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Keywords = API 5L X-65

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16 pages, 13876 KB  
Article
Effect of Electrochemical Hydrogen Charging on the Notch Tensile Properties of Natural Gas Transportation Pipeline Steel with Electroless-Plated Coatings and Their Adhesiveness Characterization
by Ladislav Falat, Lucia Čiripová, Viktor Puchý, Ivan Petrišinec and Róbert Džunda
Metals 2025, 15(9), 1032; https://doi.org/10.3390/met15091032 - 18 Sep 2025
Viewed by 300
Abstract
Traditional natural gas transportation pipeline steels, such as API 5L X42 grade and the higher grades, are currently receiving a lot of attention in terms of their potential implementation in hydrogen transmission infrastructure. However, the microstructural constitution of steels with a ferrite phase [...] Read more.
Traditional natural gas transportation pipeline steels, such as API 5L X42 grade and the higher grades, are currently receiving a lot of attention in terms of their potential implementation in hydrogen transmission infrastructure. However, the microstructural constitution of steels with a ferrite phase and the presence of welds, with their non-polyhedral “sharp” microstructures acting as structural notches, make these steels prone to hydrogen embrittlement (HE). In this work, the notch tensile properties of copper- or nickel–phosphorus-coated API 5L X42 grade pipeline steel were studied in both the non-hydrogenated and electrochemically hydrogen-charged conditions in order to estimate anticipated protective effects of the coatings against HE. Both the Cu and Ni–P coatings were produced using conventional coating solutions for electroless plating. To study the material systems’ HE sensitivity, electrochemical hydrogenation of cylindrical, circumferentially V-notched tensile specimens was performed in a solution of hydrochloric acid with the addition of hydrazine sulfate. Notch tensile tests were carried out for the uncoated steel, Cu-coated steel, and Ni–P-coated steel at room temperature. The HE resistance was evaluated by determination of the hydrogen embrittlement index (HEI) in terms of relative changes in notch tensile properties related to the non-hydrogenated and hydrogen-charged material conditions. The results showed that pure electroless deposition of both coatings induced some degree of HE, likely due to the presence of hydrogen ions in the coating solutions used and the lower surface quality of the coatings. However, after the electrochemical hydrogen charging, the coated systems showed improved HE resistance (lower HEIRA values) compared with the uncoated material. This behavior was accompanied by the hydrogen-induced coatings’ deterioration, including the occurrence of superficial defects, such as bubbling, flocks, and spallation. Thus, further continuing research is needed to improve the coatings’ surface quality and long-term durability, including examination of their performance under pressurized hydrogen gas charging conditions. Full article
(This article belongs to the Special Issue Hydrogen Embrittlement of Metals: Behaviors and Mechanisms)
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17 pages, 7068 KB  
Article
Effect of Ni-Based Buttering on the Microstructure and Mechanical Properties of a Bimetallic API 5L X-52/AISI 316L-Si Welded Joint
by Luis Ángel Lázaro-Lobato, Gildardo Gutiérrez-Vargas, Francisco Fernando Curiel-López, Víctor Hugo López-Morelos, María del Carmen Ramírez-López, Julio Cesar Verduzco-Juárez and José Jaime Taha-Tijerina
Metals 2025, 15(8), 824; https://doi.org/10.3390/met15080824 - 23 Jul 2025
Viewed by 549
Abstract
The microstructure and mechanical properties of welded joints of API 5L X-52 steel plates cladded with AISI 316L-Si austenitic stainless steel were evaluated. The gas metal arc welding process with pulsed arc (GMAW-P) and controlled arc oscillation were used to join the bimetallic [...] Read more.
The microstructure and mechanical properties of welded joints of API 5L X-52 steel plates cladded with AISI 316L-Si austenitic stainless steel were evaluated. The gas metal arc welding process with pulsed arc (GMAW-P) and controlled arc oscillation were used to join the bimetallic plates. After the root welding pass, buttering with an ERNiCrMo-3 filler wire was performed and multi-pass welding followed using an ER70S-6 electrode. The results obtained by optical and scanning electron microscopy indicated that the shielding atmosphere, welding parameters, and electric arc oscillation enabled good arc stability and proper molten metal transfer from the filler wire to the sidewalls of the joint during welding. Vickers microhardness (HV) and tensile tests were performed for correlating microstructural and mechanical properties. The mixture of ERNiCrMo-3 and ER70S-6 filler materials presented fine interlocked grains with a honeycomb network shape of the Ni–Fe mixture with Ni-rich grain boundaries and a cellular-dendritic and equiaxed solidification. Variation of microhardness at the weld metal (WM) in the middle zone of the bimetallic welded joints (BWJ) is associated with the manipulation of the welding parameters, promoting precipitation of carbides in the austenitic matrix and formation of martensite during solidification of the weld pool and cooling of the WM. The BWJ exhibited a mechanical strength of 380 and 520 MPa for the yield stress and ultimate tensile strength, respectively. These values are close to those of the as-received API 5L X-52 steel. Full article
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17 pages, 6934 KB  
Article
Fatigue Life Anisotropy of API 5L X42 Pipeline Steel in Axial Force-Controlled Tests
by Manuel A. Beltrán-Zúñiga, Jorge L. González-Velázquez, Diego I. Rivas-López, Héctor J. Dorantes-Rosales, Carlos Ferreira-Palma, Felipe Hernández-Santiago and Fernando Larios-Flores
Materials 2025, 18(11), 2484; https://doi.org/10.3390/ma18112484 - 26 May 2025
Cited by 1 | Viewed by 526
Abstract
Fatigue endurance anisotropic behavior was evaluated for an API 5L X42 pipeline steel through axial force-controlled fatigue tests amongst Longitudinal, Diagonal, and Circumferential directions. This study shows that fatigue life anisotropy is mainly controlled by pearlite banding degree (Ai) and [...] Read more.
Fatigue endurance anisotropic behavior was evaluated for an API 5L X42 pipeline steel through axial force-controlled fatigue tests amongst Longitudinal, Diagonal, and Circumferential directions. This study shows that fatigue life anisotropy is mainly controlled by pearlite banding degree (Ai) and ferritic grain orientation (Ω12). Also, it is foreseen that the observed behavior can be related to the dislocation arrays generated by the cyclic loading in relation to microstructure orientation, and the interactions of the fatigue crack tip with the microstructure during the crack propagation stage. Full article
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19 pages, 6943 KB  
Article
A Comparative Transcriptomic Analysis of miRNAs and Their Target Genes During the Formation of Melanin in Apis mellifera
by Xiangjie Zhu, Yuanmingyue Tian, Mingjie Cao, Chenyu Zhu, Jiaqi Shang, Jiaqi Sun, Yiming Liu, Bingfeng Zhou, Shujing Zhou and Xinjian Xu
Agriculture 2025, 15(9), 992; https://doi.org/10.3390/agriculture15090992 - 3 May 2025
Viewed by 611
Abstract
Melanin is an important component of the body color of honeybees, and its formation changes with the age of a capped brood of bees. However, up to now, the regulatory mechanism of melanin formation in honeybees remains unclear. To analyze the differential expression [...] Read more.
Melanin is an important component of the body color of honeybees, and its formation changes with the age of a capped brood of bees. However, up to now, the regulatory mechanism of melanin formation in honeybees remains unclear. To analyze the differential expression profile of microRNAs (miRNAs) in worker bees of Apis mellifera and to reveal the regulatory roles of differentially expressed miRNAs (DEmiRNAs) and mRNAs in the formation process of melanin during the capped brood stage, we used sRNA-seq technology and related software to analyze samples from four key developmental stages during the capped brood stage, when body color develops in Apis mellifera, namely, mature larvae (L0), pre-pupae (PP3), early pupae (P6) and mid-pupae (P9). A total of 1291 miRNAs were identified by bioinformatics. Three comparison groups were analyzed: L0 vs. PP3, PP3 vs. P6, and P6 vs. P9. A total of 171, 94, and 19 DEmiRNAs were identified in these groups, respectively, which regulate 1481, 690, and 182 differentially expressed target mRNAs (target DEmRNAs). The functional analysis of target DEmRNAs indicated that DEmiRNAs might regulate the formation of capped brood melanin in honeybees by activating expression changes in key genes in signaling pathways, such as the Wnt signaling pathway, melanogenesis, and the Toll and Imd signaling pathway, through activating miR-315-x, miR-8, ple, yellow family genes, wnt1, etc. Our research provides a theoretical basis for future analysis of the regulatory role of miRNAs in the formation of melanin in honeybees. Full article
(This article belongs to the Section Farm Animal Production)
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39 pages, 10913 KB  
Article
Corrosion Behavior of X65 API 5L Carbon Steel Under Simulated Storage Conditions: Influence of Gas Mixtures, Redox States, and Temperature Assessed Using Electrochemical Methods for up to 100 Hours
by Yendoube Charles Sano Moyeme, Stephanie Betelu, Johan Bertrand, Karine Groenen Serrano and Ioannis Ignatiadis
Metals 2025, 15(2), 221; https://doi.org/10.3390/met15020221 - 18 Feb 2025
Cited by 1 | Viewed by 1577
Abstract
In the context of the deep geological disposal of high-level and intermediate-level long-lived radioactive waste in France, the Callovian–Oxfordian (Cox) clay formation has been selected as a natural barrier. Thus, understanding the corrosion phenomena between the carbon steel used (API 5L X65) for [...] Read more.
In the context of the deep geological disposal of high-level and intermediate-level long-lived radioactive waste in France, the Callovian–Oxfordian (Cox) clay formation has been selected as a natural barrier. Thus, understanding the corrosion phenomena between the carbon steel used (API 5L X65) for the waste lining tubes and the Cox pore water, as well as its possible future evolutions, is of great importance. A controlled laboratory experiment was conducted using robust handmade API 5L X65 carbon steel electrodes in synthetic Cox pore water under equilibrium with three distinct gas atmospheres, simulating oxic, anoxic, and sulfide-rich environments at 25 °C and 80 °C, in a batch-type electrochemical cell. The experimental methodology involved linear polarization resistance (LPR) cycles, electrochemical impedance spectroscopy (EIS), and Tafel extrapolation at regular intervals over a period of 70 to 100 h to elucidate corrosion mechanisms and obtain corrosion current densities. At the same time, the fluid’s key geochemical parameters (temperature, pH, and redox potential) were monitored for temporal variation. This study, with results showing high corrosion rates under the three conditions investigated at two temperatures, underscores the importance of controlling the immediate environment of the containment materials to prevent exposure to variable conditions and to ensure that corrosion remains controlled over the long term. Full article
(This article belongs to the Section Metal Casting, Forming and Heat Treatment)
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19 pages, 5751 KB  
Article
Effect of the Use of Some Rare Earth Compounds as Corrosion Inhibitors for API 5L X70 Steel in Saline Medium
by Salvador Hernández García, Araceli Espinoza Vázquez, Laura Nadxieli Palacios-Grijalva, Anatolio Martínez Jiménez, Francisco Javier Rodríguez Gómez, Óscar Armando Gómez Vargas, Alan Miralrio, Miguel Castro and Ricardo Orozco Cruz
Metals 2025, 15(2), 195; https://doi.org/10.3390/met15020195 - 13 Feb 2025
Viewed by 1216
Abstract
This work presents a comparative study of five rare earth compounds—Erbium nitrate pentahydrate lll (Er), Neodymium nitrate pentahydrate (Nd), Samarium III Nitrate Hexahydrate (Sm), Yterbium III Chloride Hexahydrate (Yb) and Praseodymium nitrate hexahydrate lll (Pr)—protecting API 5L X70 steel from corrosion in saline [...] Read more.
This work presents a comparative study of five rare earth compounds—Erbium nitrate pentahydrate lll (Er), Neodymium nitrate pentahydrate (Nd), Samarium III Nitrate Hexahydrate (Sm), Yterbium III Chloride Hexahydrate (Yb) and Praseodymium nitrate hexahydrate lll (Pr)—protecting API 5L X70 steel from corrosion in saline medium that uses electrochemical impedance spectroscopy (EIS) and polarization curves (CPs) at different concentrations and in static mode. The results show that Erbium is the best corrosion inhibitor, containing 50 ppm and reaching an inhibition efficiency of about 89%, and similar result was shown by Sm with an IE~87.9%, while the other rare earths (Nd, Yb and Pr) showed a decrease in corrosion protection at the same concentration, since they were below an IE~80%. On the other hand, with the Langmuir model it was possible to describe that the adsorption process of the three rare earths follows a combined physisorption–chemisorption process to protect the metal’s surface. The observed adsorption free energy, ΔG°ads, reaches −38.7 kJ/mol for Er, −34.4 kJ/mol for Nd, and −33.6 kJ/mol for Pr; whereas Sm and Yb have adsorption free energies of −33.9 and −35.0 kJ/mol, respectively. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) further confirmed the formation of a protective film. Their characterization using density functional theory showed the transference of charge from the iron cluster towards the rare earth metal compounds. The adsorption process produced a slightly polarized region of interaction with the metal surface. Also, it was found that the adsorption of the rare earths affected the magnetic properties of the surface of the iron cluster. Quantum chemical descriptors, such as Pearson’s HSAB (Hard and Soft Acids and Bases) descriptors, were useful in predicting the behavior of the flow of electrons between the metal surface and the interacting rare earth ions. Full article
(This article belongs to the Special Issue Advances in Corrosion and Protection of Materials (Third Edition))
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20 pages, 17899 KB  
Article
Modification of Ceritinib Crystal Morphology via Spherical Crystallization
by Iva Zokić, Jasna Prlić Kardum, Lana Crnac, Mirta Sabol, Juraj Vuić and Valentina Travančić
Crystals 2024, 14(11), 975; https://doi.org/10.3390/cryst14110975 - 12 Nov 2024
Cited by 2 | Viewed by 1626
Abstract
The formulation process for some drugs can be challenging, due to their unfavorable physical and mechanical properties and poor water solubility. Powder technology has made a significant impact in regard to the modification of the particles in active pharmaceutical ingredients (APIs) to produce [...] Read more.
The formulation process for some drugs can be challenging, due to their unfavorable physical and mechanical properties and poor water solubility. Powder technology has made a significant impact in regard to the modification of the particles in active pharmaceutical ingredients (APIs) to produce high-quality granules. Spherical particles are preferred over other shapes, due to their high tap and bulk density, reduced dustiness, better flowability, strong anti-caking properties, and better mechanical performance during tableting. The present study investigates the possibility of obtaining spherical crystals of ceritinib, a drug used for the treatment of anaplastic lymphoma kinase (ALK)-positive advanced non-small cell lung cancer, which belongs to BCS class IV drugs and has a platy crystal shape. Ceritinib spheres were prepared by spherical agglomeration, in a ternary system, and quasi-emulsion solvent diffusion, with the addition of polyvinylpyrrolidone, as well as a combination of these two methods. With the combined method of spherical crystallization, crystals with the most favorable morphology and the narrowest distribution of particle sizes were obtained, which was the reason for further optimization. The influence of different impeller geometries and mixing rates on the morphology of the obtained crystals was examined and the optimal conditions for the process were selected. Using empirical correlations and a visual criterion, the process was scaled up from a 0.1 L to a 1 L batch crystallizer. The obtained crystals were characterized by light and scanning electron microscopy. The addition of a bridging liquid and/or a polymer additive did not change the internal structure of the ceritinib crystals, which was confirmed by X-ray powder diffraction. Full article
(This article belongs to the Collection Feature Papers in Biomolecular Crystals)
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15 pages, 4372 KB  
Article
Exploring NRB Biofilm Adhesion and Biocorrosion in Oil/Water Recovery Operations Within Pipelines
by Hadjer Didouh, Hifsa Khurshid, Mohammed Hadj Meliani, Rami K. Suleiman, Saviour A. Umoren and Izzeddine Sameut Bouhaik
Bioengineering 2024, 11(10), 1046; https://doi.org/10.3390/bioengineering11101046 - 20 Oct 2024
Cited by 1 | Viewed by 2045
Abstract
Microbially influenced corrosion represents a critical challenge to the integrity and durability of carbon steel infrastructure, particularly in environments conducive to biofilm formation by nitrate-reducing bacteria (NRB). This study investigated the impact of NRB biofilms on biocorrosion processes within oil/water recovery operations in [...] Read more.
Microbially influenced corrosion represents a critical challenge to the integrity and durability of carbon steel infrastructure, particularly in environments conducive to biofilm formation by nitrate-reducing bacteria (NRB). This study investigated the impact of NRB biofilms on biocorrosion processes within oil/water recovery operations in Algerian pipelines. A comprehensive suite of experimental and analytical techniques, including microbial analysis, gravimetric methods, and surface characterization, were employed to elucidate the mechanisms of microbially influenced corrosion (MIC). Weight loss measurements revealed that carbon steel samples exposed to injection water exhibited a corrosion rate of 0.0125 mm/year, significantly higher than the 0.0042 mm/year observed in crude oil environments. The microbial analysis demonstrated that injection water harbored an average of (4.4 ± 0.56) × 106 cells/cm2 for sessile cells and (3.1 ± 0.25) × 105 CFU/mL for planktonic cells, in stark contrast to crude oil, which contained only (2.4 ± 0.34) × 103 cells/cm2 for sessile cells and (4.5 ± 0.12) × 102 CFU/mL for planktonic cells, thereby highlighting the predominant role of injection water in facilitating biofilm formation. Contact angle measurements of injection water on carbon showed 45° ± 2°, compared to 85° ± 4° for crude oil, suggesting an increased hydrophilicity associated with enhanced biofilm adhesion. Scanning electron microscopy further confirmed the presence of thick biofilm clusters and corrosion pits on carbon steel exposed to injection water, while minimal biofilm and corrosion were observed in the crude oil samples. Full article
(This article belongs to the Section Biochemical Engineering)
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19 pages, 7036 KB  
Article
Experimental and Numerical Analysis of the Impact of Corrosion on the Failure Pressure of API 5L X65 Pipeline
by Hongyang Zhao, Xu Liang, Zhiguo Yang, Pei He and Bowen Zhao
J. Mar. Sci. Eng. 2024, 12(10), 1810; https://doi.org/10.3390/jmse12101810 - 10 Oct 2024
Cited by 5 | Viewed by 1871
Abstract
This paper employs the Finite Element Method (FEM) to simulate and analyze the effects of corrosion defect parameters on the stress and failure pressure of pipelines. It investigates how the boundary conditions of the pipeline model influence stress and examines the sensitivity of [...] Read more.
This paper employs the Finite Element Method (FEM) to simulate and analyze the effects of corrosion defect parameters on the stress and failure pressure of pipelines. It investigates how the boundary conditions of the pipeline model influence stress and examines the sensitivity of failure pressure to corrosion defect parameters. A nonlinear regression equation has been developed from a dataset obtained through simulation experiments to predict the failure pressure of corroded pipelines. To validate the effects of corrosion defect parameters on failure pressure, a hydrostatic test platform for an API 5L X65 pipeline with corrosion defects was established to measure stress levels and failure pressures across varying corrosion defects. This study reveals that failure pressure is negatively correlated with corrosion length and depth, while positively correlated with corrosion width. Among these parameters, corrosion depth exerts a more significant influence on the pipeline’s failure pressure than corrosion length and width. Within the range of corrosion defect parameters examined, the maximum deviation of the prediction equation’s results from the simulation results is 8.71%, with an average deviation of 5.81%. The standard deviation of the fitted residuals is 0.01837. Additionally, the maximum deviation between the predicted results and experimental measurements is 8.39%, with an average deviation of 7.77%. The strong agreement between the predicted results from the equation and the actual measured data underscores the effectiveness of the nonlinear regression equation. Full article
(This article belongs to the Section Ocean Engineering)
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19 pages, 11905 KB  
Article
Influence of Centerline Segregation Region on the Hydrogen Embrittlement Susceptibility of API 5L X80 Pipeline Steels
by Mathews Lima dos Santos, Arthur Filgueira de Almeida, Guilherme Gadelha de Sousa Figueiredo, Marcos Mesquita da Silva, Theophilo Moura Maciel, Tiago Felipe Abreu Santos and Renato Alexandre Costa de Santana
Metals 2024, 14(10), 1154; https://doi.org/10.3390/met14101154 - 10 Oct 2024
Cited by 3 | Viewed by 1758
Abstract
The influence of the centerline segregation region (CSR) on the hydrogen embrittlement (HE) of two different API 5L X80 pipeline steel plates was investigated. The novelty of this work was to establish relationships between the CSR, microstructure, and distribution of localized fragile particles [...] Read more.
The influence of the centerline segregation region (CSR) on the hydrogen embrittlement (HE) of two different API 5L X80 pipeline steel plates was investigated. The novelty of this work was to establish relationships between the CSR, microstructure, and distribution of localized fragile particles on HE susceptibility and on fracture morphology. This work intended to establish a relationship between centerline segregation and HE susceptibility in high-strength low-alloy steels submitted to inhomogeneous transformations. Microscopy, hydrogen permeation, and slow strain rate (SSR) tests were used to investigate hydrogen-related degradation. The solution used on the charging cell of the permeation tests—and on the SSR test cell—was 0.5 mol L−1 H2SO4 + 10 mg L−1 As2O3, and in the oxidation cell, 0.1 M NaOH was used as a solution. The CSR led the thicker plate to present the highest HE index (0.612) in analyses carried out in the mid-thickness; however, the same plate showed the lowest HE index in near-surface tests. The presence of hydrogen changed the fracture morphology from ductile to a brittle and ductile feature; this occurred due to the interaction with localized fragile particles and the significant reduction of the shear stress necessary for the dislocation movement. Full article
(This article belongs to the Special Issue Mechanical Behaviors and Damage Mechanisms of Metallic Materials)
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13 pages, 41685 KB  
Article
Evaluating the Effect of Blended and Pure Hydrogen in X60 Pipeline Steel for Low-Pressure Transmission Using Hollow-Specimen Slow-Strain-Rate Tensile Testing
by Rashiga Walallawita, Matthew C. Hinchliff, Dimitry Sediako, John Quinn, Vincent Chou, Kim Walker and Matthew Hill
Metals 2024, 14(10), 1132; https://doi.org/10.3390/met14101132 - 4 Oct 2024
Cited by 5 | Viewed by 2229
Abstract
This study employs a custom hollow specimen setup to investigate the HE in API 5L X60 pipeline base and welded materials exposed to pure hydrogen and a 20% hydrogen–natural gas blend at 2.07 MPa. Results indicate embrittlement with increasing hydrogen concentration. The base [...] Read more.
This study employs a custom hollow specimen setup to investigate the HE in API 5L X60 pipeline base and welded materials exposed to pure hydrogen and a 20% hydrogen–natural gas blend at 2.07 MPa. Results indicate embrittlement with increasing hydrogen concentration. The base material showed a hydrogen embrittlement index (HEI) of 11.6% at 20% hydrogen and 12.4% at 100% hydrogen. For the welded material, the HEI was 14.6% at 20% hydrogen and 18.0% at 100% hydrogen. Fractography analysis revealed that the base and welded materials exhibited typical ductile fracture features in the absence of hydrogen, transitioning to a mixture of quasi-cleavage and micro-void coalescence (MVC) features in hydrogen environments. Additionally, with hydrogen, increased formation of secondary cracks was observed. Notably, the study identified the Hydrogen-Enhanced Localized Plasticity (HELP) mechanism as a probable contributor to hydrogen-assisted fracture. Full article
(This article belongs to the Special Issue Hydrogen Embrittlement of Metals and Alloys)
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14 pages, 1320 KB  
Article
Development of a Simple and Validated LC–MS/MS Method for Quantitative Determination of Ketotifen in Beagle Dog Plasma and Its Application to Bioequivalence Study of Ketotifen Syrup Dosage Form
by Eunseo Song, Wang-Seob Shim, Doowon Choi, Yuna Song, Hyeong Geun Jo, Soobok Lee, Suk Han Jung, Yeo Jin Choi and Kyung-Tae Lee
Molecules 2024, 29(18), 4505; https://doi.org/10.3390/molecules29184505 - 23 Sep 2024
Cited by 1 | Viewed by 1929
Abstract
A highly accurate, precise, and simple liquid chromatography-tandem mass spectrometry (LC–MS/MS) method for ketotifen (KTF) estimation from Beagle dog plasma was developed and validated, with ketotifen-d3 (KTF-d3) as the internal standard (IS). KTF and IS were detected on an API 4000 mass spectrometer [...] Read more.
A highly accurate, precise, and simple liquid chromatography-tandem mass spectrometry (LC–MS/MS) method for ketotifen (KTF) estimation from Beagle dog plasma was developed and validated, with ketotifen-d3 (KTF-d3) as the internal standard (IS). KTF and IS were detected on an API 4000 mass spectrometer in multiple reaction monitoring (MRM) mode in electrospray ionization (ESI) positive ionization mode. The transitions were monitored at m/z 310.2 → 96.0 for KTF and m/z 313.2 → 99.1 for IS. KTF and IS were extracted from plasma using liquid-liquid extraction with methyl tertiary-butyl ether and then analyzed for 3 min with extracted samples (7 µL) into the LC–MS/MS system. Analytes were separated on a Luna® Hilic column (50 × 2.0 mm i.d., 3 μm) using the Nexera X2 HPLC. The mobile phase A consisted of 10 mmol/L ammonium formate (pH 3.0), while mobile phase B consisted of 0.05% formic acid in acetonitrile. The ratio of mobile phase was 5:95 (v/v) at a flow rate of 0.2 mL/min. The method has been thoroughly validated in accordance with the bioanalytical method validation guidelines established by the Ministry of Food and Drug Safety in Korea and the U.S. Food and Drug Administration, addressing selectivity, lower limit of quantification, linearity, carryover, precision, accuracy, recovery, matrix effect, and stability. The developed LC–MS/MS method was effectively utilized for the bioequivalence assessment of ketotifen in Beagle dog plasma following the oral administration of ketotifen syrup. Full article
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20 pages, 6197 KB  
Article
Wearable ECG Device and Machine Learning for Heart Monitoring
by Zhadyra Alimbayeva, Chingiz Alimbayev, Kassymbek Ozhikenov, Nurlan Bayanbay and Aiman Ozhikenova
Sensors 2024, 24(13), 4201; https://doi.org/10.3390/s24134201 - 28 Jun 2024
Cited by 13 | Viewed by 12661
Abstract
With cardiovascular diseases (CVD) remaining a leading cause of mortality, wearable devices for monitoring cardiac activity have gained significant, renewed interest among the medical community. This paper introduces an innovative ECG monitoring system based on a single-lead ECG machine, enhanced using machine learning [...] Read more.
With cardiovascular diseases (CVD) remaining a leading cause of mortality, wearable devices for monitoring cardiac activity have gained significant, renewed interest among the medical community. This paper introduces an innovative ECG monitoring system based on a single-lead ECG machine, enhanced using machine learning methods. The system only processes and analyzes ECG data, but it can also be used to predict potential heart disease at an early stage. The wearable device was built on the ADS1298 and a microcontroller STM32L151xD. A server module based on the architecture style of the REST API was designed to facilitate interaction with the web-based segment of the system. The module is responsible for receiving data in real time from the microcontroller and delivering this data to the web-based segment of the module. Algorithms for analyzing ECG signals have been developed, including band filter artifact removal, K-means clustering for signal segmentation, and PQRST analysis. Machine learning methods, such as isolation forests, have been employed for ECG anomaly detection. Moreover, a comparative analysis with various machine learning methods, including logistic regression, random forest, SVM, XGBoost, decision forest, and CNNs, was conducted to predict the incidence of cardiovascular diseases. Convoluted neural networks (CNN) showed an accuracy of 0.926, proving their high effectiveness for ECG data processing. Full article
(This article belongs to the Section Biomedical Sensors)
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29 pages, 12204 KB  
Article
Optimizing Rolling Strategies for API 5L X80 Steel Heavy Plates Produced by Thermomechanical Processing in a Reversible Single-Stand Mill
by Luiz Gustavo de Oliveira Abreu, Geraldo Lúcio de Faria, Ricardo José de Faria, Daniel Bojikian Matsubara and Rodrigo Rangel Porcaro
Metals 2024, 14(7), 746; https://doi.org/10.3390/met14070746 - 25 Jun 2024
Cited by 4 | Viewed by 1718
Abstract
This study focuses on advancing the production of predominantly bainitic heavy plates to meet the API 5L X80 standard. The investigation involves a thorough evaluation of the influence of rolling parameters and austenite conditioning on both microstructural characteristics and mechanical properties. Accurate specifications [...] Read more.
This study focuses on advancing the production of predominantly bainitic heavy plates to meet the API 5L X80 standard. The investigation involves a thorough evaluation of the influence of rolling parameters and austenite conditioning on both microstructural characteristics and mechanical properties. Accurate specifications for chemical composition, processing temperatures, and mean deformations were established using mathematical models and bibliographical references. Four rolling conditions were performed in a reversible single-stand mill, allowing for comprehensive comparison and critical analysis. Microstructural and mechanical characterizations were performed utilizing several techniques, including optical microscopy (OM), scanning electron microscopy (SEM), tensile tests, Charpy impact tests, and hardness tests to ensure adherence to API 5L standards. Additionally, the SEM-EBSD (electron backscattered diffraction) technique was employed for a complementary analysis. The EBSD analysis included crystallographic misorientation maps, mean kernel misorientation parameters (ϑ), low- and high-angle grains boundaries, mean equivalent diameter, and evaluation of the contribution of different strengthening mechanisms to yield strength. Results underscored the significant influence of austenite conditioning on both microstructure and mechanical properties. Considering the specificities of a reversible single-stand mill, it was concluded that, unlike the classic approach for ferritic or ferritic–pearlitic HSLA (high-strength low-alloy steel), when a product with a predominantly bainitic microstructure is required, the accumulated deformation in the austenite during the finishing rolling stage, as well as its temperature, must be meticulously controlled. It was shown that the greater the deformation and the lower the temperature, the more favorable the scenario for the undesired polygonal ferrite formation, which will deteriorate the material’s performance. Furthermore, an optimized production route was identified and adapted to the specificities of the employed rolling mill. The presented data have great importance for researchers, manufacturers, and users of API 5L X80 heavy plates. Full article
(This article belongs to the Section Metal Casting, Forming and Heat Treatment)
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12 pages, 4067 KB  
Article
Binary Mixtures of Meloxicam and L-Tartaric Acid for Oral Bioavailability Modulation of Pharmaceutical Dosage Forms
by Cristina Macasoi, Viorica Meltzer, Ioana Stanculescu, Cosmin Romanitan and Elena Pincu
J. Funct. Biomater. 2024, 15(4), 104; https://doi.org/10.3390/jfb15040104 - 16 Apr 2024
Cited by 2 | Viewed by 2281
Abstract
Binary mixtures of active pharmaceutical ingredients (API) are researched to improve the oral bioavailability of pharmaceutical dosage forms. The purpose of this study was to obtain mixtures of meloxicam and L-tartaric acid because tartaric acid improves intestinal absorption and meloxicam is more soluble [...] Read more.
Binary mixtures of active pharmaceutical ingredients (API) are researched to improve the oral bioavailability of pharmaceutical dosage forms. The purpose of this study was to obtain mixtures of meloxicam and L-tartaric acid because tartaric acid improves intestinal absorption and meloxicam is more soluble in a weakly basic environment. The mixtures in the 0–1 molar fraction range, obtained from solvent-assisted mechanosynthesis, were investigated by differential scanning calorimetry (DSC), Fourier Transform Infrared (FTIR) spectroscopy, Fourier Transform Raman spectroscopy (FT-Raman), X-ray powder diffraction (XRD) and solubility tests. The physicochemical characteristics of the compounds obtained from DSC data reveal, for the first time, the formation of a co-crystal at meloxicam molar fraction of 0.5. FTIR spectroscopy data show the existence of hydrogen bonds between the co-crystal components meloxicam and L-tartaric acid. FT-Raman spectroscopy was used complementary with FT-IR spectroscopy to analyze the pure APIs and their mixtures, to emphasize the appearance/disappearance and the shifts of the position/intensity of vibrational bands, following the formation of hydrogen-bonded structures or van der Waals interactions, and to especially monitor the crystal lattice vibrations below 400 cm−1. The experimental results obtained by X-ray powder diffraction confirmed the formation of the co-crystal by the loss and, respectively, the apparition of peaks from the single components in the co-crystal diffractogram. The solubility tests showed that the co-crystal product has a lower aqueous solubility due to the acidic character of the other component, tartaric acid. However, when the solubility tests were performed in buffer solution of pH 7.4, the solubility of meloxicam from the co-crystal mixture was increased by 57% compared to that of pure meloxicam. In conclusion, the studied API mixtures may be considered potential biomaterials for improved drug release molecular solids. Full article
(This article belongs to the Special Issue Biomaterials for Translational Medicine)
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