called chance constrained programming, an effective method of stochastic programming, to solve shakedown analysis problem under random condition of strength. In this our investigation, the loading is deterministic, the strength is distributed as normal or lognormal variables.