Search results for: chiral sensing
Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 1151

Search results for: chiral sensing

1151 Chiral Carbon Quantum Dots for Paper-Based Photoluminescent Sensing Platforms

Authors: Erhan Zor, Funda Copur, Asli I. Dogan, Haluk Bingol

Abstract:

Current trends in the wide-scale sensing technologies rely on the development of miniaturized, rapid and easy-to-use sensing platforms. Quantum dots (QDs) with strong and easily tunable luminescence and high emission quantum yields have become a well-established photoluminescent nanomaterials for sensor applications. Although the majority of the reports focused on the cadmium-based QDs which have toxic effect on biological systems and eventually would cause serious environmental problems, carbon-based quantum dots (CQDs) that do not contain any toxic class elements have attracted substantial research interest in recent years. CQDs are small carbon nanostructures (less than 10 nm in size) with various unique properties and are widely-used in different fields during the last few years. In this respect, chiral nanostructures have become a promising class of materials in various areas such as pharmacology, catalysis, bioanalysis and (bio)sensor technology due to the vital importance of chirality in living systems. We herein report the synthesis of chiral CQDs with D- or L-tartaric acid as precursor materials. The optimum experimental conditions were examined and the purification procedure was performed using ethanol/water by column chromatography. The purified chiral CQDs were characterized by UV-Vis, FT-IR, XPS, PL and TEM techniques. The resultants display different photoluminescent characteristics due to the size and conformational difference. Considering the results, it can be concluded that chiral CQDs is expected to be used as optical chiral sensor in different platforms.

Keywords: carbon quantum dots, chirality, sensor, tartaric acid

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1150 Twisted Bilayer Crescent Chiral Metasurface

Authors: Semere Araya Asefa

Abstract:

I described twisted bilayer crescent metasurfaces that link optical properties between two layers and enhance circular dichroism. The interactions between the metasurface layers cause circular dichroism. And we evaluated the parameters that affect the chiroptical response of the crescent

Keywords: chiroptical response, chiral metasurface, circular dichroism, chiral sensing

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1149 Synthesis and Characterization of Chiral Dopant Based on Schiff's Base Structure

Authors: Hong-Min Kim, Da-Som Han, Myong-Hoon Lee

Abstract:

CLCs (Cholesteric liquid crystals) draw tremendous interest due to their potential in various applications such as cholesteric color filters in LCD devices. CLC possesses helical molecular orientation which is induced by a chiral dopant molecules mixed with nematic liquid crystals. The efficiency of a chiral dopant is quantified by the HTP (helical twisting power). In this work, we designed and synthesized a series of new chiral dopants having a Schiff’s base imine structure with different alkyl chain lengths (butyl, hexyl and octyl) from chiral naphthyl amine by two-step reaction. The structures of new chiral dopants were confirmed by 1H-NMR and IR spectroscopy. The properties were investigated by DSC (differential scanning calorimetry calorimetry), POM (polarized optical microscopy) and UV-Vis spectrophotometer. These solid state chiral dopants showed excellent solubility in nematic LC (MLC-6845-000) higher than 17wt%. We prepared the CLC(Cholesteric Liquid Crystal) cell by mixing nematic LC (MLC-6845-000) with different concentrations of chiral dopants and injecting into the sandwich cell of 5μm cell gap with antiparallel alignment. The cholesteric liquid crystal phase was confirmed from POM, in which all the samples showed planar phase, a typical phase of the cholesteric liquid crystals. The HTP (helical twisting power) is one of the most important properties of CLC. We measured the HTP values from the UV-Vis transmittance spectra of CLC cells with varies chiral dopant concentration. The HTP values with different alkyl chains are as follows: butyl chiral dopant=29.8μm-1; hexyl chiral dopant= 31.8μm-1; octyl chiral dopant=27.7μm-1. We obtained the red, green and blue reflection color from CLC cells, which can be used as color filters in LCDs applications.

Keywords: cholesteric liquid crystal, color filter, display, HTP

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1148 Characterization of 3D Printed Re-Entrant Chiral Auxetic Geometries

Authors: Tatheer Zahra

Abstract:

Auxetic materials have counteractive properties due to re-entrant geometry that enables them to possess Negative Poisson’s Ratio (NPR). These materials have better energy absorbing and shock resistance capabilities as compared to conventional positive Poisson’s ratio materials. The re-entrant geometry can be created through 3D printing for convenient application of these materials. This paper investigates the mechanical properties of 3D printed chiral auxetic geometries of various sizes. Small scale samples were printed using an ordinary 3D printer and were tested under compression and tension to ascertain their strength and deformation characteristics. A maximum NPR of -9 was obtained under compression and tension. The re-entrant chiral cell size has been shown to affect the mechanical properties of the re-entrant chiral auxetics.

Keywords: auxetic materials, 3D printing, Negative Poisson’s Ratio, re-entrant chiral auxetics

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1147 Separation of Some Pyrethroid Insecticides by High-Performance Liquid Chromatography

Authors: Fairouz Tazerouti, Samira Ihadadene

Abstract:

Pyrethroids are synthetic pesticides that originated from the modification of natural pyrethrins to improve their biological activity and stability. They are a family of chiral pesticides with a large number of stereoisomers. Enantiomers of synthetic pyretroids present different insecticidal activity, toxicity against aquatic invertebrates and persistence in the environment so the development of rapid and sensitive chiral methods for the determination of different enantiomers is necessary. In this study, the separation of enantiomers of pyrethroid insecticides has been systematically studied using three commercially chiral high-performance liquid chromatography columns. Useful resolution was obtained for compounds with a variety of acid and alcohol moieties, and containing one to four chiral centres. The chromatographic behaviour of the diastereomers of some of these insecticides by using normal, polar and reversed mobile phase mode were also examined.

Keywords: pesticides, analysis, liquid chromatography, pyrethroids

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1146 Asymmetric Synthesis of β- and γ-Borylated Amines via Rh-Catalyzed Hydroboration of Allylamine Derivatives

Authors: Rukshani Wickrama-Arachchi, Tanner Metz, James M. Takacs

Abstract:

Amines bearing γ-stereocenters are important structural motifs found in many biologically active compounds. Regioselective Rh-catalyzed asymmetric hydroboration of acyclic allylamines is used to synthesize amines bearing chiral β- and γ-boronic esters yields up to 70% with 98:2 enantioselectivity. The major enantiomeric outcome can be independent of starting alkene geometry, revealing that cis/trans-isomerization of alkene can occur before hydroboration. Stereospecific transformations of the newly generated C-B bond illustrates the utility of these chiral synthons.

Keywords: allylamines, borylated amines, chiral amines, hydroboration, rhodium-catalysis

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1145 Separation of Fexofenadine Enantiomers Using Beta Cyclodextrin as Chiral Counter Ion in Mobile Phase

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

Abstract:

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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1144 Functionalization of Polypropylene with Chiral Monomer for Improving Hemocompatibility

Authors: Xiaodong Xu, Dan Zhao, Xiujuan Chang, Chunming Li, Huiyun Zhou, Xin Li, Qiang Shi, Shifang Luan, Jinghua Yin

Abstract:

Polypropylene (PP) is one of the most commonly used plastics because of its low density, outstanding mechanical properties, and low cost. However, its drawbacks such as low surface energy, poor dyeability, lack of chemical functionalities, and poor compatibility with polar polymers and inorganic materials, have restricted the application of PP. To expand its application in biomedical materials, functionalization is considered to be the most effective way. In this study, PP was functionalized with a chiral monomer, (S)-1-acryloylpyrrolidine-2-carboxylic acid ((S)-APCA), by free-radical grafting in the solid phase. The grafting degree of PP-g-APCA was determined by chemical titration method, and the chemical structure of functionalized PP was characterized by FTIR spectroscopy, which confirmed that the chiral monomer (S)-APCA was successfully grafted onto PP. Static water contact angle results suggested that the surface hydrophilicity of PP was significantly improved by solid phase grafting and assistance of surface water treatment. Protein adsorption and platelet adhesion results showed that hemocompatibility of PP was greatly improved by grafting the chiral monomer.

Keywords: functionalization, polypropylene, chiral monomer, hemocompatibility

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1143 Asymmetric Synthesis of Catalponol Using Chiral Iridium Catalyst

Authors: Takeyuki Suzuki, Ismiyarto, Da-Yang Zhou, Kaori Asano, Hiroaki Sasai

Abstract:

The development of catalytic asymmetric reaction is important for the synthesis of natural products. To construct the multiple stereogenic centers, the desymmetrization of meso compounds is powerful strategy for the synthesis of chiral molecules. Oxidative desymmetrization of meso diols using chiral iridium catalyst provides a chiral hydroxyl ketone. The reaction is practical and an environmentally benign method which does not require the use of stoichiometric amount of heavy metals. This time we report here catalytic asymmetric synthesis of catalponol based on tandem coupling of meso-diols and an aldehyde. The tandem reaction includes oxidative desymmetrization of meso-diols, aldol condensation with an aldehyde. The reaction of meso-diol, benzaldehyde in the presence of a catalytic amount of chiral Ir complex and CsOH in tetrahydrofuran afforded the desired benzylidene ketone in 82% yield with 96% ee (enantiomeric excess). Next, we applied this benzylidene ketone derivative to the synthesis of catalponol. The corresponding benzylidene ketone was obtained in 87% yield with 99% ee. Finally, catalponol was synthesized by the regio- and stereo-selective reduction of dienone moiety in good yield.

Keywords: catalponol, desymmetrization, iridium, oxidation

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1142 Comparative Investigation of Miniaturized Antennas Based on Chiral Slotted Ground Plane

Authors: Oussema Tabbabi, Mondher Laabidi, Fethi Choubani, J. David

Abstract:

This study presents a miniaturized antenna based on chiral metamaterials slotted ground plane. To decrease resonant frequency while keeping the antennas physical dimensions the same, we propose a two novel patch antennas with double Z and cross slots on the ground plane. The length of the each type of slot are also altered to investigate the effect on miniaturization performance. Resonance frequency reduction has been achieved nearly to 30% and 23% as well as size reduction of almost 28% and 22% for the double Z and the cross shape respectively.

Keywords: chiral metamaterials, miniaturized antenna, miniaturization, resonance frequency

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1141 Inverted Umbrella-type Chiral Non-coplanar Ferrimagnetic Structure in Co(NO₃)₂

Authors: O. Maximova, I. L. Danilovich, E. B. Deeva, K. Y. Bukhteev, A. A. Vorobyova, I. V. Morozov, O. S. Volkova, E. A. Zvereva, I. V. Solovyev, S. A. Nikolaev, D. Phuyal, M. Abdel-Hafiez, Y. C. Wang, J. Y. Lin, J. M. Chen, D. I. Gorbunov, K. Puzniak, B. Lake, A. N. Vasiliev

Abstract:

The low-dimensional magnetic systems tend to reveal exotic spin liquid ground states or form peculiar types of long-range order. Among systems of vivid interest are those characterized by the triangular motif in two dimensions. The realization of either ordered or disordered ground state in a triangular, honeycomb, or kagome lattices is are dictated by the competition of exchange interactions, also being sensitive to anisotropy and the spin value of magnetic ions. While the low-spin Heisenberg systems may arrive at a spin liquid long-range entangled quantum state with emergent gauge structures, the high-spin Ising systems may establish the rigid non-collinear structures. This study presents the case of chiral non-coplanar inverted umbrella-type ferrimagnet formed in cobalt nitrate Co(NO₃)₂ below T

Keywords: chiral magnetic structures, low dimensional magnetic systems, umbrella-type ferrimagnets, chiral non-coplanar magnetic structures

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1140 Nanoparticles Using in Chiral Analysis with Different Methods of Separation

Authors: Bounoua Nadia, Rebizi Mohamed Nadjib

Abstract:

Chiral molecules in relation to particular biological roles are stereoselective. Enantiomers differ significantly in their biochemical responses in a biological environment. Despite the current advancement in drug discovery and pharmaceutical biotechnology, the chiral separation of some racemic mixtures continues to be one of the greatest challenges because the available techniques are too costly and time-consuming for the assessment of therapeutic drugs in the early stages of development worldwide. Various nanoparticles became one of the most investigated and explored nanotechnology-derived nanostructures, especially in chirality, where several studies are reported to improve the enantiomeric separation of different racemic mixtures. The production of surface-modified nanoparticles has contributed to these limitations in terms of sensitivity, accuracy, and enantioselectivity that can be optimized and therefore makes these surface-modified nanoparticles convenient for enantiomeric identification and separation.

Keywords: chirality, enantiomeric recognition, selectors, analysis, surface-modified nanoparticles

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1139 High-Performance Liquid Chromatographic Method with Diode Array Detection (HPLC-DAD) Analysis of Naproxen and Omeprazole Active Isomers

Authors: Marwa Ragab, Eman El-Kimary

Abstract:

Chiral separation and analysis of omeprazole and naproxen enantiomers in tablets were achieved using high-performance liquid chromatographic method with diode array detection (HPLC-DAD). Kromasil Cellucoat chiral column was used as a stationary phase for separation and the eluting solvent consisted of hexane, isopropanol and trifluoroacetic acid in a ratio of: 90, 9.9 and 0.1, respectively. The chromatographic system was suitable for the enantiomeric separation and analysis of active isomers of the drugs. Resolution values of 2.17 and 3.84 were obtained after optimization of the chromatographic conditions for omeprazole and naproxen isomers, respectively. The determination of S-isomers of each drug in their dosage form was fully validated.

Keywords: chiral analysis, esomeprazole, S-Naproxen, HPLC-DAD

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1138 Estimation of Enantioresolution of Multiple Stereogenic Drugs Using Mobilized and/or Immobilized Polysaccharide-Based HPLC Chiral Stationary Phases

Authors: Mohamed Hefnawy, Abdulrahman Al-Majed, Aymen Al-Suwailem

Abstract:

Enantioseparation of drugs with multiple stereogenic centers is challenging. This study objectives to evaluate the efficiency of different mobilized and/or immobilized polysaccharide-based chiral stationary phases to separate enantiomers of some drugs containing multiple stereogenic centers namely indenolol, nadolol, labetalol. The critical mobile phase variables (composition of organic solvents, acid/base ratios) were carefully studied to compare the retention time and elution order of all isomers. Different chromatographic parameters such as capacity factor (k), selectivity (α) and resolution (Rs) were calculated. Experimental conditions and the possible chiral recognition mechanisms have been discussed.

Keywords: HPLC, polysaccharide columns, enantio-resolution, indenolol, nadolol, labetalol

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1137 Selective Circular Dichroism Sensor Based on the Generation of Quantum Dots for Cadmium Ion Detection

Authors: Pradthana Sianglam, Wittaya Ngeontae

Abstract:

A new approach for the fabrication of cadmium ion (Cd2+) sensor is demonstrated. The detection principle is based on the in-situ generation of cadmium sulfide quantum dots (CdS QDs) in the presence of chiral thiol containing compound and detection by the circular dichroism spectroscopy (CD). Basically, the generation of CdS QDs can be done in the presence of Cd2+, sulfide ion and suitable capping compounds. In addition, the strong CD signal can be recorded if the generated QDs possess chiral property (from chiral capping molecule). Thus, the degree of CD signal change depends on the number of the generated CdS QDs which can be related to the concentration of Cd2+ (excess of other components). In this work, we use the mixture of cysteamine (Cys) and L-Penicillamine (LPA) as the capping molecules. The strong CD signal can be observed when the solution contains sodium sulfide, Cys, LPA, and Cd2+. Moreover, the CD signal is linearly related to the concentration of Cd2+. This approach shows excellence selectivity towards the detection of Cd2+ when comparing to other cation. The proposed CD sensor provides low limit detection limits around 70 µM and can be used with real water samples with satisfactory results.

Keywords: circular dichroism sensor, quantum dots, enaniomer, in-situ generation, chemical sensor, heavy metal ion

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1136 Synthesis, Biological Evaluation and Molecular Modeling Studies on Chiral Chloroquine Analogues as Antimalarial Agents

Authors: Srinivasarao Kondaparla, Utsab Debnath, Awakash Soni, Vasantha Rao Dola, Manish Sinha, Kumkum Kumkum Srivastava, Sunil K. Puri, Seturam B. Katti

Abstract:

In a focused exploration, we have designed synthesized and biologically evaluated chiral conjugated new chloroquine (CQ) analogs with substituted piperazines as antimalarial agents. In vitro as well as in vivo studies revealed that compound 7c showed potent activity [for in vitro IC₅₀= 56.98nM (3D7), 97.76nM (K1); for in vivo (up to at the dose of 12.5 mg/kg); SI = 3510] as a new lead of antimalarial agent. Other compounds 6b, 6d, 7d, 7h, 8c, 8d, 9a, and 9c are also showing moderate activity against CQ-sensitive (3D7) strain and superior activity against resistant (K1) strain of P. falciparum. Furthermore, we have carried out docking and 3D-QSAR studies of all in-house data sets (168 molecules) of chiral CQ analogs to explain the structure activity relationships (SAR). Our new findings specified the significance of H-bond interaction with the side chain of heme for biological activity. In addition, the 3D-QSAR study against 3D7 strain indicated the favorable and unfavorable sites of CQ analogs for incorporating steric, hydrophobic and electropositive groups to improve the antimalarial activity.

Keywords: piperazines, CQ-sensitive strain-3D7, in-vitro and in-vivo assay, docking, 3D-QSAR

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1135 Chiral Diphosphine Ligands and Their Transition Metal Diphosphine Complexes in Asymmetric Catalysis

Authors: Shannen Lorraine, Paul Maragh, Tara Dasgupta, Kamaluddin Abdur-Rashid

Abstract:

(R)-(4,4',6,6'-tetramethoxybiphenyl-2,2'-diyl)bis(diphenylphosphine) (R-Ph-Garphos), and (S)-(4,4',6,6'-tetramethoxybiphenyl-2,2'-diyl)bis(diphenylphosphine) (S-Ph-Garphos) are novel, nucleophilic, chiral atropisomeric ligands. The research explored the synthesis of chiral transition metal complexes containing these ligands and their applications in various asymmetric catalytic transformations. Herein, the transition metal complexes having ruthenium(II), rhodium(I) and iridium(I) metal centres will be discussed. These are air stable complexes and were characterized by CHN analysis, 1H, 13C, and 31P NMR spectroscopy, and polarimetry. Currently, there is an emphasis on 'greener' catalysts and the need for 'green' solvents in asymmetric catalysis. As such, the Ph-Garphos ligands were demethylated thereby introducing hydroxyl moieties unto the ligand scaffold. The facile tunability of the biaryl diphosphines led to the preparation of the (R)-(4,4',6,6'-tetrahydroxybiphenyl-2,2'-diyl)bis(diphenylphosphine) (R-Ph-Garphos-OH), and (S)-(4,4',6,6'-tetrahydroxybiphenyl-2,2'-diyl)bis(diphenylphosphine) (S-Ph-Garphos-OH) ligands. These were successfully characterized by CHN analysis, 1H, 13C, and 31P NMR spectroscopy, and polarimetry. The use of the Ph-Garphos and Ph-Garphos-OH ligands and their transition metal complexes in asymmetric hydrogenations will be reported. Additionally, the scope of the research will highlight the applicability of the Ph-Garphos-OH ligand and its transitional metal complexes as 'green' catalysts.

Keywords: catalysis, asymmetric hydrogenation, diphosphine transition metal complexes, Ph-Garphos ligands

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1134 Capacity Optimization in Cooperative Cognitive Radio Networks

Authors: Mahdi Pirmoradian, Olayinka Adigun, Christos Politis

Abstract:

Cooperative spectrum sensing is a crucial challenge in cognitive radio networks. Cooperative sensing can increase the reliability of spectrum hole detection, optimize sensing time and reduce delay in cooperative networks. In this paper, an efficient central capacity optimization algorithm is proposed to minimize cooperative sensing time in a homogenous sensor network using OR decision rule subject to the detection and false alarm probabilities constraints. The evaluation results reveal significant improvement in the sensing time and normalized capacity of the cognitive sensors.

Keywords: cooperative networks, normalized capacity, sensing time

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1133 Transformation of Glycals to Chiral Fused Aromatic Cores via Annulative π-Extension Reaction with Arynes

Authors: Nazar Hussain, Debaraj Mukherjee

Abstract:

Carbohydrate-derived chiral intermediates which contain arrays of defined stereocenters have found enormous applications in organic synthesis due to their inherent functional group, stereochemical and structural diversities as well as their ready availability. Stereodiversity of these classes of molecules has motivated synthetic organic chemistry over the years. One major challenge is control of relative configuration during construction of acyclic fragments. Here, we show that The Diels Alder addition of arynes to appropriately substituted vinyl/aryl glycals followed by π-extension via pyran ring opening smoothly furnished meta-disubstituted fused aromatic cores containing a stereo-defined orthogonally protected chiral side chain. The method is broad in terms of aryl homologation affording benzene, naphthalene, and phenanthrene derivatives. Base-induced deprotonation followed by cleavage of the allylic C-O bond appears to be the crucial steps leading to the development of aromaticity, which is the driving force behind the annulative π-extension process. The present protocol can be used for the synthesis of meta-disubstituted naphthalene aldehydes and substrates for aldolases.

Keywords: vinyl/C-2 aryl glycal, arynes, cyclization, ring opening

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1132 Effect of Using a Mixture of Al2O3 Nanoparticles and 3-Aminopropyltriethoxysilane as the Sensing Membrane for Polysilicon Wire on pH Sensing

Authors: You-Lin Wu, Zong-Xian Wu, Jing-Jenn Lin, Shih-Hung Lin

Abstract:

In this work, a polysilicon wire (PSW) coated with a mixture of 3-aminopropyltriethoxysilane (r-APTES) and Al2O3 nanoparticles as the sensing membrane prepared with various Al2O3/r-APTES and dispersing agent/r-APTES ratios for pH sensing is studied. The r-APTES and dispersed Al2O3 nanoparticles mixture was directly transferred to PSW surface by solution phase deposition (SPD). It is found that using a mixture of Al2O3 nanoparticles and r-APTES as the sensing membrane help in improving the pH sensing of the PSW sensor and a 5 min SPD deposition time is the best. Dispersing agent is found to be necessary for better pH sensing when preparing the mixture of Al2O3 nanoparticles and r-APTES. The optimum condition for preparing the mixture is found to be Al2O3/r-APTES ratio of 2% and dispersing agent/r-APTES ratio of 0.3%.

Keywords: al2o3 nanoparticles, ph sensing, polysilicon wire sensor, r-aptes

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1131 Reliability Factors Based Fuzzy Logic Scheme for Spectrum Sensing

Authors: Tallataf Rasheed, Adnan Rashdi, Ahmad Naeem Akhtar

Abstract:

The accurate spectrum sensing is a fundamental requirement of dynamic spectrum access for deployment of Cognitive Radio Network (CRN). To acheive this requirement a Reliability factors based Fuzzy Logic (RFL) Scheme for Spectrum Sensing has been proposed in this paper. Cognitive Radio User (CRU) predicts the presence or absence of Primary User (PU) using energy detector and calculates the Reliability factors which are SNR of sensing node, threshold of energy detector and decision difference of each node with other nodes in a cooperative spectrum sensing environment. Then the decision of energy detector is combined with Reliability factors of sensing node using Fuzzy Logic. These Reliability Factors used in RFL Scheme describes the reliability of decision made by a CRU to improve the local spectrum sensing. This Fuzzy combining scheme provides the accuracy of decision made by sensornode. The simulation results have shown that the proposed technique provide better PU detection probability than existing Spectrum Sensing Techniques.

Keywords: cognitive radio, spectrum sensing, energy detector, reliability factors, fuzzy logic

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1130 Synthesis of (S)-Naproxen Based Amide Bond Forming Chiral Reagent and Application for Liquid Chromatographic Resolution of (RS)-Salbutamol

Authors: Poonam Malik, Ravi Bhushan

Abstract:

This work describes a very efficient approach for synthesis of activated ester of (S)-naproxen which was characterized by UV, IR, ¹HNMR, elemental analysis and polarimetric studies. It was used as a C-N bond forming chiral derivatizing reagent for further synthesis of diastereomeric amides of (RS)-salbutamol (a β₂ agonist that belongs to the group β-adrenolytic and is marketed as racamate) under microwave irradiation. The diastereomeric pair was separated by achiral phase HPLC, using mobile phase in gradient mode containing methanol and aqueous triethylaminephosphate (TEAP); separation conditions were optimized with respect to pH, flow rate, and buffer concentration and the method of separation was validated as per International Council for Harmonisation (ICH) guidelines. The reagent proved to be very effective for on-line sensitive detection of the diastereomers with very low limit of detection (LOD) values of 0.69 and 0.57 ng mL⁻¹ for diastereomeric derivatives of (S)- and (R)-salbutamol, respectively. The retention times were greatly reduced (2.7 min) with less consumption of organic solvents and large (α) as compared to literature reports. Besides, the diastereomeric derivatives were separated and isolated by preparative HPLC; these were characterized and were used as standard reference samples for recording ¹HNMR and IR spectra for determining absolute configuration and elution order; it ensured the success of diastereomeric synthesis and established the reliability of enantioseparation and eliminated the requirement of pure enantiomer of the analyte which is generally not available. The newly developed reagent can suitably be applied to several other amino group containing compounds either from organic syntheses or pharmaceutical industries because the presence of (S)-Npx as a strong chromophore would allow sensitive detection.This work is significant not only in the area of enantioseparation and determination of absolute configuration of diastereomeric derivatives but also in the area of developing new chiral derivatizing reagents (CDRs).

Keywords: chiral derivatizing reagent, naproxen, salbutamol, synthesis

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1129 Chiral Amine Synthesis and Recovery by Using High Molecular Weight Amine Donors

Authors: Claudia Matassa, Matthias Hohne, Dominic Ormerod, Yamini Satyawali

Abstract:

Chiral amines integrate the backbone of several active pharmaceutical ingredients (APIs) used in modern medicine for the treatment of a vast range of diseases. Despite the demand, their synthesis remains challenging. Besides a range of chemicals and enzymatical methods, chiral amine synthesis using transaminases (EC 2.6.1.W) represents a useful alternative to access this important class of compounds. Even though transaminases exhibit excellent stereo and regioselectivity and the potential for high yield, the reaction suffers from a number of challenges, including the thermodynamic equilibrium, product inhibition, and low substrate solubility. In this work, we demonstrate a membrane assisted strategy for addressing these challenges. It involves the use of high molecular weight (HMW) amine donors for the transaminase-catalyzed synthesis of 4-phenyl-2-butylamine in both aqueous and organic solvent media. In contrast to common amine donors such as alanine or isopropylamine, these large molecules, provided in excess for thermodynamic equilibrium shifting, are easily retained by commercial nanofiltration membranes; thus a selective permeation of the desired smaller product amine is possible. The enzymatic transamination in aqueous media, combined with selective product removal shifted the equilibrium enhancing substrate conversion by an additional 25% compared to the control reaction. Along with very efficient amine product removal, there was undesirable loss of ketone substrate and low product concentration was achieved. The system was therefore further improved by performing the reaction in organic solvent (n-heptane). Coupling the reaction system with membrane-assisted product removal resulted in a highly concentrated and relatively pure ( > 97%) product solution. Moreover, a product yield of 60% was reached, compared to 15% without product removal.

Keywords: amine donor, chiral amines, in situ product removal, transamination

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1128 Performance of Nakagami Fading Channel over Energy Detection Based Spectrum Sensing

Authors: M. Ranjeeth, S. Anuradha

Abstract:

Spectrum sensing is the main feature of cognitive radio technology. Spectrum sensing gives an idea of detecting the presence of the primary users in a licensed spectrum. In this paper we compare the theoretical results of detection probability of different fading environments like Rayleigh, Rician, Nakagami-m fading channels with the simulation results using energy detection based spectrum sensing. The numerical results are plotted as P_f Vs P_d for different SNR values, fading parameters. It is observed that Nakagami fading channel performance is better than other fading channels by using energy detection in spectrum sensing. A MATLAB simulation test bench has been implemented to know the performance of energy detection in different fading channel environment.

Keywords: spectrum sensing, energy detection, fading channels, probability of detection, probability of false alarm

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1127 Method Development and Validation for Quantification of Active Content and Impurities of Clodinafop Propargyl and Its Enantiomeric Separation by High-Performance Liquid Chromatography

Authors: Kamlesh Vishwakarma, Bipul Behari Saha, Sunilkumar Sing, Abhishek Mishra, Sreenivas Rao

Abstract:

A rapid, sensitive and inexpensive method has been developed for complete analysis of Clodinafop Propargyl. Clodinafop Propargyl enantiomers were separated on chiral column, Chiral Pak AS-H (250 mm. 4.6mm x 5µm) with mobile phase n-hexane: IPA (96:4) at flow rate 1.5 ml/min. The effluent was monitored by UV detector at 230 nm. Clodinafop Propagyl content and impurity quantification was done with reverse phase HPLC. The present study describes a HPLC method using simple mobile phase for the quantification of Clodinafop Propargyl and its impurities. The method was validated and found to be accurate, precise, convenient and effective. Moreover, the lower solvent consumption along with short analytical run time led to a cost effective analytical method.

Keywords: Clodinafop Propargyl, method, validation, HPLC-UV

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1126 Radio-Frequency Technologies for Sensing and Imaging

Authors: Cam Nguyen

Abstract:

Rapid, accurate, and safe sensing and imaging of physical quantities or structures finds many applications and is of significant interest to society. Sensing and imaging using radio-frequency (RF) techniques, particularly, has gone through significant development and subsequently established itself as a unique territory in the sensing world. RF sensing and imaging has played a critical role in providing us many sensing and imaging abilities beyond our human capabilities, benefiting both civilian and military applications - for example, from sensing abnormal conditions underneath some structures’ surfaces to detection and classification of concealed items, hidden activities, and buried objects. We present the developments of several sensing and imaging systems implementing RF technologies like ultra-wide band (UWB), synthetic-pulse, and interferometry. These systems are fabricated completely using RF integrated circuits. The UWB impulse system operates over multiple pulse durations from 450 to 1170 ps with 5.5-GHz RF bandwidth. It performs well through tests of various samples, demonstrating its usefulness for subsurface sensing. The synthetic-pulse system operating from 0.6 to 5.6 GHz can assess accurately subsurface structures. The synthetic-pulse system operating from 29.72-37.7 GHz demonstrates abilities for various surface and near-surface sensing such as profile mapping, liquid-level monitoring, and anti-personnel mine locating. The interferometric system operating at 35.6 GHz demonstrates its multi-functional capability for measurement of displacements and slow velocities. These RF sensors are attractive and useful for various surface and subsurface sensing applications. This paper was made possible by NPRP grant # 6-241-2-102 from the Qatar National Research Fund (a member of Qatar Foundation). The statements made herein are solely the responsibility of the authors.

Keywords: RF sensors, radars, surface sensing, subsurface sensing

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1125 Highly Sensitive and Selective H2 Gas Sensor Based on Pd-Pt Decorated Nanostructured Silicon Carbide Thin Films for Extreme Environment Application

Authors: Satyendra Mourya, Jyoti Jaiswal, Gaurav Malik, Brijesh Kumar, Ramesh Chandra

Abstract:

Present work describes the fabrication and sensing characteristics of the Pd-Pt decorated nanostructured silicon carbide (SiC) thin films on anodized porous silicon (PSi) substrate by RF magnetron sputtering. The gas sensing performance of Pd-Pt/SiC/PSi sensing electrode towards H2 gas under low (10–400 ppm) detection limit and high operating temperature regime (25–600 °C) were studied in detail. The chemiresistive sensor exhibited high selectivity, good sensing response, fast response/recovery time with excellent stability towards H2 at high temperature. The selectivity measurement of the sensing electrode was done towards different oxidizing and reducing gases and proposed sensing mechanism discussed in detail. Therefore, the investigated Pd-Pt/SiC/PSi structure may be a highly sensitive and selective hydrogen gas sensing electrode for deployment in extreme environment applications.

Keywords: RF Sputtering, silicon carbide, porous silicon, hydrogen gas sensor

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1124 Persistent Homology of Convection Cycles in Network Flows

Authors: Minh Quang Le, Dane Taylor

Abstract:

Convection is a well-studied topic in fluid dynamics, yet it is less understood in the context of networks flows. Here, we incorporate techniques from topological data analysis (namely, persistent homology) to automate the detection and characterization of convective/cyclic/chiral flows over networks, particularly those that arise for irreversible Markov chains (MCs). As two applications, we study convection cycles arising under the PageRank algorithm, and we investigate chiral edges flows for a stochastic model of a bi-monomer's configuration dynamics. Our experiments highlight how system parameters---e.g., the teleportation rate for PageRank and the transition rates of external and internal state changes for a monomer---can act as homology regularizers of convection, which we summarize with persistence barcodes and homological bifurcation diagrams. Our approach establishes a new connection between the study of convection cycles and homology, the branch of mathematics that formally studies cycles, which has diverse potential applications throughout the sciences and engineering.

Keywords: homology, persistent homolgy, markov chains, convection cycles, filtration

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1123 Multifunctional Composite Structural Elements for Sensing and Energy Harvesting

Authors: Amir H. Alavi, Kaveh Barri, Qianyun Zhang

Abstract:

This study presents a new generation of lightweight and mechanically tunable structural composites with sensing and energy harvesting functionalities. This goal is achieved by integrating metamaterial and triboelectric energy harvesting concepts. Proof-of-concept polymeric beam prototypes are fabricated using 3D printing methods based on the proposed concept. Experiments and theoretical analyses are conducted to quantitatively investigate the mechanical and electrical properties of the designed multifunctional beams. The results show that these integrated structural elements can serve as nanogenerators and distributed sensing mediums without a need to incorporating any external sensing modules and electronics. The feasibility of design self-sensing and self-powering structural elements at multiscale for next generation infrastructure systems is further discussed.

Keywords: multifunctional structures, composites, metamaterial, triboelectric nanogenerator, sensors, structural health monitoring, energy harvesting

Procedia PDF Downloads 165
1122 Condition Monitoring of Railway Earthworks using Distributed Rayleigh Sensing

Authors: Andrew Hall, Paul Clarkson

Abstract:

Climate change is predicted to increase the number of extreme weather events intensifying the strain on Railway Earthworks. This paper describes the use of Distributed Rayleigh Sensing to monitor low frequency activity on a vulnerable earthworks sectionprone to landslides alongside a railway line in Northern Spain. The vulnerable slope is instrumented with conventional slope stability sensors allowing an assessment to be conducted of the application of Distributed Rayleigh Sensing as an earthwork condition monitoring tool to enhance the resilience of railway networks.

Keywords: condition monitoring, railway earthworks, distributed rayleigh sensing, climate change

Procedia PDF Downloads 169