Search results for: Raman spectroscopy

Authors: Diptiman Dinda, Shyamal Kumar Saha

Abstract:

In the 21st century, sensitive and selective detection of trace amounts of explosives has become a serious problem. Generally, nitro compound and its derivatives are being used worldwide to prepare different explosives. Recently, TNP (2, 4, 6 trinitrophenol) is the most commonly used constituent to prepare powerful explosives all over the world. It is even powerful than TNT or RDX. As explosives are electron deficient in nature, it is very difficult to detect one separately from a mixture. Again, due to its tremendous water solubility, detection of TNP in presence of other explosives from water is very challenging. Simple instrumentation, cost-effective, fast and high sensitivity make fluorescence based optical sensing a grand success compared to other techniques. Graphene oxide (GO), with large no of epoxy grps, incorporate localized nonradiative electron-hole centres on its surface to give very weak fluorescence. In this work, GO is functionalized with 2, 6-diamino pyridine to remove those epoxy grps. through SN2 reaction. This makes GO into a bright blue luminescent fluorophore (DAP/rGO) which shows an intense PL spectrum at ∼384 nm when excited at 309 nm wavelength. We have also characterized the material by FTIR, XPS, UV, XRD and Raman measurements. Using this as fluorophore, a large fluorescence quenching (96%) is observed after addition of only 200 µL of 1 mM TNP in water solution. Other nitro explosives give very moderate PL quenching compared to TNP. Such high selectivity is related to the operation of FRET mechanism from fluorophore to TNP during this PL quenching experiment. TCSPC measurement also reveals that the lifetime of DAP/rGO drastically decreases from 3.7 to 1.9 ns after addition of TNP. Our material is also quite sensitive to 125 ppb level of TNP. Finally, we believe that this graphene based luminescent material will emerge a new class of sensing materials to detect trace amounts of explosives from aqueous solution.

Keywords: graphene, functionalization, fluorescence quenching, FRET, nitroexplosive detection

Procedia PDF Downloads 440

Authors: Maryam Kiani, Abdul Basit Kiani

Abstract:

Simple hydrothermal method to synthesize new nanocomposites consisting of nitrogen-doped graphene and NiFe₂O₄. By analyzing the X-Ray Powder Diffraction (XRD) images, we confirmed that the NiFe₂O₄ phase is pure and has a Face Centered Cubic (FCC) structure. The average size of the NiFe₂O₄ nanoparticles is approximately 40±2 nm. Additionally, we used X-ray photoelectron spectroscopy (XPS) to study the surface chemical composition and cation oxidation states of both the NiFe₂O₄ nanoparticles and the nitrogen-doped graphene/NiFe₂O₄ nanocomposites. A magnetic interaction between nitrogen doped graphene/NiFe₂O₄ was studied. Increases in hydrothermal synthesis temperature lead to the improved crystalline structure of NiFe₂O₄ nanoparticles, which improves the magnetic properties.

Keywords: nickel ferrite spinal, nitrogen doped graphene, magnetic nanocomposite, hydrothermal synthesis

Procedia PDF Downloads 131

Authors: Shrikaant Kulkarni, Akshata Naik Nimbalkar

Abstract:

In this worki a method protocol has been developed for the synthesis of innovative Co3O4 material by using a method of chemical synthesis followed by calcination. The effect of calcination temperature on the morphology, structure and catalytic performance on material in question is investigated by using characterization tools like scanning electron microscopy (SEM), X-ray diffraction (XRD) spectroscopy and electrochemical techniques. The SEM images reveal that the morphology of the Co3O4 material undergoes a change from the rod to a beadlike shape on calcination at temperature of 700 °C. The XRD image shows that although the morphology of synthesized Co3O4 material exhibits a cubic phase but it differs in crystallinity depending upon morphology. Similarly spherical beadlike Co3O4 material has exhibited better activity than its rodlike counterpart which is reflected from electrochemical findings. Further, its performance in terms of bifunctional nature and hlods a lot much of promise as a excellent electrode material in the next generation batteries and fuel cells.

Keywords: bifunctional, next generation material, Co3O4, XRD

Procedia PDF Downloads 379

Authors: Fatemeh Rezaei, Babak Shokri

Abstract:

In this study, PMMA films are modified by oxygen plasma treatment for biomedical applications. The plasma generator is capacitively coupled radio frequency (13.56 MHz) power source. The oxygen pressure and gas flow rate are kept constant at 40 mTorr and 30 sccm, respectively and samples are treated for 2 minutes. Hydrophilicity and biocompatibility of PMMA films are studied before and after treatments in different applied powers (10-80 W). In order to monitor the plasma process, the optical emission spectroscopy is used. The wettability and cellular response of samples are investigated by water contact angle (WCA) analysis and MTT assay, respectively. Also, surface free energy (SFE) variations are studied based on the contact angle measurements of three liquids. It is found that RF oxygen plasma treatment enhances the biocompatibility and also hydrophilicity of PMMA films.

Keywords: cellular response, hydrophilicity, MTT assay, PMMA, RF plasma

Procedia PDF Downloads 671

Authors: Irlana C. do Mar, Thayna A. Ferreira, Dayane S. Rezende, Bruno A. M. Figueira, José M. R. Mercury

Abstract:

This work presents a low-cost Mn starting material to synthesis manganese oxide octahedral molecular sieve with Mg²⁺ in the tunnel (Mg-OMS-1), based on the Mn residues from Carajás Mineral Province (Amazon, Brazil). After hydrothermal and cation exchange procedures, the Mn residues transformed to a single phase, Mg-OMS-1. The raw material and the synthesis processes were analyzed by means of X-ray diffraction (XRD), Scanning electron microscopy (SEM) and Infrared spectroscopy (FTIR). The tunnel structure was synthesized hydrothermally at 180 °C for three days without impurities. According to the XRD analysis, the formation of crystalline Mg-OMS-1 was identified through reflections at 9.8º, 12º and 18º (2θ), as well as a thermal stability around 300 ºC. The SEM analysis indicated that the final product presents good crystallinity with a homogeneous size. In addition, an intense and diagnostic FTIR band was identified at 515 cm⁻¹ related to the MnO₆ octahedral stretching vibrations.

Keywords: Mn residues , Octahedral Molecular Sieve, Synthesis, Characterization

Procedia PDF Downloads 192

Authors: Ali Akbar Kazemi Asl, Mansour Rahsepar

Abstract:

Mesoporous carbon nanospheres (MCNs) with uniform particle size distribution having an average of 290 nm and large specific surface area (274.4 m²/g) were synthesized by a one-step hydrothermal method followed by the calcination process and then utilized as an enzyme-free glucose biosensor. Morphology, crystal structure, and porous nature of the synthesized nanospheres were characterized by scanning electron microscopy (SEM), X-Ray diffraction (XRD), and Brunauer–Emmett–Teller (BET) analysis, respectively. Also, the electrochemical performance of the MCNs@GCE electrode for the measurement of glucose concentration in alkaline media was investigated by electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), and chronoamperometry (CA). MCNs@GCE electrode shows good sensing performance, including a rapid glucose oxidation response within 3.1 s, a wide linear range of 0.026-12 mM, a sensitivity of 212.34 μA.mM⁻¹.cm⁻², and a detection limit of 25.7 μM with excellent selectivity.

Keywords: biosensor, electrochemical, glucose, mesoporous carbon, non-enzymatic

Procedia PDF Downloads 190

Authors: Bhupinder Kaur, O. P. Pandey

Abstract:

An automobile industry is using variety of materials for better comfort and utility. The present work describes the details of failure analysis done for windshield glass of a four-wheeler class. The failure occurred in two different models of the heavy duty class of four wheelers, which analysed separately. The company reported that the failure has occurred only in their rear windshield when vehicles parked under shade for several days. These glasses were characterised by dilatometer, differential thermal analyzer, and X-ray diffraction. The glasses were further investigated under scanning electron microscope with energy dispersive X-ray spectroscopy and X-ray dot mapping. The microstructural analysis of the glasses done at the surface as well as at the fractured area indicates that carbon as an impurity got segregated as banded structure throughout the glass. Since carbon absorbs higher heat, it causes thermal mismatch to the entire glass system, and glass shattered down. In this work, the details of sequential analysis done to predict the cause of failure are present.

Keywords: failure, windshield, thermal mismatch, carbon

Procedia PDF Downloads 247

Authors: JongWon Han, NoHoon Kim, HyoIk Ahn, HaeWoo Lee

Abstract:

In this study, shielded metal arc welding was performed as a function of Nb content at 2.24 wt%, 3.25 wt%, and 4.26 wt%. The microstructure was observed using scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDS) and showed the development of a columnar dendrite structure in the specimen having the least Nb content. From the hardness test, the hardness value was confirmed to reduce with decreasing Nb content. From electron backscatter diffraction (EBSD) analysis, the largest grain size was found in the specimen with Nb content of 2.24 wt%. The potentiodynamic polarization test was carried out to determine the pitting corrosion resistance; there was no significant difference in the pitting corrosion resistance with increasing Nb content. To evaluate the degree of sensitization to intergranular corrosion, the Double Loop Electrochemical Potentiodynamic Reactivation(DL-EPR test) was conducted. A similar degree of sensitization was found in two specimens except with a Nb content of 2.24 wt%, while a relatively high degree of sensitization was found in the specimen with a Nb content of 2.24 wt%.

Keywords: inconel 625, Nb content, potentiodynamic test, DL-EPR test

Procedia PDF Downloads 308

Authors: Ambrish Singh

Abstract:

The corrosion inhibition performance of pyran (AP) and benzimidazole (BI) derivatives on J55 steel in 3.5% NaCl solution saturated with CO₂ was investigated by electrochemical, weight loss, surface characterization, and theoretical studies. The electrochemical studies included electrochemical impedance spectroscopy (EIS), potentiodynamic polarization (PDP), electrochemical frequency modulation (EFM), and electrochemical frequency modulation trend (EFMT). Surface characterization was done using contact angle, scanning electron microscopy (SEM), and atomic force microscopy (AFM) techniques. DFT and molecular dynamics (MD) studies were done using Gaussian and Materials Studio softwares. All the studies suggested the good inhibition by the synthesized inhibitors on J55 steel in 3.5% NaCl solution saturated with CO₂ due to the formation of a protective film on the surface. Molecular dynamic simulation was applied to search for the most stable configuration and adsorption energies for the interaction of the inhibitors with Fe (110) surface.

Keywords: corrosion, inhibitor, EFM, AFM, DFT, MD

Procedia PDF Downloads 105

Authors: Flavio A. F. Da Ponte, Jackson Q. Malveira, Monica C. G. Albuquerque

Abstract:

In recent years a worldwide interest in renewable resources from the biomass has spurred the industry. In this work the chemical structure of oleic acid chains was modified by homogeneous and heterogeneous catalysis in order to produce esters. The homogeneous epoxidation was carried out at H2O2 to oleic acid unsaturation molar ratio of 20:1. The reaction temperature was 338 K and reaction time 16 h. Formic acid was used as catalyst. For heterogeneous catalysis reaction temperature was 343 K and reaction time 24 h. The esters production was carried out by heterogeneous catalysis of the epoxidized oleic acid and butanol using Mg/SBA-15 as catalyst. The resulting products were confirmed by NMR (1H and 13C) and FTIR spectroscopy. The products were characterized before and after each reaction. The catalysts were characterized by X-ray diffraction, X-ray fluorescence, thermogravimetric analysis (TGA) and BET surface areas. The results were satisfactory for the bioproducts formed.

Keywords: acid oleic, bioproduct, esters, epoxidation

Procedia PDF Downloads 356

Authors: M. Mujahid, Omar A. Al-Hartomy

Abstract:

Ag-doped ZnO2 loaded on the Pt-carbon spheres have been synthesized and characterized by standard analytical techniques. i.e., UV-Vis spectroscopy, X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). In order to find the effect of loading of Ag doping on ZnO2, the concentration of Ag was varied from 0-3.5%. The XRD analysis showed that the obtained particles are anatase phase. The SEM images showed Ag-doped ZnO2 are loaded on the surface of the Pt-carbon spheres. The photocatalytic activity of the synthesized particles was tested by studying the degradation of methyl orange dye and 4-chlorophenol as a function of time on irradiation in aqueous suspension. Ag-doped ZnO2@Pt-carbon sphere particle with platinum concentration of 3.0 % showed the highest photocatalytic activity as compared to the other Ag concentrations for the degradation of methyl orange and 4-chlorophenol.

Keywords: Ag-ZnO2, Pt-carbon spheres, degradation, methyl orange, 4-chlorophenol

Procedia PDF Downloads 370

Authors: Dhuha Albusalih, David Weston, Simon Gill

Abstract:

Nanocomposites Co-SiC with well dispersed nanoparticles and Co nano grain size has produced using Pulse Reverse Plating (PRP) and using anionic surfactant. Different particle contents of nanocomposites were produced by altering the plating parameters. The method allows great control over the level of nanoparticles in the coating, without changing bath chemistry. Examination by Scanning Electron Microscopy (SEM), Energy Dispersive Spectroscopy (EDX), TEM and X-Ray Diffraction (XRD) analysis was performed to characterize and study the strengthening mechanisms of these nanocomposites. The primary strengthening mechanisms were shown to be grain refinement and dispersion strengthening. Tribological performances of the produced electroplated nanocomposite Co-SiC coatings were examined. Results showed that the coating with the higher volume fraction (vol. %) of SiC and the smallest grain size has the higher hardness and low wear rate.

Keywords: nanocomposites, pulse reverse plating, tribological performance of cobalt nanocomposites

Procedia PDF Downloads 307

Authors: Md. Hafezur Rahaman, Mohd. Maniruzzaman, Md. Shadiqul Islam, Md. Masud Rana

Abstract:

With the growth of environmental awareness, enormous researches are running to develop the next generation materials based on sustainability, eco-competence, and green chemistry to preserve and protect the environment. Due to biodegradability and biocompatibility, poly (L-lactic acid) (PLLA) has a great interest in ecological and medical applications. Also, cellulose is one of the most abundant biodegradable, renewable polymers found in nature. It has several advantages such as low cost, high mechanical strength, biodegradability and so on. Recently, an immense deal of attention has been paid for the scientific and technological development of α-cellulose based composite material. PLLA could be used for grafting of cellulose to improve the compatibility prior to the composite preparation. Here it is quite difficult to form a bond between lower hydrophilic molecules like PLLA and α-cellulose. Dimmers and oligomers can easily be grafted onto the surface of the cellulose by ring opening or polycondensation method due to their low molecular weight. In this research, α-cellulose extracted from jute fiber is grafted with oligo(D-lactic acid) (ODLA) via graft polycondensation reaction in presence of para-toluene sulphonic acid and potassium persulphate in toluene at 130°C for 9 hours under 380 mmHg. Here ODLA is synthesized by ring opening polymerization of D-lactides in the presence of stannous octoate (0.03 wt% of lactide) and D-lactic acids at 140°C for 10 hours. Composites of PLLA with ODLA grafted α-cellulose are prepared by solution mixing and film casting method. Confirmation of grafting was carried out through FTIR spectroscopy and SEM analysis. A strongest carbonyl peak of FTIR spectroscopy at 1728 cm⁻¹ of ODLA grafted α-cellulose confirms the grafting of ODLA onto α-cellulose which is absent in α-cellulose. It is also observed from SEM photographs that there are some white areas (spot) on ODLA grafted α-cellulose as compared to α-cellulose may indicate the grafting of ODLA and consistent with FTIR results. Analysis of the composites is carried out by FTIR, SEM, WAXD and thermal gravimetric analyzer. Most of the FTIR characteristic absorption peak of the composites shifted to higher wave number with increasing peak area may provide a confirmation that PLLA and grafted cellulose have better compatibility in composites via intermolecular hydrogen bonding and this supports previously published results. Grafted α-cellulose distributions in composites are uniform which is observed by SEM analysis. WAXD studied show that only homo-crystalline structures of PLLA present in the composites. Thermal stability of the composites is enhanced with increasing the percentages of ODLA grafted α-cellulose in composites. As a consequence, the resultant composites have a resistance toward the thermal degradation. The effects of length of the grafted chain and biodegradability of the composites will be studied in further research.

Keywords: α-cellulose, composite, graft polycondensation, oligo(D-lactic acid), poly(L-lactic acid)

Procedia PDF Downloads 117

Authors: Brajendra S. Sengar, Vivek Garg, Gaurav Siddharth, Nisheka Anadkat, Amitesh Kumar, Shaibal Mukherjee

Abstract:

The optimal band gap (~ 1 to 1.5 eV) and high absorption coefficient ~104 cm⁻¹ has made Cu₂ZnSn(S,Se)₄ (CZTSSe) films as one of the most promising absorber materials in thin-film photovoltaics. Additionally, CZTSSe consists of elements that are abundant and non-toxic, makes it even more favourable. The CZTSSe thin films are grown at 100 to 500ᵒC substrate temperature (Tsub) on Soda lime glass (SLG) substrate by Elettrorava dual ion beam sputtering (DIBS) system by utilizing a target at 2.43x10⁻⁴ mbar working pressure with RF power of 45 W in argon ambient. The chemical composition, depth profiling, structural properties and optical properties of these CZTSSe thin films prepared on SLG were examined by energy dispersive X-ray spectroscopy (EDX, Oxford Instruments), Hiden secondary ion mass spectroscopy (SIMS) workstation with oxygen ion gun of energy up to 5 keV, X-ray diffraction (XRD) (Rigaku Cu Kα radiation, λ=.154nm) and Spectroscopic Ellipsometry (SE, M-2000D from J. A. Woollam Co., Inc). It is observed that from that, the thin films deposited at Tsub=200 and 300°C show Cu-poor and Zn-rich states (i.e., Cu/(Zn + Sn) < 1 and Zn/Sn > 1), which is not the case for films grown at other Tsub. It has been reported that the CZTSSe thin films with the highest efficiency are typically at Cu-poor and Zn-rich states. The values of band gap in the fundamental absorption region of CZTSSe are found to be in the range of 1.23-1.70 eV depending upon the Cu/(Zn+Sn) ratio. It is also observed that there is a decline in optical band gap with the increase in Cu/(Zn+Sn) ratio (evaluated from EDX measurement). Cu-poor films are found to have higher optical band gap than Cu-rich films. The decrease in the band gap with the increase in Cu content in case of CZTSSe films may be attributed to changes in the extent of p-d hybridization between Cu d-levels and (S, Se) p-levels. CZTSSe thin films with Cu/(Zn+Sn) ratio in the range 0.86–1.5 have been successfully deposited using DIBS. Optical band gap of the films is found to vary from 1.23 to 1.70 eV based on Cu/(Zn+Sn) ratio. CZTSe films with Cu/ (Zn+Sn) ratio of .86 are found to have optical band gap close to the ideal band gap (1.49 eV) for highest theoretical conversion efficiency. Thus by tailoring the value of Cu/(Zn+Sn), CZTSSe thin films with the desired band gap could be obtained. Acknowledgment: We are thankful to DIBS, EDX, and XRD facility equipped at Sophisticated Instrument Centre (SIC) at IIT Indore. The authors B. S. S and A. K. acknowledge CSIR, and V. G. acknowledges UGC, India for their fellowships. B. S. S is thankful to DST and IUSSTF for BASE Internship Award. Prof. Shaibal Mukherjee is thankful to DST and IUSSTF for BASE Fellowship and MEITY YFRF award. This work is partially supported by DAE BRNS, DST CERI, and DST-RFBR Project under India-Russia Programme of Cooperation in Science and Technology. We are thankful to Mukul Gupta for SIMS facility equipped at UGC-DAE Indore.

Keywords: CZTSSe, DIBS, EDX, solar cell

Procedia PDF Downloads 250

Authors: Selma Hamimed, Abdelwaheb Chatti

Abstract:

The current study deals with the biological treatment of saline wastewaters generated by various agro-food industries using Yarrowia lipolytica. The ability of this yeast was studied on the mixture of olive mill wastewater and tuna wash processing wastewater. Results showed that the high proportion of olive mill wastewater in the mixture about (75:25) is the suitable one for the highest Y. lipolytica biomass production, reaching 11.3 g L⁻¹ after seven days. In addition, results showed significant removal of chemical oxygen demand (COD) and phosphorous of 97.49 % and 98.90 %, respectively. On the other hand, Y. lipolytica was found to be effective to desalinate all mixtures reaching a removal of 92.21 %. Moreover, the analytical results using Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and scanning electron microscopy (SEM) confirmed the biosorption of NaCl on the surface of the yeast as nanocrystals form with a size of 47.3 nm.

Keywords: nanocrystallization of NaCl, desalination, wastewater treatment, yarrowia lipolytica

Procedia PDF Downloads 187

Authors: M. N. Akhtar, J. N. Akhtar

Abstract:

The present study evaluates the properties of class F fly ash as a replacement of natural materials in civil engineering construction industry. The low-lime flash similar to class F is the prime variety generated in India, although it has significantly smaller volumes of high-lime fly ash as compared to class C. The chemical and physical characterization of the sample is carried out with the number of experimental approaches in order to investigate all relevant features present in the samples. For chemical analysis, elementary quantitative results from point analysis and scanning electron microscopy (SEM)/dispersive spectroscopy (EDS) techniques were used to identify the element images of different fractions. The physical properties found very close to the range of common soils. Furthermore, the fly ash-based bricks were prepared by the same sample of class F fly ash and the results of compressive strength similar to that of Standard Clay Brick Grade 1 available in the local market of India.

Keywords: fly ash, class F, class C, chemical, physical, SEM, EDS

Procedia PDF Downloads 181

Authors: L. Rozumová, J. Seidlerová

Abstract:

The aim of this paper was to study the sorption properties of a blast furnace sludge used as the sorbent. The sorbent was utilized for reduction of content of lead and zinc ions. Sorbent utilized in this work was obtained from metallurgical industry from process of wet gas treatment in iron production. The blast furnace sludge was characterized by X-Ray diffraction, scanning electron microscopy, and XRFS spectroscopy. Sorption experiments were conducted in batch mode. The sorption of metal ions in the sludge was determined by correlation of adsorption isotherm models. The adsorption of lead and zinc ions was best fitted with Langmuir adsorption isotherms. The adsorption capacity of lead and zinc ions was 53.8 mg.g^-1 and 10.7 mg.g^-1, respectively. The results indicated that blast furnace sludge could be effectively used as secondary material and could be also employed as a low-cost alternative for the removal of heavy metals ions from wastewater.

Keywords: blast furnace sludge, lead, zinc, sorption

Procedia PDF Downloads 302

Authors: Siva Prasad Peddi

Abstract:

Silver nanoparticles were successfully synthesized from silver nitrate through a rapid green synthesis method using Eclipta prostrata leaf extract as a reducing cum stabilizing agent. The experimental procedure was readily conducted at room temperature and pressure, and could be easily scaled up. The silver nanoparticles thus obtained were characterized using UV-Visible Spectroscopy (UV-VIS) which yielded an absorption peak at 416 nm. The biomolecules responsible for capping of the bio-reduced silver nanoparticles synthesized using plant extract were successfully identified through FTIR analysis. It was evinced through Scanning Electron Microscope (SEM), and X-ray diffraction (XRD) analysis that the silver nanoparticles were crystalline in nature and spherical in shape. The average size of the particles obtained using Scherrer’s formula was 27.4 nm. The adopted technique for silver nanoparticle synthesis is suitable for large-scale production.

Keywords: silver nanoparticles, green synthesis, characterization, Eclipta prostrata

Procedia PDF Downloads 468

Authors: Gurpreet Singh, Hazoor Singh, Buta Singh Sidhu

Abstract:

In the current investigation plasma spray technique was used for depositing hydroxyapatite (HA) and HA – silicon oxide (SiO2) coatings on 316L SS substrate. In HA-SiO2 coating, 20 wt% SiO2 was mixed with HA. The feedstock and coatings were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM)/energy-dispersive X-ray spectroscopy (EDX) analyses. The corrosion resistance of the uncoated, HA coated and HA + 20 wt% SiO2 coated 316L SS was investigated by electrochemical corrosion testing in simulated human body fluid (Ringer’s solution). The influence of SiO2 (20 wt%) on corrosion resistance was determined. After the corrosion testing, the samples were analyzed by XRD and SEM/EDX analyses. The addition of SiO2 reduces the crystallinity of the coating. The corrosion resistance of the 316L SS was found to increase after the deposition of the HA + 20 wt% SiO2 and HA coatings.

Keywords: HA, SiO2, corrosion, Ringer’s solution, 316L SS

Procedia PDF Downloads 419

Authors: M. Shopska, D. Paneva, G. Kadinov, Z. Cherkezova-Zheleva, I. Mitov

Abstract:

The iron containing materials are used as catalysts in different processes. The chemical methods of their synthesis use toxic and expensive chemicals; sophisticated devices; energy consumption processes that raise their cost. Besides, dangerous waste products are formed. At present time such syntheses are out of date and wasteless technologies are indispensable. The bioinspired technologies are consistent with the ecological requirements. Different microorganisms participate in the biomineralization of the iron and some phytochemicals are involved, too. The methods for biogenic production of iron containing materials are clean, simple, nontoxic, realized at ambient temperature and pressure, cheaper. The biogenic iron materials embrace different iron compounds. Due to their origin these substances are nanosized, amorphous or poorly crystalline, porous and have number of useful properties like SPM, high magnetism, low toxicity, biocompatibility, absorption of microwaves, high surface area/volume ratio, active sites on the surface with unusual coordination that distinguish them from the bulk materials. The biogenic iron materials are applied in the heterogeneous catalysis in different roles - precursor, active component, support, immobilizer. The application of biogenic iron oxide materials gives rise to increased catalytic activity in comparison with those of abiotic origin. In our study we investigated the catalytic behavior of biomasses obtained by cultivation of Leptothrix bacteria in three nutrition media – Adler, Fedorov, and Lieske. The biomass composition was studied by Moessbauer spectroscopy and transmission IRS. Catalytic experiments on CO oxidation were carried out using in situ DRIFTS. Our results showed that: i) the used biomasses contain α-FeOOH, γ-FeOOH, γ-Fe2O3 in different ratios; ii) the biomass formed in Adler medium contains γ-FeOOH as main phase. The CO conversion was about 50% as evaluated by decreased integrated band intensity in the gas mixture spectra during the reaction. The main phase in the spent sample is γ-Fe2O3; iii) the biomass formed in Lieske medium contains α-FeOOH. The CO conversion was about 20%. The main phase in the spent sample is α-Fe2O3; iv) the biomass formed in Fedorov medium contains γ-Fe2O3 as main phase. CO conversion in the test reaction was about 19%. The results showed that the catalytic activity up to 200°C resulted predominantly from α-FeOOH and γ-FeOOH. The catalytic activity at temperatures higher than 200°C was due to the formation of γ-Fe2O3. The oxyhydroxides, which are the principal compounds in the biomass, have low catalytic activity in the used reaction; the maghemite has relatively good catalytic activity; the hematite has activity commensurate with that of the oxyhydroxides. Moreover it can be affirmed that catalytic activity is inherent in maghemite, which is obtained by transformation of the biogenic lepidocrocite, i.e. it has biogenic precursor.

Keywords: nanosized biogenic iron compounds, catalytic behavior in reaction of CO oxidation, in situ DRIFTS, Moessbauer spectroscopy

Procedia PDF Downloads 369

Authors: Mala Nath, Nagamani Kompelli, Partha Roy, Snehasish Das

Abstract:

Two new metal-based anticancer chemotherapeutic agents, [(Ph2Sn)2(HGuO)2(phen)Cl2] 1 and [(Ph3Sn)(HGuO)(phen)]- Cl.CH3OH.H2O 2, were designed, prepared and characterized by analytical and spectral (IR, ESI-Mass, 1H, 13C and 119Sn NMR) techniques. The proposed geometry of Sn(IV) in 1 and 2 is distorted octahedral and distorted trigonal-bipyramidal, respectively. Both 1 and 2 exhibit potential cytotoxicity in vitro against MCF-7, HepG-2 and DU-145 cell lines. The intrinsic binding constant (Kb) values of 1 (2.33 × 105 M-1) and 2 (2.46 × 105 M-1) evaluated from UV-Visible absorption studies suggest non-classical electrostatic mode of interaction via phosphate backbone of DNA double helix. The Stern-Volmer quenching constant (Ksv) of 1 (9.74 × 105 M-1) and 2 (2.9 × 106 M-1) determined by fluorescence studies suggests the groove binding and intercalation mode for 1 and 2, respectively. Effective cleavage of pBR322 DNA is induced by 1. Their interaction with DNA of cancer cells may account for potency.

Keywords: anticancer agents, DNA binding studies, NMR spectroscopy, organotin

Procedia PDF Downloads 257

Authors: R. Rosazley, M. A. Izzati, A. W. Fareezal, M. Z. Shazana, I. Rushdan, M. A. Ainun Zuriyati

Abstract:

This study focuses on production and characterizations of nanofibrillated cellulose (NFC) from kenaf core. NFC was produced by employing ultrasonic treatments in aqueous solution. Field emission scanning electron microscope (FESEM) and scanning transmission electron microscopy (STEM) were used to study the size and morphology structure. The chemical and characteristics of the cellulose and NFC were studied using Fourier-transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), X-ray diffraction (XRD) and viscometer. Degrees of polymerization (DP) of cellulose and NFC were obtained via viscosity value. Results showed that 5 to 47 nm diameters of fibrils were measured. Moreover, the thermal stability of the NFC was increased as compared to the cellulose that confirmed by TGA analysis. It was also found that NFC had higher crystallinity and lower viscosity than the cellulose which were measured by XRD and viscometer, respectively. The NFC characteristics have enormous prospect related to bio-nanocomposite.

Keywords: crystallinity, kenaf core, nanofibrillated cellulose, ultrasonic

Procedia PDF Downloads 326

Authors: P. Kaewchanthuek, R. Rawonghad, B. Marungsri

Abstract:

This paper presents the experimental results of high-density polyethylene cable spacers for 22 kV distribution systems under salt water dip wheel test based on IEC 62217. The strength of anti-tracking and anti-erosion of cable spacer surface was studied in this study. During the test, dry band arc and corona discharge were observed on cable spacer surface. After 30,000 cycles of salt water dip wheel test, obviously surface erosion and tracking were observed especially on the ground end. Chemical analysis results by fourier transforms infrared spectroscopy showed chemical changed from oxidation and carbonization reaction on tested cable spacer. Increasing of C=O and C=C bonds confirmed occurrence of these reactions.

Keywords: cable spacer, HDPE, ageing of cable spacer, salt water dip wheel test

Procedia PDF Downloads 379

Authors: Nam Chol Yu, GyongIl Chu, HoJong Ri

Abstract:

Using DLTS (Deep-level transient spectroscopy) measurement techniques, we determined the dominant recombination center levels (defects of both A and B) in gold and platinum doped n-type silicon. Also, the injection and temperature dependence of the Shockley-Read-Hall (SRH) carrier lifetime was studied under low-level injection and high-level injection. Here measurements show that the dominant level under low-level injection located at EC-0.25 eV (A) correlated to the Pt+G1 and the dominant level under high-level injection located at EC-0.54 eV (B) correlated to the Au+G4. Finally, A and B are the same dominant levels for controlling the lifetime in gold-platinum doped n-silicon.

Keywords: recombination center level, lifetime, carrier lifetime control, Gold, Platinum, Silicon

Procedia PDF Downloads 69

Authors: Bourfaa Fouzia, Meryem Lamri Zeggar, Adjimi Amel, Mohammed Salah Aida, Nadir Attaf

Abstract:

Semiconductor photocatalysts such as ZnO has attracted much attention in recent years due to their various applications for the degradation of organic pollutants in water, air and in dye sensitized photovoltaic solar cell. In the present work, ZnO thin films were prepared by ultrasonic spray pyrolysis by using different precursors namely: Acetate, chloride and zinc nitrate in order to investigate their influence on ZnO photocatalytic activity. The films crystalline structure was studied by mean of X-ray diffraction measurements (XRD) and the films surface morphology by Scanning Electron Microscopy (SEM). The films optical properties were studied by mean of UV–visible spectroscopy. The prepared films were tested for the degradation of the red reactive dye largely used in textile industry. As a result, we found that the zinc nitrate is the best precursor to prepare ZnO thin films suitable for a good photocatalytic activity.

Keywords: precursor, thins films, spray pyrolysis, zinc oxide

Procedia PDF Downloads 327

Authors: K. Brince Paul, Nagendra Pratap Singh, Shiv Govind Singh, Siva Rama Krishna Vanjari

Abstract:

In this paper, we report optimized procedure for synthesizing highly oriented, horizontally aligned, Zinc oxide (ZnO) nanowires targeted towards developing highly sensitive piezoelectric transduction elements. The synthesis was carried out using Electrospinning technique, a facile, robust, low cost technique for producing nanowires. The as-synthesized ZnO nanowires were characterized by X-ray powder diffraction (XRD), Field Emission scanning electron microscopy (FESEM) and Energy-dispersive X-ray spectroscopy (EDX).The Piezoelectric behavior of these nanowires was characterized using Peizoelectric Force microscopy (PFM). A very high d33 coefficient of 23.1 pm/V obtained through the PFM measurements is an indicative of its potential application towards developing miniaturized piezoelectric transduction elements for nanoscale devices.

Keywords: electrospinning, piezoelectric, technique, zinc oxide

Procedia PDF Downloads 405

Authors: Ahmed A. Elshami, Stephanie Bonnet, Abdelhafid Khelidj

Abstract:

Corrosion inhibitors are widely used in concrete industry to reduce the corrosion rate of steel rebar which is present in contact with aggressive environments. The present work aims to using Zamzam water from well located within the Masjid al-Haram in Mecca, Saudi Arabia 20 m (66 ft) east of the Kaaba, the holiest place in Islam as corrosion inhibitor for steel in rain water and simulated acid rain. The effect of Zamzam water was investigated by electrochemical impedance spectroscopy (EIS) and Potentiodynamic polarization techniques in Department of Civil Engineering - IUT Saint-Nazaire, Nantes University, France. Zamzam water is considered to be one of the most important steel corrosion inhibitor which is frequently used in different industrial applications. Results showed that zamzam water gave a very good inhibition for steel corrosion in rain water and simulated acid rain.

Keywords: Zamzam water, corrosion inhibitor, rain water, simulated acid rain

Procedia PDF Downloads 394

Authors: Saeeda Nadir Ali, Najma Sultana, Muhammad Saeed Arayne

Abstract:

Charge transfer complexes of omeprazole with bromothymol blue, methyl orange, and picric acid in the Beer’s law ranges 7-56, 6-48, and 10-80 µg mL-1, exhibiting stoichiometric ratio 1:1, and maximum wavelength 400, 420 and 373 nm respectively have been studied in aqueous medium. ICH guidelines were followed for validation study. Spectroscopic parameters including oscillator’s strength, dipole moment, ionization potential, energy of complexes, resonance energy, association constant and Gibb’s free energy changes have also been investigated and Benesi-Hildebrand plot in each case has been obtained. In addition, the methods were fruitfully employed for omeprazole determination in pharmaceutical formulations with no excipients obstruction during analysis. Solid omeprazole complexes with all the acceptors were synthesized and then structure was elucidated by IR and 1H NMR spectroscopy.

Keywords: omeprazole, bromothymol blue, methyl orange and picric acid, charge transfer complexes

Procedia PDF Downloads 540

Authors: O. P. Yadav

Abstract:

Nano-size Ag-N co-doped ZnO/CuO composite photo-catalyst has been synthesized by chemical method and characterized using XRD, TEM, FTIR, AAS and UV-Vis spectroscopic techniques. Photo-catalytic activity of as-synthesized nanomaterial has been studied using degradation of methyl orange as a probe under UV as well as visible radiations. Ag-N co-doped ZnO/CuO composite showed higher photo-catalytic activity than Ag- or N-doped ZnO and undoped ZnO-CuO composite photo-catalysts. The observed highest activity of Ag-N co-doped ZnO-CuO among the studied photo-catalysts is attributed to the cumulative effects of lowering of band-gap energy and decrease of recombination rate of photo-generated electrons and holes owing to doped N and Ag, respectively. Effects of photo-catalyst load, pH and substrate initial concentration on degradation of methyl orange have also been studied. Photo-catalytic degradation of methyl orange follows pseudo first order kinetics.

Keywords: degradation, nanocomposite, photocatalyst, spectroscopy, XRD

Procedia PDF Downloads 497

Authors: Igor Bilenko, Artem Shitikov, Michael Gorodetsky

Abstract:

Optical whispering gallery mode (WGM) resonators combine very high optical quality factor (Q) with small size. Resonators made from low loss crystalline fluorites (CaF2, MgF2) may have Q as high as 1010 that make them unique devices for modern applications including ultrasensitive sensors, frequency control, and precision spectroscopy. While silicon is a promising material transparent from near infrared to terahertz frequencies, fundamental limit for Si WGM quality factor was not reached yet. In our paper, we presented experimental results on the preparation and testing of resonators at 1550 nm wavelength made from crystalline silicon grown and treated by different techniques. Q as high as 3x107 was demonstrated. Future steps need to reach a higher value and possible applications are discussed.

Keywords: optical quality factor, silicon optical losses, silicon optical resonator, whispering gallery modes

Procedia PDF Downloads 493