Search results for: column chromatography

Authors: Abubakar Danbaba

Abstract:

Sudoku squares have been widely used to design an experiment where each treatment occurs exactly once in each row, column or sub-block. For some experiments, the size of row (or column or sub-block) may be larger than the number of treatments. Since each treatment appears only once in each row (column or sub-block) with an additional empty cell such designs are partially balanced Sudoku designs (PBSD) with NP-complete structures. This paper proposed methods for constructing PBSD of prime order of treatments by a modified Kronecker product and swap of matrix row (or column) in cyclic order. In addition, linear model and procedure for the analysis of data for PBSD are proposed.

Keywords: sudoku design, partial sudoku, NP-complete, Kronecker product, row and column swap

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Authors: R. Fegas, S. Zerkout, S. Taberkokt, M. Righezza

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The present work demonstrate the potential of Betacyclodextrine (BCD) for the chiral analysis of a drug .Various separation mechanisms were applied and several parameters affecting the separation were studied, including the type and concentration of chiral selector, and pH of buffer. A simple and sensitive high-performance liquid chromatography (HPLC) method was developed as an assay for fexofenadine enantiomers in pharmaceutical preparation. Fexofenadine enantiomers were separated using a mobile phase of 0.25mM NaH2PO4–acetonitrile (65:35, v/v) – Betacyclodextrine on achiral phenyl-urea column at a flow rate of 1ml/min and measurement at 220nm. The chiral mechanism of separation was mainly based on specific interaction between the solute and the stationary phase. The retention was directly controlled by mobile phase composition but not the selectivity which results of the two mechanisms, electrostatic interactions and partition mechanism.

Keywords: fexofenadine enantiomer, HPLC, achiral phenyl-urea column

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Authors: X. Han, S. Duan, C. Liu, C. Zhou, W. Zhu, L. Kong

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The ionic imprinting technique refers to the three-dimensional rigid structure with the fixed pore sizes, which was formed by the binding interactions of ions and functional monomers and used ions as the template, it has a high level of recognition to the ionic template. The preparation of monolithic column by the in-situ polymerization need to put the compound of template, functional monomers, cross-linking agent and initiating agent into the solution, dissolve it and inject to the column tube, and then the compound will have a polymerization reaction at a certain temperature, after the synthetic reaction, we washed out the unread template and solution. The monolithic columns are easy to prepare, low consumption and cost-effective with fast mass transfer, besides, they have many chemical functions. But the monolithic columns have some problems in the practical application, such as low-efficiency, quantitative analysis cannot be performed accurately because of the peak shape is wide and has tailing phenomena; the choice of polymerization systems is limited and the lack of theoretical foundations. Thus the optimization of components and preparation methods is an important research direction. During the preparation of ionic imprinted monolithic columns, pore-forming agent can make the polymer generate the porous structure, which can influence the physical properties of polymer, what’ s more, it can directly decide the stability and selectivity of polymerization reaction. The compounds generated in the pre-polymerization reaction could directly decide the identification and screening capabilities of imprinted polymer; thus the choice of pore-forming agent is quite critical in the preparation of imprinted monolithic columns. This article mainly focuses on the research that when using different pore-forming agents, the impact of zinc ion imprinted monolithic column on the enrichment performance of zinc ion.

Keywords: high performance liquid chromatography (HPLC), ionic imprinting, monolithic column, pore-forming agent

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Authors: Rabab Allouzi, Amer Alkloub

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As the complex shaped buildings become a popular trend for architects, this paper is presented to investigate the performance of reinforced concrete flat plate-inclined column connection. The studies on the inclined column and flat plate connections are not sufficient in comparison to those on the conventional structures. The effect of column angle of inclination on the punching shear strength is found significant and studied herein. This paper presents a non-linear finite element based modeling approach to estimate behavior of RC flat plate inclined column connection. Results from simulations of RC flat plate-straight column connection show good agreement with experimental response of specimens tested by other researchers. The model is further used to study the response of inclined columns to punching at various ranges of inclination angles. The inclination angle can be included in the punching shear strength provisions provided by ACI 318-14 to account for the effect of column inclination.

Keywords: punching shear, non-linear finite element, inclined columns, reinforced concrete connection

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Authors: Abdul Hakim Chikho

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Calculating the ultimate load of a column in a sway framed structure involves, in the currently used design method, the calculation of the column effective length and utilizing the interaction formulas or tables. Therefore, no allowance is usually made for the effects of the presence of semi rigid connections or the presence of infill panels. In this paper, a new and simple design procedure is recommend to calculate the ultimate load of a framed Column allowing for the presence of rotational end restraints, semi rigid connections, the column end moments resulted from the applied vertical and horizontal loading and infill panels in real steel structure. In order to verify the accuracy of the recommended method to predict good and safe estimations of framed column ultimate loads, several examples have been solved utilizing the recommended procedure, and the results were compared to those obtained using a second order computer program, and good correlation had been obtained. Therefore, the accuracy of the proposed method to predict the Behaviour of practical steel columns in framed structures has been verified.

Keywords: column ultimate load, semi rigid connections, steel column, infill panel, steel structure

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Authors: Walid El Kamash

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Sand columns (or granular piles) can be employed as soil strengthening for flexible constructions such as road embankments, oil storage tanks in addition to multistory structures. The challenge of embedding the sand columns in soft soil is that the surrounding soft soil cannot avail the enough confinement stress in order to keep the form of the sand column. Therefore, the sand columns which were installed in such soil will lose their ability to perform needed load-bearing capacity. The encasement, besides increasing the strength and stiffness of the sand column, prevents the lateral squeezing of sands when the column is installed even in extremely soft soils, thus enabling quicker and more economical installation. This paper investigates the improvement in load capacity of the sand column by encasement through a comprehensive parametric study using the 3-D finite difference analysis for the soft clay of soil in Egypt. Moreover, the study was extended to include a comparison study between encased sand column and Deep Mixed columns (DM). The study showed that confining the sand by geosynthetic resulted in an increment of shear strength. That result paid the attention to use encased sand stone rather than deep mixed columns due to relative high permeability of the first material.

Keywords: encased sand column, Deep mixed column, numerical analysis, improving soft soil

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Authors: Rifqi Irvansyah, Abdullah Abdullah, Yunita Idris, Bunga Raihanda

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Banda Aceh is particularly susceptible to heightened vulnerability during natural disasters due to its concentrated exposure to multi-hazard risks. Despite urgent priorities during the aftermath of natural disasters, such as the 2004 Indian Ocean earthquake and tsunami, several public facilities, including school buildings, sustained damage yet continued operations without adequate repairs, even though they were submerged by the tsunami. This research aims to evaluate the consequences of column damage induced by tsunami inundation on the structural integrity of buildings. The investigation employs interaction diagrams for columns to assess their capacity, taking into account factors such as rebar deterioration and corrosion. The analysis result shows that one-fourth of the K1 columns on the first floor fall outside of the column interaction diagram, indicating that the column structure cannot handle the load above it, as evidenced by the presence of Pu and Mu, which are greater than the column's design strength. This suggests that the five columns of K1 should be cause for concern, as the column's capacity is decreasing. These results indicate that the structure of the building cannot sustain the applied load because the column cross-section has deteriorated. In contrast, all K2 columns meet the design strength, indicating that the column structure can withstand the structural loads.

Keywords: tsunami inundation, column damage, column interaction diagram, mitigation effort

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Authors: Omar M. Ben-Sasi

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Ductility of slab-column connections of flat slab structures is a desirable property that should be considered when designing such connections which are susceptible to punching failure around their columns. Tests to failure on six half-scale specimens were conducted for slab-interior column connections transferring shear force and unbalanced moment. The influences on connection ductility of four parameters; namely, the moment to shear force ratio, the ratio of column side length to slab effective depth, the aspect ratio of the column cross section, and the presence of four square openings located next to column corners were investigated. The study revealed marked effects of these parameters on connection ductility. Increasing the first and second parameters, were found to be in favor of increasing connection ductility, while the third and fourth parameters were found to have negative effects on the connection ductility. These findings should, hopefully, help in designing interior connections of flat slab structures.

Keywords: ductility, flat slab, failure, shear force, moment, unbalanced moment, punching failure, connection, interior-column connection

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Authors: L. Pavithra, R. Sharmila, Shivani Sridhar

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Columns severe structural damage needs proportioning a significant portion of earthquake energy can be dissipated yielding in the beams. Presence of axial load along with cyclic loading has a significant influence on column. The objective of this paper is to present the analytical results of columns subjected to biaxial cyclic loading.

Keywords: RC column, Seismic behaviour, cyclic behaviour, biaxial testing, ductile behaviour

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Authors: Thidarat Duangyod, Chanida Palanuvej, Nijsiri Ruangrungsi

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Pentace burmanica Kurz., belonging to the Malvaceae family, is commonly used for anti-diarrhea in Thai traditional medicine. A method for quantification of (+)-catechin and (-)-epicatechin in P. burmanica stem bark from 12 different Thailand markets by reverse-phase high performance liquid chromatography (HPLC) was investigated and validated. The analysis was performed by a Shimadzu DGU-20A3 HPLC equipped with a Shimadzu SPD-M20A photo diode array detector. The separation was accomplished with an Inersil ODS-3 column (5 µm x 4.6 x 250 mm) using 0.1% formic acid in water (A) and 0.1% formic acid in acetonitrile (B) as mobile phase at the flow rate of 1 ml/min. The isocratic was set at 20% B for 15 min and the column temperature was maintained at 40 ºC. The detection was at the wavelength of 280 nm. Both (+)-catechin and (-)-epicatechin existed in the ethanolic extract of P. burmanica stem bark. The content of (-)-epicatechin was found as 59.74 ± 1.69 µg/mg of crude extract. In contrast, the quantitation of (+)-catechin content was omitted because of its small amount. The method was linear over a range of 5-200 µg/ml with good coefficients (r2 > 0.99) for (+)-catechin and (-)-epicatechin. Limit of detection values were found to be 4.80 µg/ml for (+)-catechin and 5.14 µg/ml for (-)-epicatechin. Limit of quantitation of (+)-catechin and (-)-epicatechin were of 14.54 µg/ml and 15.57 µg/ml respectively. Good repeatability and intermediate precision (%RSD < 3) were found in this study. The average recoveries of both (+)-catechin and (-)-epicatechin were obtained with good recovery in the range of 91.11 – 97.02% and 88.53 – 93.78%, respectively, with the %RSD less than 2. The peak purity indices of catechins were more than 0.99. The results suggested that HPLC method proved to be precise and accurate and the method can be conveniently used for (+)-catechin and (-)-epicatechin determination in ethanolic extract of P. burmanica stem bark. Moreover, the stem bark of P. burmanica was found to be a rich source of (-)-epicatechin.

Keywords: pentace burmanica, (+)-catechin, (-)-epicatechin, high performance liquid chromatography

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Authors: Vijayalakshmi Marella, NageswaraRaoPilli

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This paper describes a simple, rapid and sensitive liquid chromatography / tandem mass spectrometry assay for the determination of montelukast in human plasma using montelukast d6 as an internal standard. Analyte and the internal standard were extracted from 50 µL of human plasma via solid phase extraction technique without evaporation, drying and reconstitution steps. The chromatographic separation was achieved on a C18 column by using a mixture of methanol and 5mM ammonium acetate (80:20, v/v) as the mobile phase at a flow rate of 0.8 mL/min. Good linearity results were obtained during the entire course of validation. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. A run time of 2.5 min for each sample made it possible to analyze more number of samples in short time, thus increasing the productivity. The proposed method was found to be applicable to clinical studies.

Keywords: Montelukast, tandem mass spectrometry, montelukast d6, FDA guidelines

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Authors: Muneerah Jeludin

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The vibrated column has been widely used over the last three decades to improve the performance of soft ground and engineered compacted fill. The main reason for adopting this technique is that it is economically viable and environmental friendly. The performance of granular column with regards to bearing capacity has been well documented; however, information regarding the settlement behavior of granular columns is still limited. This paper aims to address the findings from a laboratory model study in terms of its settlement improvement. A 300 mm diameter and 400 mm high kaolin clay model was used in this investigation. Columns of various heights were installed in the clay bed using replacement method. The results in relation to load sharing mechanism between the column and surrounding clay just under the footing indicated that in short column, the available shaft resistance was not significant and introduces a potential for end braing failure as opposed to bulging failure in long columns. The settlement improvement factor corroborates well with field observations.

Keywords: ground improvement, model test, reinforced soil, foundation

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Authors: Hansoo Kim, Seunghak Shin

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The differential column shortening in tall buildings can be reduced by improving material and structural characteristics of the structural systems. This paper proposes structural methods to reduce differential column shortening in reinforced concrete tall buildings; connecting columns with rigidly jointed horizontal members, using outriggers, and placing additional reinforcement at the columns. The rigidly connected horizontal members including outriggers reduce the differential shortening between adjacent vertical members. The axial stiffness of columns with greater shortening can be effectively increased by placing additional reinforcement at the columns, thus the differential column shortening can be reduced in the design stage. The optimum distribution of additional reinforcement can be determined by applying a gradient based optimization technique.

Keywords: column shortening, long-term behavior, optimization, tall building

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Authors: Anil P. Dewani, Alok S. Tripathi, Anil V. Chandewar

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Present manuscript reports the development and validation of a quantitative high performance liquid chromatography method for the pharmacokinetic evaluation of Glimepiride (GLM) and Ilaprazole (ILA) in rat plasma. The plasma samples were involved with Solid phase extraction process (SPE). The analytes were resolved on a Phenomenex C18 column (4.6 mm× 250 mm; 5 µm particle size) using a isocratic elution mode comprising methanol:water (80:20 % v/v) with pH of water modified to 3 using Formic acid, the total run time was 10 min at 225 nm as common wavelength, the flow rate throughout was 1ml/min. The method was validated over the concentration range from 10 to 600 ng/mL for GLM and ILA, in rat plasma. Metformin (MET) was used as Internal Standard. Validation data demonstrated the method to be selective, sensitive, accurate and precise. The limit of detection was 1.54 and 4.08 and limit of quantification was 5.15 and 13.62 for GLM and ILA respectively, the method demonstrated excellent linearity with correlation coefficients (r2) 0.999. The intra and inter-day precision (RSD%) values were < 2.0% for both ILA and GLM. The method was successfully applied in pharmacokinetic studies followed by oral administration in rats.

Keywords: pharmacokinetics, glimepiride, ilaprazole, HPLC, SPE

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Authors: Y. T. Lee, J. H. Na, S. H. Kim, S. U. Hong

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In this study, an experimental research for estimation of slab depth, column size and location of rebar of concrete specimen is conducted using the Impact Echo Method (IE) based on stress wave among non-destructive test methods. Estimation of slab depth had total length of 1800×300 and 6 different depths including 150 mm, 180 mm, 210 mm, 240 mm, 270 mm and 300 mm. The concrete column specimen was manufactured by differentiating the size into 300×300×300 mm, 400×400×400 mm and 500×500×500 mm. In case of the specimen for estimation of rebar, rebar of ∅22 mm was used in a specimen of 300×370×200 and arranged at 130 mm and 150 mm from the top to the rebar top. As a result of error rate of slab depth was overall mean of 3.1%. Error rate of column size was overall mean of 1.7%. Mean error rate of rebar location was 1.72% for top, 1.19% for bottom and 1.5% for overall mean showing relative accuracy.

Keywords: impact echo method, estimation, slab depth, column size, rebar location, concrete

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Authors: Abid Fida Masih

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Forced degradation study of Rifaximin was conducted to determine the stability indicating potential of HPLC testing method for detection of Rifaximin in formulated tablets to be employed for quality control and stability testing. The questioned method applied with mobile phase methanol: water (70:30), 5µm, 250 x 4.6mm, C18 column, wavelength 293nm and flow rate of 1.0 ml/min. Forced degradation study was performed under oxidative, acidic, basic, thermal and photolytic conditions. The applied method successfully determined the degradation products after acidic and basic degradation without interfering with Rifaximin detection. Therefore, the method was said to be stability indicating and can be applied for quality control and stability testing of Rifaxmin tablets during its shelf life.

Keywords: forced degradation, high-performance liquid chromatography, method validation, rifaximin, stability indicating method

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Authors: Evgeny E. Tereshatov

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Astatine-211 is considered one of the most promising radionuclides for Targeted Alpha Therapy. In order to develop reliable procedures to label biomolecules and utilize efficient delivery vehicle principles, one should understand the main chemical characteristics of astatine. The short half-life of 211At (~7.2 h) and absence of any stable isotopes of this element are limiting factors towards studying the behavior of astatine. Our team has developed a procedure for rapid and efficient isolation of astatine from irradiated bismuth material in nitric acid media based on 3-octanone and 1-octanol extraction chromatography resins. This process has been automated and it takes 20 min from the beginning of the target dissolution to the At-211 fraction elution. Our next step is to consider commercially available chromatography resins and their applicability in astatine purification in the same media. Results obtained along with the corresponding sorption mechanisms will be discussed.

Keywords: astatine-211, chromatography, automation, mechanism, radiopharmaceuticals

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Authors: Khalifa Kherafa

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This east project consists in studying beam–column joints concrete subjected to seismic loads. A bibliographical study was introduced to clarify the work undertaken by the researchers in the field during the three last decades and especially the two last year’s results which were to study for the determination of the method of calculating of transverse reinforcement in the various nodes of a structure. For application, the efforts in the posts el the beams of a building in R+4 in zone 3 were calculate according to the finite element method through the software .

Keywords: beam–column joints, cyclic loading, shearing force, damaged joint

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Authors: Sumi Deka, Krishna Gopal Bhattacharyya

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This paper evaluate the industrial use of Kala Jamun (Syzygiumcumini L.) Seed powder (KSP) for the continuous adsorption of Cr(VI) in a column adsorption process. Adsorption of Cr(VI) onto Kala jamun (Syzygiumcumini L.) Seed Powder have been examined with the variation of (a) bed depth of the adsorbents, (b) flow rate of the adsorbents and (c) Cr(VI) concentration. The results showed that both the adsorption and the regeneration of the Cr(VI) onto Kala Jamun (Syzygiumcumini L.) seed Powder (KSP) can effectively occur in the column mode of adsorption. On increasing the bed depth, the adsorption of Cr(VI) onto KSP increases whereas on increasing the flow rate and the Cr(VI) concentration of KSP adsorption decreases. The results of the column studies were also fitted to Bed Depth Service Time (BDST) model. The BDST model was appropriate for designing the column for industrial purpose.

Keywords: bed-depth-service-time, continuous adsorption, Cr(VI), KSP

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Authors: Naveeda Akhtar Qureshi, Wajiha

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Coccidiosis is a protozoan parasitic disease of genus Eimeria. It is an avian infection causing a great economic loss of 3 billion USD per year globally. A number of anticoccidial drugs are in use however many of them have side effects and cost effective. With increase in poultry demand throughout the world there is a need of more drugs and vaccines against coccidiosis. The present study is based upon the use of F. racemosa a medicinal plant to be a potential source of anticoccidial agents. The methanolic leaves extract was fractionated by column and thin layer chromatography and got nineteen fractions. Each fraction different concentrations was evaluated for its anticoccidial properties in an invitro experiment against E. tenella, E. necatrix and E. mitis. The anticoccidial active fractions were further characterized by spectroscopy (UV-Vis, FTIR) and GC-MS analysis. The in silico molecular docking of active fractions identified compounds were carried out. Among all fractions significantly maximum sporulation inhibition efficacy was shown by F-19 (67.11±2.18) followed by F-15 (65.21±1.34) at concentration of 30mg/ml against E. tenella. The significantly highest sporozoites viability inhibition was shown by F-19 (69.23±2.11) followed by F-15 (67.14±1.52) against E. necatrix at concentration 30mg/ml. Anticoccidial active fractions 15 and 19 showed peak spectrum at 207 and 202nm respectively by UV analysis. Their FTIR analysis confirmed the presence of carboxylic acid, amines, phenols, etc. Anticoccidial active compounds like Cyclododecane methanol, oleic acid, Octadecanoic acid, etc were identified by GC-MS analysis. Identified compounds in silico molecular docking study showed that cyclododecane methanol of F-19 and oleic acid of F-15 showed highest binding affinity with target S-Adenosylmethionine synthase. Hence for further authentication in vivo anticoccidial studies are recommended.

Keywords: ficus racemosa, cluster fig, column chromatography, anticoccidial fractions, GC-MS, molecular docking., s-adenosylmethionine synthase

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Authors: Nina N. Serdar, Jelena R. Pejović

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This paper presents seismic risk assessment of two bridge structure, based on the probabilistic performance-based seismic assessment methodology. Both investigated bridges are tree span continuous RC curved bridges with the difference in column shapes. First bridge (type A) has a wall-type pier and second (type B) has a two-column bent with circular columns. Bridges are designed according to European standards: EN 1991-2, EN1992-1-1 and EN 1998-2. Aim of the performed analysis is to compare seismic behavior of these two structures and to detect the influence of column shapes on the seismic response. Seismic risk assessment is carried out by obtaining demand fragility curves. Non-linear model was constructed and time-history analysis was performed using thirty five pairs of horizontal ground motions selected to match site specific hazard. In performance based analysis, peak column drift ratio (CDR) was selected as engineering demand parameter (EDP). For seismic intensity measure (IM) spectral displacement was selected. Demand fragility curves that give probability of exceedance of certain value for chosen EDP were constructed and based on them conclusions were made.

Keywords: RC curved bridge, demand fragility curve, wall type column, nonlinear time-history analysis, circular column

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Authors: M. Chafi, S. Akazdam, C. Asrir, L. Sebbahi, B. Gourich, N. Barka, M. Essahli

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Fixed bed adsorption has become a frequently used industrial application in wastewater treatment processes. Various low cost adsorbents have been studied for their applicability in treatment of different types of effluents. In this work, the intention of the study was to explore the efficacy and feasibility for azo dye, Acid Orange 7 (AO7) adsorption onto fixed bed column of NaOH Treated eggshell (TES). The effect of various parameters like flow rate, initial dye concentration, and bed height were exploited in this study. The studies confirmed that the breakthrough curves were dependent on flow rate, initial dye concentration solution of AO7 and bed depth. The Thomas, Yoon–Nelson, and Adams and Bohart models were analysed to evaluate the column adsorption performance. The adsorption capacity, rate constant and correlation coefficient associated to each model for column adsorption was calculated and mentioned. The column experimental data were fitted well with Thomas model with coefficients of correlation R2 ≥0.93 at different conditions but the Yoon–Nelson, BDST and Bohart–Adams model (R2=0.911), predicted poor performance of fixed-bed column. The (TES) was shown to be suitable adsorbent for adsorption of AO7 using fixed-bed adsorption column.

Keywords: adsorption models, acid orange 7, bed depth, breakthrough, dye adsorption, fixed-bed column, treated eggshell

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Authors: Stoyan Nedeltchev, Markus Schubert

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The gas holdup fluctuations in a bubble column (0.15 m in ID) have been recorded by means of a conductivity wire-mesh sensor in order to extract information about the main transition velocities. These parameters are very important for bubble column design, operation and scale-up. For this purpose, the classical definition of the Shannon entropy was modified and used to identify both the onset (at UG=0.034 m/s) of the transition flow regime and the beginning (at UG=0.089 m/s) of the churn-turbulent flow regime. The results were compared with the Kolmogorov entropy (KE) results. A slight discrepancy was found, namely the transition velocities identified by means of the KE were shifted to somewhat higher (0.045 and 0.101 m/s) superficial gas velocities UG.

Keywords: bubble column, gas holdup fluctuations, modified Shannon entropy, Kolmogorov entropy

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Authors: Chong Zhang, Mu-Xuan Tao

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In several earthquakes, numerous reinforced concrete (RC) frames subjected to seismic excitation demonstrated a collapse pattern characterized by column hinges, though designed according to the Strong-Column-Weak-Beam (S-C-W-B) criteria. The effect of biaxial seismic excitation on the disparity between design and actual performance is carefully investigated in this article. First, a modified load contour method is proposed to derive a closed-form equation of biaxial bending moment strength, which is verified by numerical and experimental tests. Afterwards, a group of time history analyses of a simple frame modeled by fiber beam-column elements subjected to biaxial seismic excitation are conducted to verify that the current S-C-W-B criteria are not adequate to prevent the occurrence of column hinges. A biaxial over-strength factor is developed based on the proposed equation, and the reinforcement of columns is appropriately amplified with this factor to prevent the occurrence of column hinges under biaxial excitation, which is proved to be effective by another group of time history analyses.

Keywords: biaxial bending moment capacity, biaxial seismic excitation, fiber beam model, load contour method, strong-column-weak-beam

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Authors: A. Ramachandra Reddy, V. Murugan, Prema Kumari

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Residual solvents in Pharmaceutical samples are monitored using gas chromatography with headspace (GC-HS). Based on current regulatory and compendial requirements, measuring the residual solvents are mandatory for all release testing of active pharmaceutical ingredients (API). Generally, isopropyl alcohol is used as the residual solvent in proline and tryptophan; methanol in cysteine monohydrate hydrochloride, glycine, methionine and serine; ethanol in glycine and lysine monohydrate; acetic acid in methionine. In order to have a single method for determining these residual solvents (isopropyl alcohol, ethanol, methanol and acetic acid) in all these 7 amino acids a sensitive and simple method was developed by using gas chromatography headspace technique with flame ionization detection. During development, no reproducibility, retention time variation and bad peak shape of acetic acid peaks were identified due to the reaction of acetic acid with the stationary phase (cyanopropyl dimethyl polysiloxane phase) of column and dissociation of acetic acid with water (if diluent) while applying temperature gradient. Therefore, dimethyl sulfoxide was used as diluent to avoid these issues. But most the methods published for acetic acid quantification by GC-HS uses derivatisation technique to protect acetic acid. As per compendia, risk-based approach was selected as appropriate to determine the degree and extent of the validation process to assure the fitness of the procedure. Therefore, Total error concept was selected to validate the analytical procedure. An accuracy profile of ±40% was selected for lower level (quantitation limit level) and for other levels ±30% with 95% confidence interval (risk profile 5%). The method was developed using DB-Waxetr column manufactured by Agilent contains 530 µm internal diameter, thickness: 2.0 µm, and length: 30 m. A constant flow of 6.0 mL/min. with constant make up mode of Helium gas was selected as a carrier gas. The present method is simple, rapid, and accurate, which is suitable for rapid analysis of isopropyl alcohol, ethanol, methanol and acetic acid in amino acids. The range of the method for isopropyl alcohol is 50ppm to 200ppm, ethanol is 50ppm to 3000ppm, methanol is 50ppm to 400ppm and acetic acid 100ppm to 400ppm, which covers the specification limits provided in European pharmacopeia. The accuracy profile and risk profile generated as part of validation were found to be satisfactory. Therefore, this method can be used for testing of residual solvents in amino acids drug substances.

Keywords: amino acid, head space, gas chromatography, total error

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Authors: Shipra Shukla, Gaurav Chaudhary, S. K. Tewari, Mahesh Pal, D. K. Upreti

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Cassia tora L. is widely distributed in tropical Asian countries, commonly known as sickle pod. Various parts of the plant are reported for their medicinal value due to presence of anthraquinones, phenolic compounds, emodin, β-sitosterol, and chrysophanol. Therefore a sensitive analytical procedure using UHPLC-ESI-MS/MS was developed and validated for simultaneous quantification of five phenolic compounds in leaf, stem and root extracts of Cassia tora. Rapid chromatographic separation of compounds was achieved on Acquity UHPLC BEH C18 column (50 mm×2.1 mm id, 1.7µm) column in 2.5 min. Quantification was carried out using negative electrospray ionization in multiple-reaction monitoring mode. The method was validated as per ICH guidelines and showed good linearity (r2 ≥ 0.9985) over the concentration range of 0.5-200 ng/mL. The intra- and inter-day precisions and accuracy were within RSDs ≤ 1.93% and ≤ 1.90%, respectively. The developed method was applied to investigate variation of five phenolic compounds in the three geographical collections. Results indicated significant variation among analyzed samples collected from different locations in India.

Keywords: Cassia tora, phenolic compounds, quantification, UHPLC-ESI-MS/MS

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Authors: Ebrahim Zamani Beydokhti, Hashem Shariatmadar

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This paper presents an experimental and analytical investigation on the behavior of retrofitted beam-column joints subjected to reversed cyclic loading. The experimental program comprises 8 external beam–column joint connection subassemblages tested in 2 phases; one was the damaging phase and second was the repairing phase. The beam-column joints were no seismically designed, i.e. the joint, beam and column critical zones had no special transverse stirrups. The joins were tested under cyclic loading in previous research. The experiment had two phases named damage phase and retrofit phase. Then the experimental results compared with analytical results achieved from modeling in OpenSees software. The presence of lateral slab and the axial load amount were analytically investigated. The results showed that increasing the axial load and presence of lateral slab increased the joint capacity. The presence of lateral slab increased the dissipated energy, while the axial load had no significant effect on it.

Keywords: concrete beam-column joints, CFRP sheets, lateral slab, axial load

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Authors: A. B. Bazaralieva, A. A. Turgumbayeva

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The phytosubstance from garlic was obtained by extraction with liquid carbon dioxide under critical conditions. Methods of processing raw materials are proposed, and the chemical composition of garlic is studied by gas chromatography and mass spectrometry. The garlic extract's composition was determined using gas chromatography (GC) and gas chromatography-mass spectrophotometry (GC-MS). The phytosubstance had 54 constituents. The extract included the following main compounds: Manool (39.56%), Viridifrolol (7%), Podocarpa-1,8,11,13-tetraen-3-one, 14-isopropyl-1,13-dimethoxy- 5,15 percent, (+)-2-Bornanone (4.29%), Thujone (3.49%), Linolic acid ethyl ester (3.41%), and 12-O-Methylcarn.

Keywords: Allium sativum, bioactive compounds of garlic, carbon dioxide extraction of garlic, GS-MS method

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Authors: Kausar Ali

Abstract:

There are several ground treatment techniques which may meet the twin objectives of increasing the bearing capacity with simultaneous reduction of settlements, but the use of stone columns is one of the most suited techniques for flexible structures such as embankments, oil storage tanks etc. that can tolerate some settlement and used worldwide. However, when the stone columns in very soft soils are loaded; stone columns undergo excessive settlement due to low lateral confinement provided by the soft soil, leading to the failure of the structure. The poor performance of stone columns under these conditions can be improved by encasing the columns with a suitable geosynthetic. In this study, the effect of reinforcement on bearing capacity of composite soil has been investigated by conducting laboratory model tests on floating and end bearing long stone columns with l/d ratio of 12. The columns were reinforced by providing geosynthetic encasement over varying column length (upper 25%, 50%, 75%, and 100% column length). In this study, a group of columns has been used instead of single column, because in the field, columns used for the purpose always remain in groups. The tests indicate that the encasement over the full column length gives higher failure stress as compared to the encasement over the partial column length for both floating and end bearing long columns. The performance of end-bearing columns was found much better than the floating columns.

Keywords: geosynthetic, ground improvement, soft clay, stone column

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Authors: Layla El Gaini, Majdouline Belaqziz, Meriem Outaki, Mariam Minhaj

Abstract:

In this study, it introduce and validate a high-performance liquid chromatography method with diode-array detection (HPLC-DAD) specifically designed for the accurate quantification of caffeic acid in phenolic extracts obtained from olive mill wastewater. The separation process of caffeic acid was effectively achieved through the use of an Acclaim Polar Advantage column (5µm, 250x4.6mm). A meticulous multi-step gradient mobile phase was employed, comprising water acidified with phosphoric acid (pH 2.3) and acetonitrile, to ensure optimal separation. The diode-array detection was adeptly conducted within the UV–VIS spectrum, spanning a range of 200–800 nm, which facilitated precise analytical results. The method underwent comprehensive validation, addressing several essential analytical parameters, including specificity, repeatability, linearity, as well as the limits of detection and quantification, alongside measurement uncertainty. The generated linear standard curves displayed high correlation coefficients, underscoring the method's efficacy and consistency. This validated approach is not only robust but also demonstrates exceptional reliability for the focused analysis of caffeic acid within the intricate matrices of wastewater, thus offering significant potential for applications in environmental and analytical chemistry.

Keywords: high-performance liquid chromatography (HPLC-DAD), caffeic acid analysis, olive mill wastewater phenolics, analytical method validation

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