TY - JOUR A1 - Staat, Manfred T1 - Plastic collapse analysis of longitudinally flawed pipes and vessels N2 - Improved collapse loads of thick-walled, crack containing pipes and vessels are suggested. Very deep cracks have a residual strength which is better modelled by a global limit load. In all burst tests, the ductility of pressure vessel steels was sufficiently high whereby the burst pressure could be predicted by limit analysis with no need to apply fracture mechanics. The relative prognosis error increases however, for long and deep defects due to uncertainties of geometry and strength data. KW - Druckbehälter KW - Stahl KW - Druckbelastung KW - Druckbeanspruchung KW - Rohr KW - Rohrbruch KW - Druckbehälter KW - Stahl KW - Druckbelastung KW - Druckbeanspruchung KW - Rohrbruch KW - Fehlerstellen KW - pipes KW - vessels KW - load limit KW - burst tests KW - burst pressure KW - flaw Y1 - 2004 ER - TY - JOUR A1 - Staat, Manfred T1 - Cyclic plastic deformation tests to verify FEM-based shakedown analyses N2 - Fatigue analyses are conducted with the aim of verifying that thermal ratcheting is limited. To this end it is important to make a clear distintion between the shakedown range and the ratcheting range (continuing deformation). As part of an EU-supported research project, experiments were carried out using a 4-bar model. The experiment comprised a water-cooled internal tube, and three insulated heatable outer test bars. The system was subjected to alternating axial forces, superimposed with alternating temperatures at the outer bars. The test parameters were partly selected on the basis of previous shakedown analyses. During the test, temperatures and strains were measured as a function of time. The loads and the resulting stresses were confirmed on an ongoing basis during performance of the test, and after it. Different material models were applied for this incremental elasto-plastic analysis using the ANSYS program. The results of the simulation are used to verify the FEM-based shakedown analysis. KW - Materialermüdung KW - Einspielen KW - Materialermüdung KW - shakedown analyses KW - thermal ratcheting KW - fatigue analyses Y1 - 2001 ER - TY - JOUR A1 - Staat, Manfred T1 - Local and global collapse pressure of longitudinally flawed pipes and cylindrical vessels N2 - Limit loads can be calculated with the finite element method (FEM) for any component, defect geometry, and loading. FEM suggests that published long crack limit formulae for axial defects under-estimate the burst pressure for internal surface defects in thick pipes while limit loads are not conservative for deep cracks and for pressure loaded crack-faces. Very deep cracks have a residual strength, which is modelled by a global collapse load. These observations are combined to derive new analytical local and global collapse loads. The global collapse loads are close to FEM limit analyses for all crack dimensions. KW - Finite-Elemente-Methode KW - Grenzwertberechnung KW - Axialbelastung KW - FEM KW - Grenzwertberechnung KW - Axialbelastung KW - Traglastanalyse KW - Limit analysis KW - Global and local collapse KW - Axially cracked pipe KW - Pressure loaded crack-face Y1 - 2005 ER - TY - JOUR A1 - Staat, Manfred T1 - Direct finite element route for design-by-analysis of pressure components N2 - In the new European standard for unfired pressure vessels, EN 13445-3, there are two approaches for carrying out a Design-by-Analysis that cover both the stress categorization method (Annex C) and the direct route method (Annex B) for a check against global plastic deformation and against progressive plastic deformation. This paper presents the direct route in the language of limit and shakedown analysis. This approach leads to an optimization problem. Its solution with Finite Element Analysis is demonstrated for mechanical and thermal actions. One observation from the examples is that the so-called 3f (3Sm) criterion fails to be a reliable check against progressive plastic deformation. Precise conditions are given, which greatly restrict the applicability of the 3f criterion. KW - Einspielen KW - Plastizität KW - Deformation KW - Analytischer Zulaessigkeitsnachweis KW - Einspiel-Analyse KW - fortschreitende plastische Deformation KW - alternierend Verformbarkeit KW - Einspiel-Kriterium KW - Design-by-analysis KW - Shakedown analysis KW - Progressive plastic deformation KW - Alternating plasticity KW - Shakedown criterion Y1 - 2005 ER - TY - JOUR A1 - Staat, Manfred T1 - Shakedown and ratchetting under tension-torsion loadings: analysis and experiments N2 - Structural design analyses are conducted with the aim of verifying the exclusion of ratchetting. To this end it is important to make a clear distinction between the shakedown range and the ratchetting range. The performed experiment comprised a hollow tension specimen which was subjected to alternating axial forces, superimposed with constant moments. First, a series of uniaxial tests has been carried out in order to calibrate a bounded kinematic hardening rule. The load parameters have been selected on the basis of previous shakedown analyses with the PERMAS code using a kinematic hardening material model. It is shown that this shakedown analysis gives reasonable agreement between the experimental and the numerical results. A linear and a nonlinear kinematic hardening model of two-surface plasticity are compared in material shakedown analysis. KW - Einspielen KW - Einspielen KW - Ratchetting KW - Zug-Druck Belastung KW - shakedown KW - ratchetting KW - tension–torsion loading Y1 - 2003 ER - TY - JOUR A1 - Staat, Manfred T1 - Basis Reduction for the Shakedown Problem for Bounded Kinematic Hardening Material N2 - Limit and shakedown analysis are effective methods for assessing the load carrying capacity of a given structure. The elasto–plastic behavior of the structure subjected to loads varying in a given load domain is characterized by the shakedown load factor, defined as the maximum factor which satisfies the sufficient conditions stated in the corresponding static shakedown theorem. The finite element dicretization of the problem may lead to very large convex optimization. For the effective solution a basis reduction method has been developed that makes use of the special problem structure for perfectly plastic material. The paper proposes a modified basis reduction method for direct application to the two-surface plasticity model of bounded kinematic hardening material. The considered numerical examples show an enlargement of the load carrying capacity due to bounded hardening. KW - Finite-Elemente-Methode KW - Einspielen KW - Basis Reduktion KW - konvexe Optimierung KW - FEM KW - Druckgeräte KW - Basis reduction KW - Convex optimization KW - FEM KW - Shakedown analysis Y1 - 2000 ER - TY - JOUR A1 - Staat, Manfred T1 - LISA - a European project for FEM-based limit and shakedown analysis N2 - The load-carrying capacity or the safety against plastic limit states are the central questions in the design of structures and passive components in the apparatus engineering. A precise answer is most simply given by limit and shakedown analysis. These methods can be based on static and kinematic theorems for lower and upper bound analysis. Both may be formulated as optimization problems for finite element discretizations of structures. The problems of large-scale analysis and the extension towards realistic material modelling will be solved in a European research project. Limit and shakedown analyses are briefly demonstrated with illustrative examples. KW - Einspielen KW - Traglast KW - Finite-Elemente-Methode KW - Traglastanalyse KW - Einspielanalyse KW - FEM KW - limit analysis KW - shakedown analysis Y1 - 2001 ER - TY - JOUR A1 - Staat, Manfred T1 - Direct FEM Limit and Shakedown Analysis with Uncertain Data N2 - The structural reliability with respect to plastic collapse or to inadaptation is formulated on the basis of the lower bound limit and shakedown theorems. A direct definition of the limit state function is achieved which permits the use of the highly effective first order reliability methods (FORM) is achieved. The theorems are implemented into a general purpose FEM program in a way capable of large-scale analysis. The limit state function and its gradient are obtained from a mathematical optimization problem. This direct approach reduces considerably the necessary knowledge of uncertain technological input data, the computing time, and the numerical error, leading to highly effective and precise reliability analyses. KW - Finite-Elemente-Methode KW - Einspielen KW - FEM KW - Einspielanalyse KW - shakedown KW - limit load KW - reliability analysis KW - FEM KW - direct method Y1 - 2000 ER - TY - JOUR A1 - Staat, Manfred T1 - An extension strain type Mohr–Coulomb criterion JF - Rock mechanics and rock engineering N2 - Extension fractures are typical for the deformation under low or no confining pressure. They can be explained by a phenomenological extension strain failure criterion. In the past, a simple empirical criterion for fracture initiation in brittle rock has been developed. In this article, it is shown that the simple extension strain criterion makes unrealistic strength predictions in biaxial compression and tension. To overcome this major limitation, a new extension strain criterion is proposed by adding a weighted principal shear component to the simple criterion. The shear weight is chosen, such that the enriched extension strain criterion represents the same failure surface as the Mohr–Coulomb (MC) criterion. Thus, the MC criterion has been derived as an extension strain criterion predicting extension failure modes, which are unexpected in the classical understanding of the failure of cohesive-frictional materials. In progressive damage of rock, the most likely fracture direction is orthogonal to the maximum extension strain leading to dilatancy. The enriched extension strain criterion is proposed as a threshold surface for crack initiation CI and crack damage CD and as a failure surface at peak stress CP. Different from compressive loading, tensile loading requires only a limited number of critical cracks to cause failure. Therefore, for tensile stresses, the failure criteria must be modified somehow, possibly by a cut-off corresponding to the CI stress. Examples show that the enriched extension strain criterion predicts much lower volumes of damaged rock mass compared to the simple extension strain criterion. Y1 - 2021 U6 - http://dx.doi.org/10.1007/s00603-021-02608-7 SN - 1434-453X N1 - Corresponding author: Manfred Staat VL - 54 IS - 12 SP - 6207 EP - 6233 PB - Springer Nature CY - Cham ER - TY - JOUR A1 - Sildatke, Michael A1 - Karwanni, Hendrik A1 - Kraft, Bodo A1 - Zündorf, Albert T1 - A distributed microservice architecture pattern for the automated generation of information extraction pipelines JF - SN Computer Science N2 - Companies often build their businesses based on product information and therefore try to automate the process of information extraction (IE). Since the information source is usually heterogeneous and non-standardized, classic extract, transform, load techniques reach their limits. Hence, companies must implement the newest findings from research to tackle the challenges of process automation. They require a flexible and robust system that is extendable and ensures the optimal processing of the different document types. This paper provides a distributed microservice architecture pattern that enables the automated generation of IE pipelines. Since their optimal design is individual for each input document, the system ensures the ad-hoc generation of pipelines depending on specific document characteristics at runtime. Furthermore, it introduces the automated quality determination of each available pipeline and controls the integration of new microservices based on their impact on the business value. The introduced system enables fast prototyping of the newest approaches from research and supports companies in automating their IE processes. Based on the automated quality determination, it ensures that the generated pipelines always meet defined business requirements when they come into productive use. KW - Architectural design KW - Model-driven software engineering KW - Software and systems modeling KW - Enterprise information systems KW - Information extraction Y1 - 2023 U6 - http://dx.doi.org/10.1007/s42979-023-02256-4 SN - 2661-8907 N1 - Corresponding authors: Michael Sildatke, Hendrik Karwanni IS - 4, Article number: 833 PB - Springer Singapore CY - Singapore ER - TY - JOUR A1 - Seifarth, Volker A1 - Schehl, D. A1 - Linder, Peter A1 - Gossmann, Matthias A1 - Digel, Ilya A1 - Artmann, Gerhard A1 - Porst, Dariusz A1 - Preiß, C. A1 - Kayser, Peter A1 - Pack, O. A1 - Temiz Artmann, Aysegül T1 - Ureplace: development of a bioreactor for in vitro culturing of cell seeded tubular vessels on collagen scaffolds N2 - The demand of replacements for inoperable organs exceeds the amount of available organ transplants. Therefore, tissue engineering developed as a multidisciplinary field of research for autologous in-vitro organs. Such three dimensional tissue constructs request the application of a bioreactor. The UREPLACE bioreactor is used to grow cells on tubular collagen scaffolds OPTIMAIX Sponge 1 with a maximal length of 7 cm, in order to culture in vitro an adequate ureter replacement. With a rotating unit, (urothelial) cells can be placed homogeneously on the inner scaffold surface. Furthermore, a stimulation is combined with this bioreactor resulting in an orientation of muscle cells. These culturing methods request a precise control of several parameters and actuators. A combination of a LabBox and the suitable software LabVision is used to set and conduct parameters like rotation angles, velocities, pressures and other important cell culture values. The bioreactor was tested waterproof successfully. Furthermore, the temperature controlling was adjusted to 37 °C and the CO2 - concentration regulated to 5 %. Additionally, the pH step responses of several substances showed a perfect functioning of the designed flow chamber. All used software was tested and remained stable for several days. KW - Tissue Engineering KW - Bioreaktor KW - Organkultur KW - Harnleiter Y1 - 2011 ER - TY - JOUR A1 - Schüller-Ruhl, Aaron A1 - Dinstühler, Leonard A1 - Senger, Thorsten A1 - Bergfeld, Stefan A1 - Ingenhag, Christian A1 - Fleischhaker, Robert ED - Mackenzie, Jacob T1 - Direct fabrication of arbitrary phase masks in optical glass via ultra-short pulsed laser writing of refractive index modifications JF - Applied Physics B N2 - We study the possibility to fabricate an arbitrary phase mask in a one-step laser-writing process inside the volume of an optical glass substrate. We derive the phase mask from a Gerchberg–Saxton-type algorithm as an array and create each individual phase shift using a refractive index modification of variable axial length. We realize the variable axial length by superimposing refractive index modifications induced by an ultra-short pulsed laser at different focusing depth. Each single modification is created by applying 1000 pulses with 15 μJ pulse energy at 100 kHz to a fixed spot of 25 μm diameter and the focus is then shifted axially in steps of 10 μm. With several proof-of-principle examples, we show the feasibility of our method. In particular, we identify the induced refractive index change to about a value of Δn=1.5⋅10−3. We also determine our current limitations by calculating the overlap in the form of a scalar product and we discuss possible future improvements. Y1 - 2022 U6 - http://dx.doi.org/10.1007/s00340-022-07928-2 SN - 1432-0649 (Online) SN - 0946-2171 (Print) N1 - Corresponding author: Robert Fleischhaker VL - 128 IS - Article number: 208 SP - 1 EP - 11 PB - Springer CY - Berlin ER - TY - JOUR A1 - Röthenbacher, Annika A1 - Cesari, Matteo A1 - Doppler, Christopher E.J. A1 - Okkels, Niels A1 - Willemsen, Nele A1 - Sembowski, Nora A1 - Seger, Aline A1 - Lindner, Marie A1 - Brune, Corinna A1 - Stefani, Ambra A1 - Högl, Birgit A1 - Bialonski, Stephan A1 - Borghammer, Per A1 - Fink, Gereon R. A1 - Schober, Martin A1 - Sommerauer, Michael T1 - RBDtector: an open-source software to detect REM sleep without atonia according to visual scoring criteria JF - Scientific Reports N2 - REM sleep without atonia (RSWA) is a key feature for the diagnosis of rapid eye movement (REM) sleep behaviour disorder (RBD). We introduce RBDtector, a novel open-source software to score RSWA according to established SINBAR visual scoring criteria. We assessed muscle activity of the mentalis, flexor digitorum superficialis (FDS), and anterior tibialis (AT) muscles. RSWA was scored manually as tonic, phasic, and any activity by human scorers as well as using RBDtector in 20 subjects. Subsequently, 174 subjects (72 without RBD and 102 with RBD) were analysed with RBDtector to show the algorithm’s applicability. We additionally compared RBDtector estimates to a previously published dataset. RBDtector showed robust conformity with human scorings. The highest congruency was achieved for phasic and any activity of the FDS. Combining mentalis any and FDS any, RBDtector identified RBD subjects with 100% specificity and 96% sensitivity applying a cut-off of 20.6%. Comparable performance was obtained without manual artefact removal. RBD subjects also showed muscle bouts of higher amplitude and longer duration. RBDtector provides estimates of tonic, phasic, and any activity comparable to human scorings. RBDtector, which is freely available, can help identify RBD subjects and provides reliable RSWA metrics. Y1 - 2022 U6 - http://dx.doi.org/10.1038/s41598-022-25163-9 SN - 2045-2322 VL - 12 IS - Article number: 20886 SP - 1 EP - 14 PB - Springer Nature CY - London ER - TY - JOUR A1 - Richter, Charlotte A1 - Braunstein, Björn A1 - Stäudle, Benjamin A1 - Attias, Julia A1 - Süss, Alexander A1 - Weber, Tobias A1 - Mileva, Katya N. A1 - Rittweger, Jörn A1 - Green, David A. A1 - Albracht, Kirsten T1 - Gastrocnemius medialis contractile behavior during running differs between simulated Lunar and Martian gravities JF - Scientific reports N2 - The international partnership of space agencies has agreed to proceed forward to the Moon sustainably. Activities on the Lunar surface (0.16 g) will allow crewmembers to advance the exploration skills needed when expanding human presence to Mars (0.38 g). Whilst data from actual hypogravity activities are limited to the Apollo missions, simulation studies have indicated that ground reaction forces, mechanical work, muscle activation, and joint angles decrease with declining gravity level. However, these alterations in locomotion biomechanics do not necessarily scale to the gravity level, the reduction in gastrocnemius medialis activation even appears to level off around 0.2 g, while muscle activation pattern remains similar. Thus, it is difficult to predict whether gastrocnemius medialis contractile behavior during running on Moon will basically be the same as on Mars. Therefore, this study investigated lower limb joint kinematics and gastrocnemius medialis behavior during running at 1 g, simulated Martian gravity, and simulated Lunar gravity on the vertical treadmill facility. The results indicate that hypogravity-induced alterations in joint kinematics and contractile behavior still persist between simulated running on the Moon and Mars. This contrasts with the concept of a ceiling effect and should be carefully considered when evaluating exercise prescriptions and the transferability of locomotion practiced in Lunar gravity to Martian gravity. KW - Bone quality and biomechanics KW - Environmental impact KW - Skeletal muscle KW - Tendons KW - Ultrasound Y1 - 2021 U6 - http://dx.doi.org/10.1038/s41598-021-00527-9 SN - 2045-2322 N1 - Corresponding author: Charlotte Richter VL - 11 IS - Article number: 22555 PB - Springer Nature CY - London ER - TY - JOUR A1 - Richter, Charlotte A1 - Braunstein, Bjoern A1 - Staeudle, Benjamin A1 - Attias, Julia A1 - Suess, Alexander A1 - Weber, Tobias A1 - Mileva, Katya N. A1 - Rittweger, Joern A1 - Green, David A. A1 - Albracht, Kirsten T1 - Contractile behavior of the gastrocnemius medialis muscle during running in simulated hypogravity JF - npj Microgravity N2 - Vigorous exercise countermeasures in microgravity can largely attenuate muscular degeneration, albeit the extent of applied loading is key for the extent of muscle wasting. Running on the International Space Station is usually performed with maximum loads of 70% body weight (0.7 g). However, it has not been investigated how the reduced musculoskeletal loading affects muscle and series elastic element dynamics, and thereby force and power generation. Therefore, this study examined the effects of running on the vertical treadmill facility, a ground-based analog, at simulated 0.7 g on gastrocnemius medialis contractile behavior. The results reveal that fascicle−series elastic element behavior differs between simulated hypogravity and 1 g running. Whilst shorter peak series elastic element lengths at simulated 0.7 g appear to be the result of lower muscular and gravitational forces acting on it, increased fascicle lengths and decreased velocities could not be anticipated, but may inform the development of optimized running training in hypogravity. However, whether the alterations in contractile behavior precipitate musculoskeletal degeneration warrants further study. Y1 - 2021 U6 - http://dx.doi.org/10.1038/s41526-021-00155-7 SN - 2373-8065 N1 - Corresponding author: Charlotte Richter VL - 7 IS - Article number: 32 PB - Springer Nature CY - New York ER - TY - JOUR A1 - Preiß, C. A1 - Linder, Peter A1 - Wendt, K. A1 - Krystek, M. A1 - Digel, Ilya A1 - Gossmann, Matthias A1 - Temiz Artmann, Aysegül A1 - Porst, Dariusz A1 - Kayser, Peter A1 - Bassam, Rasha A1 - Artmann, Gerhard T1 - Engineering technology for plant physiology and plant stress research N2 - Plant physiology and plant stress: Plant physiology will be much more important for human mankind because of yield and cultivation limits of crops determined by their resistance to stress. To assess and counteract various stress factors it is necessary to conduct plant research to gain information and results on plant physiology. KW - Pflanzenphysiologie KW - Pflanzenstress KW - Pflanzenscanner KW - plant stress KW - plant scanner Y1 - 2011 ER - TY - JOUR A1 - Pfaff, Raphael A1 - Enning, Manfred A1 - Sutter, Stefan T1 - A risk‑based approach to automatic brake tests for rail freight service: incident analysis and realisation concept JF - SN Applied Sciences N2 - This study reviews the practice of brake tests in freight railways, which is time consuming and not suitable to detect certain failure types. Public incident reports are analysed to derive a reasonable brake test hardware and communication architecture, which aims to provide automatic brake tests at lower cost than current solutions. The proposed solutions relies exclusively on brake pipe and brake cylinder pressure sensors, a brake release position switch as well as radio communication via standard protocols. The approach is embedded in the Wagon 4.0 concept, which is a holistic approach to a smart freight wagon. The reduction of manual processes yields a strong incentive due to high savings in manual labour and increased productivity. KW - Freight rail KW - Brake test KW - Incident analysis KW - Train composition KW - Brake set-up Y1 - 2022 U6 - http://dx.doi.org/10.1007/s42452-022-05007-x SN - 2523-3971 N1 - Corresponding author: Raphael Pfaff VL - 4 IS - 4 SP - 1 EP - 14 PB - Springer CY - Cham ER - TY - JOUR A1 - Oliveira, Danilo A. A1 - Molinnus, Denise A1 - Beging, Stefan A1 - Siqueira Jr, José R. A1 - Schöning, Michael Josef T1 - Biosensor Based on Self-Assembled Films of Graphene Oxide and Polyaniline Using a Field-Effect Device Platform JF - physica status solidi (a) applications and materials science N2 - A new functionalization method to modify capacitive electrolyte–insulator–semiconductor (EIS) structures with nanofilms is presented. Layers of polyallylamine hydrochloride (PAH) and graphene oxide (GO) with the compound polyaniline:poly(2-acrylamido-2-methyl-1-propanesulfonic acid) (PANI:PAAMPSA) are deposited onto a p-Si/SiO2 chip using the layer-by-layer technique (LbL). Two different enzymes (urease and penicillinase) are separately immobilized on top of a five-bilayer stack of the PAH:GO/PANI:PAAMPSA-modified EIS chip, forming a biosensor for detection of urea and penicillin, respectively. Electrochemical characterization is performed by constant capacitance (ConCap) measurements, and the film morphology is characterized by atomic force microscopy (AFM) and scanning electron microscopy (SEM). An increase in the average sensitivity of the modified biosensors (EIS–nanofilm–enzyme) of around 15% is found in relation to sensors, only carrying the enzyme but without the nanofilm (EIS–enzyme). In this sense, the nanofilm acts as a stable bioreceptor onto the EIS chip improving the output signal in terms of sensitivity and stability. KW - capacitive electrolyte–insulator–semiconductor sensors KW - graphene oxide KW - layer-by-layer technique KW - nanomaterials KW - polyaniline Y1 - 2021 U6 - http://dx.doi.org/10.1002/pssa.202000747 SN - 1862-6319 N1 - Corresponding author: José R. Siqueira Jr & Michael J. Schöning VL - 218 IS - 13 SP - 1 EP - 9 PB - Wiley-VCH CY - Weinheim ER - TY - JOUR A1 - Möhren, Felix A1 - Bergmann, Ole A1 - Janser, Frank A1 - Braun, Carsten T1 - On the influence of elasticity on propeller performance: a parametric study JF - CEAS Aeronautical Journal N2 - The aerodynamic performance of propellers strongly depends on their geometry and, consequently, on aeroelastic deformations. Knowledge of the extent of the impact is crucial for overall aircraft performance. An integrated simulation environment for steady aeroelastic propeller simulations is presented. The simulation environment is applied to determine the impact of elastic deformations on the aerodynamic propeller performance. The aerodynamic module includes a blade element momentum approach to calculate aerodynamic loads. The structural module is based on finite beam elements, according to Timoshenko theory, including moderate deflections. Several fixed-pitch propellers with thin-walled cross sections made of both isotropic and non-isotropic materials are investigated. The essential parameters are varied: diameter, disc loading, sweep, material, rotational, and flight velocity. The relative change of thrust between rigid and elastic blades quantifies the impact of propeller elasticity. Swept propellers of large diameters or low disc loadings can decrease the thrust significantly. High flight velocities and low material stiffness amplify this tendency. Performance calculations without consideration of propeller elasticity can lead to decreased efficiency. To avoid cost- and time-intense redesigns, propeller elasticity should be considered for swept planforms and low disc loadings. KW - Propeller KW - Finite element method KW - Blade element method KW - Propeller elasticity KW - Aeroelasticity Y1 - 2023 U6 - http://dx.doi.org/10.1007/s13272-023-00649-y SN - 1869-5590 (Online) SN - 1869-5582 (Print) N1 - Corresponding author: Felix Möhren VL - 14 SP - 311 EP - 323 PB - Springer Nature CY - Berlin ER - TY - JOUR A1 - Monakhova, Yulia A1 - Diehl, Bernd W. K. T1 - A step towards optimization of the qNMR workflow: proficiency testing exercise at an GxP-accredited laboratory JF - Applied Magnetic Resonance N2 - Quantitative nuclear magnetic resonance (qNMR) is considered as a powerful tool for multicomponent mixture analysis as well as for the purity determination of single compounds. Special attention is currently paid to the training of operators and study directors involved in qNMR testing. To assure that only qualified personnel are used for sample preparation at our GxP-accredited laboratory, weighing test was proposed. Sixteen participants performed six-fold weighing of the binary mixture of dibutylated hydroxytoluene (BHT) and 1,2,4,5-tetrachloro-3-nitrobenzene (TCNB). To evaluate the quality of data analysis, all spectra were evaluated manually by a qNMR expert and using in-house developed automated routine. The results revealed that mean values are comparable and both evaluation approaches are free of systematic error. However, automated evaluation resulted in an approximately 20% increase in precision. The same findings were revealed for qNMR analysis of 32 compounds used in pharmaceutical industry. Weighing test by six-fold determination in binary mixtures and automated qNMR methodology can be recommended as efficient tools for evaluating staff proficiency. The automated qNMR method significantly increases throughput and precision of qNMR for routine measurements and extends application scope of qNMR. Y1 - 2021 U6 - http://dx.doi.org/10.1007/s00723-021-01324-3 SN - 1613-7507 N1 - Corresponding author: Yulia Monakhova VL - 52 SP - 581 EP - 593 PB - Springer Nature CY - Wien ER -