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EN
Experimental tests and numerical simulations of a full-scale segment of a foot and cycle bridge made of polimer composites are presented in the paper. The analysed structure is made of sandwich panels, which consist of glass fibre reinforced polymer (GFRP) multi-layered laminate faces and a PET foam (obtained from recycling) core. The dimensions of the segment cross-section are the same as for the target footbridge; however, span length was reduced to 3 m. The experimental tests were conducted in a laboratory of the Faculty of Ocean Engineering and Ship Technology at Gdansk University of Technology. A single vertical force was generated by a hydraulic cylinder and was applied to the platform of the structure. The experimental tests were supported by numerical analyses performed in Femap with NX Nastran software by means of the finite element method (FEM). Results obtained in the computational model were compared with results from experiments. Thus, the numerical model was validated and the obtained conclusions were used in the next step of the design process of a composite footbridge with a span length of 14.5 m.
PL
W artykule skoncentrowano się na analizie procesów pękania w betonie z popiołem lotnym (fly ash – FA) z uwzględnieniem drugiego modelu pękania i określono parametr KIIc. Głównym celem badań było potwierdzenie zbieżności i określenie zakresu rozbieżności pomiędzy wynikami KIIc uzyskanymi na prasie MTS 810 i z zastosowaniem cyfrowej korelacji obrazu (Digital Image Correlation – DIC). Analiza wyników badań wykazała wyraźną zbieżność między wartościami uzyskanymi z obu urządzeń pomiarowych. Ponadto wyniki badań potwierdzają zależności z wcześniejszych doświadczeń dotyczących odporności na pękanie betonu zawierającego FA, przeprowadzonych przy pierwszym modelu pękania.
EN
The article focuses on analyzing the fracture processes in fly ash (FA) concrete taking into account the second model of cracking and the KIIc parameter was determined. Two measuring devices were used in the studies. The main goal of the studies was to confirm the convergence and determine the discrepancy ranges, between the KIIc results obtained on the MTS 810 press and the use of the Digital Iimage Correlation (DIC). The analysis of the obtained test results showed clear convergences between the values obtained from both measuring devices. Furthermore, the presented test results also confirm the values of previous experiments on fracture toughness of concrete containing FA conducted at the first model of cracking.
EN
In the article, a validation module, being a component of an integrated system supporting routing in software defined networks (SDNRoute), is proposed and thoroughly examined. The module allows for the verification of the results provided by the optimization module before these results are deployed in the production network. Routing policies are validated for their impact on the network quality parameters and against the threat of overloading (congestion).
EN
The process of individualizing personal protective equipment (PPE) is aimed at achievingoptimal fit to the user’s body, thus maximizing comfort, especially when PPE is applied in critical conditions. The aim of the research was to confirm the possibility of implementing PPE in rea industrial conditions and to estimate the comfort of use in real conditions of use. In order to perform the last stage of the personalization procedure for firefighter suits, process qualification was carried out in an industrial environment, and the firefighter’s PPE fabricated was validated under real conditions of firefighters’ activities. The effect of implementation of the individualization procedure confirmed optimal fitting of the PPE to the individual user’s body and allowed for improvement of the comfort of use.
PL
Przedmiotem publikacji było przedstawienie etapu procesu walidacji (kwalifikacji procesowej) opracowanej procedury w zakresie niestandardowej odzieży produkowanej w warunkach przemysłowych. Dla zrealizowania tego procesu w warunkach przemysłowych wytworzono partię prototypową, 6 kompletów zindywidualizowanych trzyczęściowych ubrań specjalnych dla funkcjonariuszy Straży Pożarnej dla potrzeb kwalifikacji procesowej (zmieniając producenta i typ ubrania poddawanego indywidualizacji) i poddano je badaniom użytkowym w warunkach rzeczywistych. Pozytywny wynik walidacji (PQ) partii prototypowej ubrań w badaniach użytkowych przeprowadzonych w warunkach rzeczywistych, pozwolił na wdrożenie opracowanej procedury, poprzedzone przeprowadzeniem szkoleń w zakładach produkcyjnych, publiczne udostępnienie informacji na stronie internetowej instytutu ITB „MORATEX”, „Procedury indywidualizacji konstrukcji zaawansowanej odzieży ochronnej dla osób pracujących w środowisku o wysokim stopniu zagrożenia zdrowia i życia, posiadającej zapisy dotyczące ochrony danych osobowych i zapisy dotyczące procesu skanowania 3D z wykorzystaniem wyników tego procesu do wytwarzania zindywidualizowanych ubrań w procesie produkcji przemysłowej”.
EN
In the designing of advanced personal protection equipment, the problem related to the continuous loss of properties associated with functionality and safety over the course of its use, storage and cleaning cycles is rarely noticed. Products and their technical characteristics are applied for the conformity assessment process, which does not take into account the risk of the reduction of safety parameters. As part of the research conducted, we established the influence of factors arising from use and cleaning cycles on the reduction of physico-mechanical parameters describing critical requirements associated with the safety and functionality of special clothing for firefighters. The scope of the research covered evaluation of the influence of atmospheric factors over the course of a period including three seasons (spring, summer and autumn) and of cleaning cycles (20 cycles of washing in water at 60°C, according to PN-EN ISO 6330:2012, distributed proportionally over three seasons of the year, with the use of commercial, commonly used washing powder) on the change in the level of parameters characterising special clothing for firefighters.
PL
W ramach prowadzonych prac badawczych określono wpływ czynników wynikających z użytkowania oraz procesów konserwacji na obniżenie parametrów fizykomechanicznych opisujących krytyczne wymagania związane z bezpieczeństwem oraz funkcjonalnością ubrań specjalnych dla funkcjonariuszy straży pożarnej różniących się składem surowcowym tkaniny wierzchniej oraz konstrukcją. Zakres badań obejmował ocenę wpływu czynników atmosferycznych w okresie obejmującym trzy pory roku (wiosna, lato, jesień) oraz procesu konserwacji (20 cykli prania wodnego wg PN-EN ISO 6330:2012 w temperaturze 60°C, rozłożonego proporcjonalnie na trzy pory roku, z wykorzystaniem komercyjnego, powszechnie używanego, proszku do prania) na zmianę poziomów parametrów charakteryzujących ubrania specjalne dla funkcjonariuszy straży pożarnej.
EN
Simplifications used in simulation program codes require the use of substitute parameters in the material databases (also called apparent or substitutive). On the one hand, they formally fit into the records used in the heat flow model, porosity, properties etc. and on the other hand they should be determined in conditions most similar to the real casting-mould system. The article presents results of a research on thermophysical parameters of gypsum mould used for precision casting moulds. Experiments were carried out on a cylindrical mould made of Plasticast gypsum, in which the heat source was a cylinder filled with liquid aluminium alloy of the temperature of 655°C. Energetic validation was carried out by using the NovaFlow&Solid ver. 6.3 simulation code. As a result of validation tests, substitute thermophysical parameters of gypsum were determined. For determined parameters, best-fit of solidification time from the experiment and simulation was obtained and the curves of gypsum mass heating were satisfactorily recreate.
EN
The aim of this paper was to determine the differences in the designed and manufactured model of a suspension. A set of key parameters was compared, including camber and toe in angles and their change w.r.t wheel travel, as well as the motion ratio. It also focused on the possibility of accurately determining the suspension system kinematics using affordable measuring devices available on the market. First, the design process, main goals and project assumptions were briefly described. Next, the CAD model and manufacturing process was presented. Finally, the measurements of both computer and real model were performed. The obtained results were compared and a significant difference between models was observed. The reason of such variation could not be determined unambiguously, as there were numerous factors that could potentially influence the results. Moreover, it was proven that accurate determination of kinematics is impossible using the given set of measuring devices.
8
Content available remote Evaluation of leakage through labyrinth seals with analytical models
EN
Secondary flows in turbomachinery highly affect the overall efficiency and rotorstability. A prime example of such a phenomenon are leakage flows. Despite their complexity, they can often be estimated with simple semi-empirical formulae, solved with hand calculations.Such an approach is much more cost and time effective during the design process. The formula econsists of a carry-over coefficient and a discharge coefficient elements. To evaluate the leakage properly, an adequate model of the carry-over coefficient has to be developed. This paper presents how the flow conditions and the cavity geometry changes in a straight through labyrinth sea laffect the amount of leakage. The effect of the number of teeth, the gap size, the Reynolds number and the pressure ratio are considered. The data to validate the results was obtained from an in-house experiment, where a vast number of cases was tested. Additionally, the study was supported by a two-dimensional steady-state CFD study. Eleven analytical models, including both very simple as well as more sophisticated methods, were solved according to the experimental case and compared. Six different seal configurations were examined. They included straight through seals with two and three straight knives for various gap sizes.The comparison highlighted differences in the results for models – a certain group presented underestimated results. However, another group of models – presented an excellent agreement with the experimental data. Based on this study, a group of models representing the results within the 10% uncertainty band was selected.
PL
W artykule zaproponowano oraz szczegółowo przebadano moduł walidatora stanowiący składową systemu obsługi trasowania (rutingu) ruchu w sieciach sterowanych programowo (SDNRoute). Moduł pozwala na weryfikację wyników działania modułu optymalizacji przed ich wdrożeniem do sieci produkcyjnej. Polityki rutingu walidowane są pod kątem wpływu na parametry jakościowe sieci oraz możliwość występowania przeciążeń.
EN
In the article, a validator module, being a component of an integrated system supporting routing in software defined networks (SDNRoute), is proposed and thoroughly examined. The module allows for the verification of the results of the optimization module before they are deployed in the production network. Routing policies are validated for their impact on the network quality parameters and the threat of overloading.
PL
Zasadniczy aspekt uczenia maszynowego stanowi ocena jakości zbudowanych modeli. Niezbędne zatem staje się staranne zaplanowanie eksperymentów. Potrzebne jest zrozumienie skutków potencjalnych błędów i niedopatrzeń. W artykule przedstawiono techniki, które mogą zostać wykorzystane w eksperymencie uczenia maszynowego. Opisano między innymi walidację prostą i krzyżową – z uwzględnieniem wyboru modelu – oraz podział czasowy. Przedstawiono wady i zalety wymienionych technik, uwzględniające między innymi rozmiar wejściowej bazy czy typ danych.
EN
The key aspect of machine learning is the model performance evaluation. Therefore, it is necessary to carefully plan the experiments. There is a need to understand the consequences of potential mistakes or omissions. This paper presents various techniques that can be used in a machine learning experiment. Simple split and cross validation – with or without model selection – as well as time split have been described. The advantages and disadvantages of these techniques have been presented – for example in terms of input database size or data type.
11
PL
Przedstawiono wyniki analizy własności energetycznych modelu wózka inwalidzkiego dźwigniowego ręcznego. Zastosowano techniki modelowania, symulacji i walidacji modelu. Parametry modelu zidentyfikowano na podstawie założeń technicznych oraz identyfikacji dynamicznej. Zbiór danych pomiarowych podzielono na dane treningowe i testujące. W identyfikacji dynamicznej momentu obrotowego hamulca oraz stopnia przełożenia kinematycznego przekładni redukcyjnych wykorzystano dane treningowe. Poprawność działania modelu sprawdzono na danych testujących. Model zaimplementowano w środowisku Matlab-Simulink. Jako wyniki pracy przedstawiono charakterystyki sprawności energetycznej napędu wózka dźwigniowego. Przedstawiono oraz udowodniono tezę, że opracowany model generuje przebiegi zmiennych stanu w sposób zgodny z otrzymywanymi wynikami pomiarów.
EN
This study presents the results of the analysis of the energy properties of a manual wheelchair model. Modeling, simulation and validation techniques were used. Parameters of the model were identified on the technical assumptions and dynamic identification. The measurement data has been divided into training and testing data. The training data were used for dynamic identification of the brake torque and the kinematic transmission ratio of the reduction gears. The testing data were used to check the accuracy of the model. The model has been implemented in the Matlab-Simulink environment. The energy efficiency characteristics of the lever drive wheelchair propulsion were presented as results of the work. The study includes the following research stages: (1) Execution of a series of measurements in the research environment, (2) Developing a nomnal and mathematical model of the stand (3) Identification of the model parameters (4) Implementation of the model in a programming environment (5) Model verification and validation (6) Carrying out the calculations of energy parameters including instantaneous efficiency and energetic efficiency of the work cycle. The study presents and proves the thesis that the developed model generates the course of state variables in a manner consistent with the obtained measurements results.
PL
Urządzenia pozwalające poddawać próbkę procesowi pirolizy w precyzyjnie określonych warunkach to pirolizery. Mogą one być łączone z różnymi aparatami, takimi jak chromatografy gazowe (z detektorami FID), spektrometry masowe oraz izotopowe spektrometry masowe. Zestawy GC-IRMS pozwalają na uzyskanie wartości δ13C poszczególnych związków z mieszaniny bez konieczności fizycznego jej rozdziału (rozdział następuje dzięki kolumnie chromatograficznej). Połączenie zestawu GC-IRMS z pirolizerem w układzie on-line pozwala na określanie składu izotopowego produktu pirolizy, a w zasadzie poszczególnych związków chemicznych produktu pirolizy. Praca przedstawia wyniki analiz produktów pirolizy próbki łupku sylurskiego. Otrzymywane produkty pirolizy to: metan, eten, etan, propylen, propan, 1-buten, n-butan oraz ditlenek węgla. Wykorzystana aparatura to spektrometr masowy Delta V Advantage firmy Thermo Scientific wraz z chromatografem Trace GC Ultra (kolumna kapilarna HP-PLOT Q, 30 m) i pirolizerem Pyroprobe 6150 (temperatura pirolizy 1000C, izoterma 30 sekund). Układ połączony on-line za pośrednictwem ConFlo IV. Metodyka Py-GC-IRMS oznaczeń składu izotopowego węgla gazowych produktów pirolizy została skalibrowana i sprawdzona poprzez ocenę powtarzalności i liniowości. Charakter oznaczeń składu izotopowego nie pozwala na określenie: granicy oznaczalności, granicy wykrywalności oraz obciążenia metody. Wszystkie wartości względnych odchyleń standardowych są poniżej pięciu procent (najniższe dla metanu: 0,6%), co jest wynikiem zadowalającym i potwierdzającym, że metoda daje powtarzalne rezultaty. Na podstawie przeprowadzonych badań uznano, że liniowość nie powinna być oceniana dla tej metody, a brak spełnienia kryterium liniowości nie świadczy o gorszych wynikach.
EN
Devices allowing to perform a pyrolysis process under precisely defined conditions are pyrolyzers. They can be combined with various apparatus such as gas chromatographs (with FID detector), mass spectrometers and isotopic mass spectrometers. The GC-IRMS kits allow to obtain δ13C values of individual compounds from the mixture without the necessity of physical separation (the separation takes place in the chromatographic column). The combination of the on-line GC-IRMS kit with the pyrolyzer allows to determine the isotopic composition of the pyrolysis product (the individual chemical compounds of the pyrolysis product). The paper presents the results of analyses of the Silurian shale pyrolysis products. The pyrolysis products obtained are: methane, ethene, ethane, propylene, propane, 1-butene, n-butane and carbon dioxide. The apparatus used is a Thermo Scientific Delta V Advantage mass spectrometer with a Trace GC Ultra chromatograph (HPPLOT/Q capillary column, 30 m) and Pyroprobe 6150 pyrolyzer (pyrolysis temperature 1000°C, isothermal 30 seconds). The Py-GC-IRMS methodology for determining the carbon isotopic composition of pyrolysis gas products has been calibrated and verified by evaluating repeatability and linearity. The nature of isotopic composition determinations does not allow to determine: the limit of quantification, the limit of detection and the method bias. All values of relative standard deviations are below five percent (the lowest for methane 0.6%), which is satisfactory and confirms that the method is reproducible. Linearity should not be evaluated for this method, and the lack of fulfillment of the linearity criterion does not indicate worse results.
EN
Solar radiation (Rs) is an essential input for estimating reference crop evapotranspiration, ETo. An accurate estimate of ETo is the first step involved in determining water demand of field crops. The objective of this study was to assess the accuracy of fifteen empirical solar radiations (Rs) models and determine its effects on ETo estimates for three sites in humid tropical environment (Abakaliki, Nsukka, and Awka). Meteorological data from the archives of NASA (from 1983 to 2005) was used to derive empirical constants (calibration) for the different models at each location while data from 2006 to 2015 was used for validation. The results showed an overall improvement when comparing measured Rs with Rs determined using original constants and Rs using the new constants. After calibration, the Swartman–Ogunlade (R2 = 0.97) and Chen 2 models (RMSE = 0.665 MJ∙m–2∙day–1) performed best while Chen 1 (R2 = 0.66) and Bristow–Campbell models (RMSE = 1.58 MJ∙m–2∙day–1) performed least in estimating Rs in Abakaliki. At the Nsukka station, Swartman–Ogunlade (R2 = 0.96) and Adeala models (RMSE = 0.785 MJ∙m–2∙day–1) performed best while Hargreaves–Samani (R2 = 0.64) and Chen 1 models (RMSE = 1.96 MJ∙m–2∙day–1) performed least in estimating Rs. Chen 2 (R2 = 0.98) and Swartman–Ogunlade models (RMSE = 0.43 MJ∙m–2∙day–1) performed best while Hargreaves–Samani (R2 = 0.68) and Chen 1 models (RMSE = 1.64 MJ∙m–2∙day–1) performed least in estimating Rs in Awka. For estimating ETo, Adeala (R2 =0.98) and Swartman–Ogunlade models (RMSE = 0.064 MJ∙m–2∙day–12 = 0.98) and Chen 2 models (RMSE = 0.43 MJ∙m–2∙day–1) performed best at Abakaliki while Angstrom–Prescott–Page (R2 = 0.96) and El-Sebaii models (RMSE = 0.0908 mm∙day–1) performed best at the Nsukka station.
PL
Promieniowanie słoneczne (Rs) stanowi istotny czynnik w trakcie określania ewapotranspiracji potencjalnej (ETo) terenów uprawnych. Dokładne oszacowanie ETo jest pierwszym etapem ustalania zapotrzebowania na wodę pól uprawnych. Celem tego badania była ocena dokładności piętnastu empirycznych modeli Rs i oznaczenie wpływu tego parametru na szacunki ewapotranspiracji w trzech stanowiskach wilgotnego środowiska tropikalnego (Abakaliki, Nsukka i Awka). Wykorzystano archiwalne dane meteorologiczne NASA z lat 1983 do 2003 do wyprowadzenia empirycznych stałych (kalibracja) dla różnych modeli w każdej z trzech lokalizacji, a dane z lat 2006 do 2015 posłużyło do oceny. Wyniki wskazują na większą zgodność mierzonego Rs i oszacowanych wartości promieniowania wyznaczonego z zastosowaniem nowych stałych. Po kalibracji modele Swartmana–Ogunladego (R2 = 0,97) i Chena 2 (RMSE = 0,665 MJ∙m–2∙d–1) dawały najlepsze wyniki, podczas gdy modele Chena 1 (R2 = 0,66) i Bristowa–Campbella (RMSE = 1,58 MJ∙m–2∙d–1) były najmniej dokładne w wyznaczaniu Rs w Akabaliki. W stacji Nsukka modele Swartmana–Ogunladego (R2 = 0,96) i Adeali (RMSE = 0,785 MJ∙m–2∙d–1) dawały najlepiej dostosowane wyniki oszacowania Rs, natomiast modele Hargreavesa–Samaniego (R2 = 0,64) i Chena 1 (RMSE = 1,96 MJ∙m–2∙d–1) najmniej. Modele Chena 2 (R2 = 0,98) i Swartmana–Ogunladego (RMSE = 0,43 MJ∙m–2∙d–1) okazały się najlepsze, a modele Hargreavesa–Samaniego (R2 = 0,68) i Chena 1 (RMSE = 1,64 MJ∙m–2∙d–1) – najgorsze w ustalaniu promieniowania w stanowisku Awka. W oszacowaniach ETo modele Adeali (R2 = 0,98) i Swartmana– Ogunladego (RMSE = 0.064 MJ∙m–2∙d–1) dawały najlepsze wyniki w przypadku danych ze stanowiska Awka, a modele Swartmana–Ogunladego (R2 = 0,98) i Chena 2 (RMSE = 0,43 MJ∙m–2∙d–1) okazały się najlepsze w przypadku danych ze stanowiska Abakaliki. W odniesieniu do stanowiska Nsukka najlepsze wyniki uzyskano, stosując modele Angstroma– Prescotta–Page’a (R2 = 0,96) i El-Sebaii (RMSE = 0,0908 mm∙d–1).
EN
The validation of the work of computational algorithms operating within the positioning system services under unusual measuring conditions is an important part of the entire system. Particularly noteworthy conditions are failures of reference stations forming the examined station network. The article evaluates the operation of the algorithm implemented to the POZGEO sub-service of the ASG-EUPOS system in the event of failure of reference stations used in the standard determination of the coordinates of the selected spatial point. The research material consisted of 117 days of continuous determination of the position of the selected spatial point using 1 hour of GPS static observations. Reports on the procedure of determining the position in the post-processing mode in POZGEO sub-service of static satellite observations were used to simulate the reduction of the number of tie vectors in coordinates’ determination method. The resistance of the automatic post-processing algorithm to failure of parts from the standard reference stations used was assessed.
EN
Because the industrial products have lifetimes, without failing, of up to millions of cycles, it is mandatory that the aerospace field puts into practice the accelerated testing techniques. The lifetime prediction methodology for industrial products presented in this paper was put into practice by performing accelerated reliability testing on an aerospace product (the pitch link of a helicopter). The results showed a significant reduction of the testing time and costs. One important aspect highlighted in this paper is the equivalence between accelerated reliability testing and the traditional reliability testing, by using the two fundamental principles of the accelerated experiments: first, the stresses applied must not alter the physical mechanism through which the defects are produced and second, the conservation of the distribution laws of the failure times. In this way, by equivalence of the accelerated experiments, the methodology contained in this paper was validated.
PL
Ponieważ okresy bezawaryjnego użytkowania produktów przemysłowych stosowanych w w branży lotniczej mogą wynosić nawet kilka milionów cykli, badanie niezawodności tych wyrobów wymaga zastosowania technik badania przyspieszonego. Metodologię prognozowania czasu pracy produktów przemysłowych przedstawioną w niniejszym artykule wykorzystano w badaniach przyspieszonych niezawodności dźwigni skoku wirnika nośnego helikoptera. Wyniki wykazały, że proponowana metoda pozwala na znaczną redukcję czasu i kosztów badania. Ważnym aspektem, podkreślonym w niniejszej pracy, jest równoważność przyspieszonych i tradycyjnych badań niezawodności, którą można uzyskać respektując dwie podstawowe zasady eksperymentów przyspieszonych: po pierwsze, zastosowane naprężenia nie mogą zmieniać fizycznego mechanizmu, który prowadzi do powstania wady, a po drugie, należy przestrzegać praw dotyczących rozkładu czasów uszkodzeń. Przeprowadzone badania potwierdzają poprawność proponowanej metody.
EN
Validation results of a theoretical model that describes the formation of bromate during ozonation of bromide-containing natural waters are presented. An axial dispersion model integrating the nonideal mixing, mass-transfer and a kinetic model that links ozone decomposition reactions from the Tomiyasu, Fukutomi and Gordon ozone decay model with direct and indirect bromide oxidation reactions, oxidation of natural organic matter and reactions of dissolved organics and aqueous bromine was verified. The model was successfully validated with results obtained both at a laboratory and a full scale. Its applicability to different water supply systems was approved.
EN
The paper presents the results of the conducted tests of torsional stiffness of the VOSCO S106 passenger car, as well as the validation process of these tests by means of numerical analyzes using the FEM finite element method. The most important element of the vehicle structure is the part of the spatial frame or the safety cage. Engine, brake system, fuel system and steering system, suspension as well as body and parts, their mounting nodes, hinges, locks, etc. are attached to the frame. The frame must therefore have adequate strength to protect the driver in the event of a tipover or impact. The frame is usually made of steel pipes with the prescribed dimensions and strength according to regulations. The torsional stiffness of the vehicle chassis has a significant influence on its driveability and therefore is an important parameter to measure. In this article, the torsional stiffness of the vehicle frame is calculated experimentally, which was then verified by finite element analysis (FEM) using the Altair HyperWorks program.
EN
This paper demonstrates kinematic analysis of multiple trailers on a tractor system for production logistics. The analysis concerned three different steering systems of the trailers: virtual clutch and drawbar system, conventional clutch and drawbar system, double Ackermann steering system. Designed kinematic models contain various variants of paths: turning at a constant value of the steering angle, changing the steering angle as a result of an approaching collision. Each of these variants also included driving in a straight line after a 90° turn. The validation of the developed kinematic model was done by using a real logistic train, which path was registered via aerial drone. For each of the developed kinematic models, a visualization of drive through the 90° turn was created.
EN
Objectives: A simple, rapid, selective, and sensitive high-performance liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed for the simultaneous determination of levocetirizine dihydrochloride and montelukast sodium in human plasma using fexofenadine hydrochloride as an internal standard. Method: Liquid–liquid extraction of both drugs and internal standard from plasma into ethyl acetate was used for sample preparation and analysis. Separation of both drugs and internal standard was achieved on an Inertsil ODS-3 (4.6 mm × 50 cm, dp 5 μm, particle size) column using an isocratic mobile phase of acetonitrile and 10 mM ammonium formate adjusted to pH 8 with 50 μL ammonium hydroxide in composition of 73:27 (v/v) at a flow rate of 0.7 mL/min. The LC–MS/MS was operated under the multiple reaction monitoring mode (MRM) using an electrospray ionization technique. Mass parameters were optimized to monitor transitions at m/z [M + H]+ 389.0 → 200.8 for levocetirizine dihydrochloride, m/z [M + H]+ 586.2 → 422.2 for montelukast sodium, and m/z [M + H]+ 502.2 → 466.0 for fexofenadine hydrochloride. Results: The method was found to be linear in the range of 1–500 ng/mL for both drugs. The intra-day and inter-day precision were in the range of 0.96–1.92% and 1.03–1.55%, respectively. Matrix effect was acceptable with %RSD < 15. Conclusion: The proposed method was validated and successfully applied for a pharmacokinetic study of both drugs in human plasma after oral administration of their pharmaceutical preparation.
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High-performance liquid chromatography (HPLC) is a widely used technique for the simultaneous detection and quantification of different drugs. The purpose of the current study was to develop a simple and cost-effective reversed-phase high-performance liquid chromatography (RP-HPLC) method for the simultaneous determination of tizanidine (TZN) HCl and meloxicam (MLX) in rabbit's plasma. Assay of TZN and MLX was performed after extraction of drug from plasma by liquid–liquid extraction technique using methanol and diethyl ether as protein precipitants. Isocratic elution was performed in a Kromasil® C18 column (dimension, 250 × 4.60 mm; particle size, 5 μm) with mobile phase consisting of methanol–water (8:2). Orthophosphoric acid was used to adjust the pH of the mobile phase 3.0, and detection was done at 228 nm. Flow rate was 0.8 mL/min with ambient temperature and average operating pressure of 1400 psig. Retention time of TZN was 2.612 min and that of MLX was 6.960 min with a resolution of 3.18. Both drugs showed satisfactory linearity in the range of 10 to 50 ng/mL with correlation coefficients (R2) of 0.9989 and 0.9972 for TZN and MLX, respectively. The developed method was validated successfully for linearity, system suitability, intra-day and inter-day accuracy, and precision, robustness, and specificity following International Conference on Harmonization (ICH) guidelines. Conclusively, a precise, stable, reproducible, economical, and suitable method for estimation of pharmacokinetic evaluation was developed and validated.
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