Search results for: IR spectroscopy

Authors: M. Jerold, V. Sivasubramanian

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This study reports the removal of Malachite Green (MG) from simulated wastewater by using marine macro algae Ulva lactuca. Batch biosorption experiments were carried out to determine the biosorption capacity. The biosorption capacity was found to be maximum at pH 10. The effect of various other operation parameters such as biosorbent dosage, initial dye concentration, contact time and agitation was also investigated. The equilibrium attained at 120 min with 0.1 g/L of biosorbent. The isotherm experimental data fitted well with Langmuir Model with R² value of 0.994. The maximum Langmuir biosorption capacity was found to be 76.92 mg/g. Further, Langmuir separation factor RL value was found to be 0.004. Therefore, the adsorption is favorable. The biosorption kinetics of MG was found to follow pseudo second-order kinetic model. The mechanistic study revealed that the biosorption of malachite onto Ulva lactuca was controlled by film diffusion. The solute transfer in a solid-liquid adsorption process is characterized by the film diffusion and/or particle diffusion. Thermodynamic study shows ΔG° is negative indicates the feasibility and spontaneous nature for the biosorption of malachite green. The biosorbent was characterized using Scanning Electron Microscopy, Fourier Transform Infrared Spectroscopy, and elemental analysis (CHNS: Carbon, Hydrogen, Nitrogen, Sulphur). This study showed that Ulva lactuca can be used as promising biosorbent for the removal of MG from wastewater.

Keywords: biosorption, Ulva lactuca, wastewater, malachite green, isotherm, kinetics

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Authors: Maha Al-Ali, Selvakannan Periasamy, Rajarathinam Parthasarathy

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Drying temperature is an important factor impacting the physicochemical properties of the dried materials, particularly the pharmaceutical powders. Drying of pharmaceuticals by using microwave radiation is very limited, and the available information about the interaction between the electromagnetic radiations and the pharmaceutical material is still scarce. Therefore, microwave drying process is employed in this work to dry the wet (moisturised) granules of the formulated naproxen-sodium drug. This study aims to investigate the influences of the microwave radiation temperatures on the moisture removal, the crystalline structure, the size and morphology of the dried naproxen-sodium particles, and identify any potential changes in the chemical groups of the drug. In this work, newly formulated naproxen-sodium is prepared and moisturized by wet granulation process and hence dried by using microwave radiation at different temperatures. Moisture analyzer, Fourier-transform infrared spectroscopy, powder X-ray diffraction, and scanning electron microscope are used to characterise the non-moisturised powder (reference powder), the moisturised granules, and the dried particles. The results show that microwave drying of naproxen-sodium at high drying temperature is more efficient than that at low temperatures in terms of the moisture removal. Although there is no significant change in the chemical structure of the dried particles, the particle size, crystallinity and morphology are relatively changed with changing of heating temperature.

Keywords: heating temperature, microwave drying, naproxen-sodium, particle size

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Authors: Mangaka C. Matoetoe, Fredrick O. Okumu

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Metal nanoparticles have attracted a great interest in scientific research and industrial applications, owing to their unique large surface area-to-volume ratios and quantum-size effects. Supported metal nanoparticles play a pivotal role in areas such as nanoelectronics, energy storage and as catalysts for the sustainable production of fuels and chemicals. Monometallics (Ag, Pt) and Silver-platinum (Ag-Pt) bimetallic (BM) nanoparticles (NPs) with a mole fraction (1:1) were prepared by reduction / co-reduction of hexachloroplatinate and silver nitrate with sodium citrate. The kinetics of the nanoparticles formation was monitored using UV-visible spectrophotometry. Transmission electron microscopy (TEM) and Energy-dispersive X-ray (EDX) spectroscopy were used for size, film morphology as well as elemental composition study. Fast reduction processes was noted in Ag NPs (0.079 s-1) and Ag-Pt NPs 1:1 (0.082 s-1) with exception of Pt NPs (0.006 s-1) formation. The UV-visible spectra showed characteristic peaks in Ag NPs while the Pt NPs and Ag-Pt NPs 1:1 had no observable absorption peaks. UV visible spectra confirmed chemical reduction resulting to formation of NPs while TEM images depicted core-shell arrangement in the Ag-Pt NPs 1:1 with particle size of 20 nm. Monometallic Ag and Pt NPs reported particle sizes of 60 nm and 2.5 nm respectively. The particle size distribution in the BM NPs was found to directly depend on the concentration of Pt NPs around the Ag core. EDX elemental composition analysis of the nanoparticle suspensions confirmed presence of the Ag and Pt in the Ag-Pt NPs 1:1. All the spectroscopic analysis confirmed the successful formation of the nanoparticles.

Keywords: kinetics, morphology, nanoparticles, platinum, silver

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Authors: Kefyalew Muleta, Tetemke Mehari

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Background: Human being require metallic elements such as copper and zinc up to certain limits that could cause problems if found in excess. Other metallic elements like cadmium and lead can be harmful to health if foodstuffs containing them are consumed regularly. Canned dry-milk and fish contain these metals in the journey from farm to fork. Objective: This study was designed to determine the concentration of Cd, Cu, Pb, and Zn in four brands of canned dry-milk and fish from supermarkets in Addis Ababa. Methods: Laboratory based cross-sectional study design was used to determine the concentration of the heavy metals in four different brands of canned dry-milk and fish imported from different country from February to March 2013. The foods brands were sampled by simple random sampling method from eight supermarkets in Addis Ababa and coded. Wet oxidation using HNO3 and H2O2 was used to extract the heavy metals from the foods samples and analyzed by Flame Atomic Absorption Spectroscopy. Conclusions: From this study, it can be concluded that the level of Cadmium and Copper residues in canned dry-milk significantly vary among brands; and the levels of copper residue significantly vary among brands of canned fish at 95 % level. The AM milk brand from Ethiopia was safe in cadmium level. The cadmium and lead level in the NF fish brands from Indonesia packed in vegetables oil, and the lead level in DF brand packed in brine are safe.

Keywords: AAS, canned dry milk, canned fish, Cd, Cu, Pb, Zn

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Authors: Quan Li, Dongcai Shen, Zhengting Xiao, Xin Liu Mingrui Wu, Licheng Liu, Qin Li, Xianguo Li, Wentai Wang

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Direct electrocatalytic nitrogen oxidation (NOR) provides a promising alternative strategy for synthesizing high-value-added nitric acid from widespread N₂, which overcomes the disadvantages of the Haber-Bosch-Ostwald process. However, the NOR process suffers from the limitation of high N≡N bonding energy (941 kJ mol− ¹), sluggish kinetics, low efficiency and yield. It is a prerequisite to develop more efficient electrocatalysts for NOR. Herein, we synthesized double-shelled CeO₂ hollow spheres (D-CeO₂) and further modified with Ti₃C₂ MXene quantum dots (MQDs) for electrocatalytic N₂ oxidation, which exhibited a NO₃− yield of 71.25 μg h− ¹ mgcat− ¹ and FE of 31.80% at 1.7 V. The unique quantum size effect and abundant edge active sites lead to a more effective capture of nitrogen. Moreover, the double-shelled hollow structure is favorable for N₂ fixation and gathers intermediate products in the interlayer of the core-shell. The in-situ infrared Fourier transform spectroscopy confirmed the formation of *NO and NO₃− species during the NOR reaction, and the kinetics and possible pathways of NOR were calculated by density functional theory (DFT). In addition, a Zn-N₂ reaction device was assembled with D-CeO₂/MQDs as anode and Zn plate as cathode, obtaining an extremely high NO₃− yield of 104.57 μg h− ¹ mgcat− ¹ at 1 mA cm− ².

Keywords: electrocatalytic N₂ oxidation, nitrate production, CeO₂, MXene quantum dots, double-shelled hollow spheres

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Authors: E. A. Alshaafi, A. Prakash

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Oil-water emulsions are commonly encountered in various industrial operations and at different stages of crude oil production and processing. Emulsions are often difficult to track and treat and can cause a number of costly problems which need to be avoided. The characteristics of the emulsion phase can vary with crude composition and types of impurities present in oil. The objectives of this study are the development of ultrasonic techniques to track and characterize emulsion phase generated during production and cleaning of crude oil. The position of emulsion layer is monitored with the help of ultrasonic probes suitably placed in the vessel. The sensitivity of the technique and its potential has been demonstrated based on extensive testing with different oil samples. The technique is also being developed to monitor emulsion phase characteristics such as stability, composition, and droplet size distribution. The ultrasonic parameters recorded are changes in acoustic velocity, signal attenuation and its frequency spectrum. Emulsion has been prepared with light mineral oil sample and the effects of various factors including mixing speed, temperature, surfactant, and solid particles concentrations have been investigated. The applied frequency for ultrasonic waves has been varied from 1 to 5 MHz to carry out a sensitivity analysis. Emulsion droplet structure is observed with optical microscopy and stability is examined by tracking the changes in ultrasonic parameters with time. A model based on ultrasonic attenuation spectroscopy is being developed and tested to track changes in droplet size distribution with time.

Keywords: ultrasonic techniques, emulsion, characterization, droplet size

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Authors: Shu-Chuan Liao, Chia-Ti Chang, Ko-Shao Chen

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Titanium and its alloy are widely used in many fields such as dentistry or orthopaedics. Due to their high strength low elastic modulus that chemical inertness and bio inert. The micro-arc oxidation used to formation a micro porous ceramic oxide layer film on Titanium surface and also to improve the resistance corrosion. For improving the biocompatibility, micro-arc oxidation surfaces bio-inert need to introduce reactive group. We introduced boundary layer by used plasma enhanced chemical vapor deposition of hexamethyldisilazane (HMDS) and organic active layer by UV light graft reactive monomer acrylic acid (AAc) therefore we can immobilize Chondroitin sulphate on surface easily by crosslinking EDC/NHS. The surface properties and composition of the modified layer were measured by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) and water contact angle. Water contact angle of the plasma-treated Ti surface decreases from 60° to 38°, which is an indication of hydrophilicity. The results of electrochemical polarization analysis showed that the sample plasma treated at micro-arc oxidation after plasma treatment has the best corrosion resistance. The result showed that we can immobilize chondroitin sulfate successful by a series of modification and MTT assay indicated the biocompatibility has been improved in this study.

Keywords: MAO, plasma, graft polymerization, biomedical application

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Authors: Sanaz Seraj, Shohre Rouhani

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Recently, graphene has gained much attention because of its unique optical, mechanical, electrical, and thermal properties. Graphene has been used as a key material in the technological applications in various areas such as sensors, drug delivery, super capacitors, transparent conductor, and solar cell. It has a superior quenching efficiency for various fluorophores. Based on these unique properties, the optical sensors with graphene materials as the energy acceptors have demonstrated great success in recent years. During quenching, the emission of a fluorophore is perturbed by a quencher which can be a substrate or biomolecule, and due to this phenomenon, fluorophore-quencher has been used for selective detection of target molecules. Among fluorescence dyes, 1,8-naphthalimide is well known for its typical intramolecular charge transfer (ICT) and photo-induced charge transfer (PET) fluorophore, strong absorption and emission in the visible region, high photo stability, and large Stokes shift. Derivatives of 1,8-naphthalimides have found applications in some areas, especially fluorescence sensors. Herein, the fluorescence quenching of graphene oxide has been carried out on a naphthalimide dye as a fluorescent probe model. The quenching ability of graphene oxide on naphthalimide dye was studied by UV-VIS and fluorescence spectroscopy. This study showed that graphene is an efficient quencher for fluorescent dyes. Therefore, it can be used as a suitable candidate sensing platform. To the best of our knowledge, studies on the quenching and absorption of naphthalimide dyes by graphene oxide are rare.

Keywords: fluorescence, graphene oxide, naphthalimide dye, quenching

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Authors: Bal Chandra Yadav, Rakesh K. Sonker, Anjali Sharma, Punit Tyagi, Vinay Gupta, Monika Tomar

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In the present study, ZnO doped SnO2 thin films of various compositions were deposited on the surface of a corning substrate by dropping the two sols containing the precursors for composite (ZSO) with subsequent heat treatment. The sensor materials used for selective detection of nitrogen dioxide (NO2) were designed from the correlation between the sensor composition and gas response. The available NO2 sensors are operative at very high temperature (150-800 °C) with low sensing response (2-100) even in higher concentrations. Efforts are continuing towards the development of NO2 gas sensor aiming with an enhanced response along with a reduction in operating temperature by incorporating some catalysts or dopants. Thus in this work, a novel sensor structure based on ZSO nanocomposite has been fabricated using chemical route for the detection of NO2 gas. The structural, surface morphological and optical properties of prepared films have been studied by using X-ray diffraction (XRD), Atomic force microscopy (AFM), Transmission electron microscope (TEM) and UV-visible spectroscopy respectively. The effect of thickness variation from 230 nm to 644 nm of ZSO composite thin film has been studied and the ZSO thin film of thickness ~ 460 nm was found to exhibit the maximum gas sensing response ~ 2.1×103 towards 20 ppm NO2 gas at an operating temperature of 90 °C. The average response and recovery times of the sensor were observed to be 3.51 and 6.91 min respectively. Selectivity of the sensor was checked with the cross-exposure of vapour CO, acetone, IPA, CH4, NH3 and CO2 gases. It was found that besides the higher sensing response towards NO2 gas, the prepared ZSO thin film was also highly selective towards NO2 gas.

Keywords: ZSO nanocomposite thin film, ZnO tetrapod structure, NO2 gas sensor, sol-gel method

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Authors: Ayman M. Ibrahim, Jinpeng Cai, Peilun Shen, Dianwen Liu

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The difference in promoting sulfurization between different ammonium salts and its anion's effect on the sulfurization of the malachite surface was systematically studied. Therefore, this study takes malachite, a typical copper oxide mineral, as the research object, field emission scanning electron microscopy and energy-dispersive X-ray analysis (FESEM‒EDS), X-ray photoelectron spectroscopy (XPS), and other analytical and testing methods, as well as pure mineral flotation experiments, were carried out to examine the superiority of the ammonium salts as the sulfurizing reagent of malachite at the microscopic level. Additionally, the promoting effects of ammonium sulfate and ammonium phosphate on the malachite sulfurization of xanthate-flotation were compared systematically from the microstructure of sulfurized products, elemental composition, chemical state of characteristic elements, and hydrophobicity surface evolution. The FESEM and AFM results presented that after being pre-treated with ammonium salts, the adhesion of sulfurized products formed on the mineral surface was denser; thus, the flake radial dimension product was significantly greater. For malachite sulfurization flotation, the impact of ammonium phosphate in promoting sulfurization is weaker than ammonium sulfate. The reason may be that hydrolyzing phosphate consumes a substantial quantity of H+ in the solution, which hastens the formation of the copper-sulfur products, decreasing the adhesion stability of copper-sulfur species on the malachite surface.

Keywords: sulfurization flotation, adsorption characteristics, malachite, hydrophobicity

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Authors: Jie Chen, Chris Cheng, Kai Zhang

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Polycrystalline diamond compact (PDC) cutters with a polycrystalline diamond (PCD) table supported by a cemented tungsten carbide substrate have been widely used for earth-drilling tools in the oil and gas industry. Both wear and impact resistances are key figure of merits of PDC cutters, and they are closely related to the microstructure of the PCD table. As oil and gas exploration enters deeper, harder, and more complex formations, plus increasing requirement of accelerated downhole drilling speed and drilling cost reduction, current PDC cutters face unprecedented challenges for maintaining a longer drilling life than ever. Excessive wear on uneven hard formations, spalling, chipping, and premature fracture due to impact loads are common failure modes of PDC cutters in the field. Tailoring microstructure of the PCD table is one of the effective approaches to improve the wear and impact resistances of PDC cutters, along with other factors such as cutter geometry and bit design. In this research, cross-sectional microstructure, fracture surface, wear surface, and elemental composition of PDC cutters were analyzed using scanning electron microscopy (SEM) with both backscattered electron and secondary electron detectors, and energy dispersive X-ray spectroscopy (EDS). The microstructure and elemental composition were further correlated with the wear and impact resistances of corresponding PDC cutters. Wear modes and impact toughening mechanisms of state-of-the-art PDCs were identified. Directions to further improve the wear and impact resistances of PDC cutters were proposed.

Keywords: fracture surface, microstructure, polycrystalline diamond, PDC, wear surface

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Authors: Uchechukwu Vincent Okpala

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Under the Sun, energy is a key factor for the sustenance of life and its environment. The need to protect the environment as energy is generated and consumed has called for renewable and green energy sources. To be part of this green revolution, we synthesized and characterized undoped and velvet tamarind doped zinc sulfide (ZnS) crystals using sol-gel methods. Velvet tamarind was whittled down using the top-down approach of nanotechnology. Sodium silicate, tartaric acid, zinc nitrate, and thiourea were used as precursors. The grown samples were annealed at 105°C. Structural, optical, and compositional analyses of the grown samples revealed crystalline structures with varied crystallite sizes influenced by doping. Energy-dispersive X-ray spectroscopy confirmed elemental compositions of Zn, S, C and O in the films. Atomic percentages of the elements varied with VT doping. FT-IR analysis indicated the presence of functional groups like O-H stretching (alcohol), C=C=C stretching (alkene group), C=C bending, C-H stretching (alkane), N-H stretching (aliphatic primary amine) and N=C=S stretching (isothiocyanate) constituent in the film. The transmittance of the samples increased from the visible region to the infrared region making the samples good for poultry and solar energy applications. The bandgap energy of the films decreased as the number of VT drops increased, from 2.4 to 2.2. They were wide band gap materials and were good for optoelectronic, photo-thermal, high temperature, high power and solar cell applications.

Keywords: doping, sol-gel, velvet tamarind, ZnS.

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Authors: Iftikhar Hussain Gul, Syeda Aatika

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Nickel ferrite was prepared via wet chemical co-precipitation route. Carbon Nano Fibers (CNFs) were used to prepare NiFe₂O₄/CNFs nanohybrids. Polar solvent (ortho-xylene) was used for the dispersion of CNFs in ferrite matrix. X-ray diffraction patterns confirmed the formation of NiFe₂O₄/CNFs nanohybrids without any impurity peak. FTIR patterns showed two consistent characteristic absorption bands for tetrahedral and octahedral sites, confirming the formation of spinel structure of NiFe₂O₄. Scanning Electron Microscopy (SEM) images confirmed the coating of nickel ferrite nanoparticles on CNFs, which confirms the efficiency of deployed method. The dielectric properties were measured as a function of frequency at room temperature. Pure NiFe₂O₄ showed dielectric constant of 1.79 ×10³ at 100 Hz, which increased massively to 2.92 ×10⁶ at 100 Hz with the addition of 20% by weight of CNFs, proving it to be potential candidate for applications in supercapacitors. The impedance analysis showed a considerable decrease of resistance, reactance and cole-cole plot which confirms the decline of impedance on addition of CNFs. The pure NiFe₂O₄ has highest impedance values of 5.89 ×10⁷ Ohm at 100 Hz while the NiFe₂O₄/CNFs nanohybrid with CNFs (20% by weight) has the lowest impedance values of 4.25×10³ Ohm at 100 Hz, which proves this nanohybrid is useful for high-frequency applications.

Keywords: AC impedance, co-precipitation, nanohybrid, Fourier transform infrared spectroscopy, x-ray diffraction

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Authors: Sheila Shahidi

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UV protection by fabrics has recently become a focus of great interest, particularly in connection with environmental degradation or ozone layer depletion. Fabrics provide simple and convenient protection against UV radiation (UVR), but not all fabrics offer sufficient UV protection. To describe the degree of UVR protection offered by clothing materials, the ultraviolet protection factor (UPF) is commonly used. UV-protective fabric can be generated by application of a chemical finish using normal wet-processing methodologies. However, traditional wet-processing techniques are known to consume large quantities of water and energy and may lead to adverse alterations of the bulk properties of the substrate. Recently, usage of plasmas to generate physicochemical surface modifications of textile substrates has become an intriguing approach to replace or enhance conventional wet-processing techniques. In this research work the effect of plasma treatment on UV protection properties of fabrics was investigated. DC magnetron sputtering was used and the parameters of plasma such as gas type, electrodes, time of exposure, power and, etc. were studied. The morphological and chemical properties of samples were analyzed using Scanning Electron Microscope (SEM) and Furrier Transform Infrared Spectroscopy (FTIR), respectively. The transmittance and UPF values of the original and plasma-treated samples were measured using a Shimadzu UV3101 PC (UV–Vis–NIR scanning spectrophotometer, 190–2, 100 nm range). It was concluded that, plasma which is an echo-friendly, cost effective and dry technique is being used in different branches of the industries, and will conquer textile industry in the near future. Also it is promising method for preparation of UV protection textile.

Keywords: fabric, plasma, textile, UV protection

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Authors: Rezzouq Asiya, Bouftou Abderrahim, Belfadil Doha, Taoufyk Azzeddine, El Bouchti Mehdi, Zyade Souad, Cherkaoui Omar, Majid Sanaa

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Plastic packaging is widely used, but its pollution is a major environmental problem. Solutions require new sustainable technologies, environmental management, and the use of bio-based polymers as sustainable packaging. Cellulose acetate (CA) is a biobased polymer used in a variety of applications such as the manufacture of plastic films, textiles, and filters. However, it has limitations in terms of thermal stability and rigidity, which necessitates the addition of plasticizers to optimize its use in packaging. Plasticizers are molecules that increase the flexibility of polymers, but their influence on the chemical and physical properties of films (CA) has not been studied in detail. Some studies have focused on mechanical and thermal properties. However, an in-depth analysis is needed to understand the interactions between the additives and the polymer matrix. In this study, the aim is to examine the effect of two types of plasticizers, glycerol (a conventional plasticizer) and an ionic liquid, on the transparency, mechanical, thermal and barrier properties of cellulose acetate (CA) films prepared by the solution-casting method . Various analytical techniques were used to characterize these films, including infrared spectroscopy (FT-IR), X-ray diffraction (XRD), thermogravimetric analysis (TGA), water vapor permeability (WVP), oxygen permeability, scanning electron microscopy (SEM), opacity, transmission analysis and mechanical tests.

Keywords: cellulose acetate, plasticizers, biopolymers, ionic liquid, glycerol.

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Authors: Ana P. R. N. Barroso, Maurício N. Kleinberg, Frederico R. Silva, Rodrigo F. Guimarães, Marcelo M. V. Parente, Walney S. Araújo

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The fight against accelerated wear of the equipment used in the oil and gas sector is a challenge for minimizing maintenance costs. Corrosion being one of the main agents of equipment deterioration, we seek alternative materials that exhibit improved corrosion resistance at low cost of production. This study aims to evaluate the corrosion behavior of experimental alloys containing 15% and 17% of chromium (Cr) and 5% of molybdenum (Mo) in comparison with an AISI 444 commercial alloy. Microstructural analyzes were performed on samples of the alloys before and after the electrochemical tests. Two samples of each solubilized alloy were also taken for analysis of the corrosion behavior by testing potentiodynamic polarization (PP) and Electrochemical Impedance Spectroscopy (EIS) with immersion time of 24 hours in electrolytic solution with acidic character. The graphics obtained through electrochemical tests of PP and EIS indicated that among the experimental alloys, the alloy with higher chromium content (17%) had a higher corrosion resistance, confirming the beneficial effect of adding chromium. When comparing the experimental alloys with the AISI 444 commercial alloy, it is observed that the AISI 444 commercial alloy showed superior corrosion resistance to that of the experimental alloys for both assays, PP and EIS. The microstructural analyzes performed after the PP and EIS tests confirmed the results previously described. These results suggest that the addition of these levels of molybdenum did not favor the electrochemical behavior of experimental ferritic alloys for the electrolytic medium studied.

Keywords: corrosion, molybdenum, electrochemical tests, experimental alloys

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Authors: Durata Haciu, Elif Sena Tekin, Gokce Ozturk, Patricia Ramey Balcı

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Coastal zones are under increasing threat due to anthropogenic activities that introduce considerable pollutants such as heavy metals into marine ecosystems. As part of a larger experimental study examining species responses to contaminated marine sediments, surface sediments (top 5cm) were analysed for major trace elements at three locations in Istanbul Straight. Samples were randomly collected by divers (May 2018) using hand-corers from Istinye (n=4), Garipce (n=10) and Poyrazköy (n=6), at water depths of 4-8m. Twelve metals were examined: As, arsenic; Pb, lead; Cd, cadmium; Cr, chromium; Cu, Copper; Fe, Iron; Ni, Nickel; Zn, Zinc; V, vanadium; Mn, Manganese; Ba, Barium; and Ag, silver by wavelength-dispersive X-ray fluorescence spectrometry (WDXRF) and Inductively Coupled Plasma/Mass Spectroscopy (ICP/MS). Preliminary results indicate that the average concentrations of metals (mg kg⁻¹) varied considerably among locations. In general, concentrations were relatively lower at Garipce compared to either Istinye or Poyrazköy. For most metals mean concentrations were highest at Poyrazköy and Ag and Cd were below detection limits (exception= Ag in a few samples). While Cd and As were undetected in all stations, the concentrations of Fe and Ni fall in the criteria of moderately polluted range and the rest of the metals in the range of low polluted range as compared to Effects Range Low (ERL) and Effects Range median (ERM) values determined by US Environmental Protection Agency (EPA).

Keywords: effect-range classification, ICP/MS, marine sediments, XRF

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Authors: Tesfay Gebremicheal Reda, K. Samatha, Paul Douglas Sanasi, D. Parajuli

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Nanoparticle technology is fast progressing and is being employed in innumerable medical applications. At this time, the public's health is seriously threatened by the rise of bacterial strains resistant to several medications. Metal nanoparticles are a potential alternate approach for tackling this global concern, and this is the main focus of this study. The citrate precursor sol-gel synthesis method was used to synthesize the Niₓ Co₁₋ₓ Fe₂ O₄, (where x = 0.0:0.2:1.0) nanoparticle. XRD identified the development of the cubic crystal structure to have a preferential orientation along (311), and the average particle size was found to be 29-38 nm. The average crystallizes assessed with ImageJ software and origin 22 of the SEM are nearly identical to the XRD results. In the created NCF NPs, the FT-IR spectroscopy reveals structural examinations and the redistribution of cations between octahedral (505-428 cm⁻¹) and tetrahedral (653-603 cm⁻¹) locales. As the Co²⁺ cation is substituted with Ni²⁺, the coercive fields HC decrease from 2384 Oe to 241.93 Oe. Band gap energy rises as Ni concentration increases, which may be attributed to the fact that the ionic radii of Ni²⁺ ions are smaller than that of Co²⁺ ions, which results in a strong electrostatic interaction. On the contrary, except at x = 0.4, the dielectric constant decreases as the nickel concentration increases. According to the findings of this research work, nanoparticles are composed of Ni₀.₄ Co₀.₆ Fe₂ O₄ have demonstrated a promising value against S. aureus and E. coli, and it suggests a proposed model for their potential use as a source of antibacterial agent.

Keywords: antimicrobial, band gap, citrate precursor, dielectric, nanoparticle

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Authors: Sajid Shah, Yoshimitsu Uemura, Katsuki Kusakabe

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Sol-gel derived hydrophobic silica membranes with pore sizes less than 1 nm are quite attractive for gas separation in a wide range of temperatures. A nano-structured hydrophobic membrane was prepared by sol-gel technique on a porous α–Al₂O₃ tubular support with yttria stabilized zirconia (YSZ) as an intermediate layer. Bistriethoxysilylethane (BTESE) derived sol was modified by adding phenyltriethoxysilylethane (PhTES) as an organic template. Six times dip coated modified silica membrane having a thickness of about 782 nm was characterized by field emission scanning electron microscopy. Thermogravimetric analysis, together along contact angle and Fourier transform infrared spectroscopy, showed that hydrophobic properties were improved by increasing the PhTES content. The contact angle of water droplet increased from 37° for pure to 111.5° for the modified membrane. The permeance of single gas H₂ was higher than H₂:CO₂ ratio of 75:25 binary feed mixtures. However, the permeance of H₂ for 60:40 H₂:CO₂ was found lower than single and binary mixture 75:25 H₂:CO₂. The binary selectivity values for 75:25 H₂:CO₂ were 24.75, 44, and 57, respectively. Selectivity had an inverse relation with PhTES content. Hydrophobicity properties were improved by increasing PhTES content in the silica matrix. The system exhibits proper three layers adhesion or integration, and smoothness. Membrane system suitable in steam environment and high-temperature separation. It was concluded that the hydrophobic silica membrane is highly promising for the separation of H₂/CO₂ mixture from various H₂-containing process streams.

Keywords: gas separation, hydrophobic properties, silica membrane, sol–gel method

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Authors: H. Djaaboube, I. Loucif, Y. Bouachiba, R. Aouati, A. Maameri, A. Taabouche, A. Bouabellou

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Thin films of pure and barium-doped zinc oxide (ZnO) were prepared using a spray pyrolysis process. The films were deposited on glass substrates at 450°C. The different samples are characterized by X-ray diffraction (XRD) and UV-Vis spectroscopy. X-ray diffraction patterns reveal the formation of a single ZnO Wurtzite structure and the good crystallinity of the films. The substitution of Ba ions influences the texture of the layers and makes the (002) plane a preferential growth plane. At concentrations below 6% Ba, the hexagonal structure of ZnO undergoes compressive stresses due to barium ions which have a radius twice of the Zn ions. This result leads to the decrees of a and c parameters and, therefore, the volume of the unit cell. This result is confirmed by the decrease in the number of crystallites and the increase in the size of the crystallites. At concentrations above 6%, barium substitutes the zinc atom and modifies the structural parameters of the thin layers. The bandgap of ZnO films decreased with increasing doping; this decrease is probably due to the 4d orbitals of the Ba atom due to the sp-d spin-exchange interactions between the band electrons and the localized d-electrons of the substituted Ba ion. Although, the Urbache energy undergoes an increase which implies the creation of energy levels below the conduction band and decreases the band gap width. The photocatalytic activity of ZnO doped 9% Ba was evaluated by the photodegradation of methylene blue under UV irradiation.

Keywords: barium, doping, photodegradation, spray pyrolysis, ZnO

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Authors: Waleed A. El-Said, Dina M. Fouad, Mohamed H. Aly, Mohamed A. El-Gahami

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Green synthesis of nanomaterials has received increasing attention as an eco-friendly technology in materials science. Here, we have used two types of extractions from green tea leaf (i.e. total extraction and tannin extraction) as reducing agents for a rapid, simple and one step synthesis method of mesoporous silica nanoparticles (MSNPs)/iron oxide (Fe3O4) nanocomposite based on deposition of Fe3O4 onto MSNPs. MSNPs/Fe3O4 nanocomposite were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, energy dispersive X-ray, vibrating sample magnetometer, N2 adsorption, and high-resolution transmission electron microscopy. The average mesoporous silica particle diameter was found to be around 30 nm with high surface area (818 m2/gm). MSNPs/Fe3O4 nanocomposite was used for removing lindane pesticide (an environmental hazard material) from aqueous solutions. Fourier transform infrared, UV-vis, High-performance liquid chromatography and gas chromatography techniques were used to confirm the high ability of MSNPs/Fe3O4 nanocomposite for sensing and capture of lindane molecules with high sorption capacity (more than 89%) that could develop a new eco-friendly strategy for detection and removing of pesticide and as a promising material for water treatment application.

Keywords: green synthesis, mesoporous silica, magnetic iron oxide NPs, adsorption Lindane

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Authors: Aasheesh Raturi, Vimal Kothiyal, P. D. Semalty

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We studied mechanical properties of Eucalyptus tereticornis using FT-NIR spectroscopy. Firstly, spectra were pre-processed to eliminate useless information. Then, prediction model was constructed by partial least squares regression. To study the influence of pre-processing on prediction of mechanical properties for NIR analysis of wood samples, we applied various pretreatment methods like straight line subtraction, constant offset elimination, vector-normalization, min-max normalization, multiple scattering. Correction, first derivative, second derivatives and their combination with other treatment such as First derivative + straight line subtraction, First derivative+ vector normalization and First derivative+ multiplicative scattering correction. The data processing methods in combination of preprocessing with different NIR regions, RMSECV, RMSEP and optimum factors/rank were obtained by optimization process of model development. More than 350 combinations were obtained during optimization process. More than one pre-processing method gave good calibration/cross-validation and prediction/test models, but only the best calibration/cross-validation and prediction/test models are reported here. The results show that one can safely use NIR region between 4000 to 7500 cm-1 with straight line subtraction, constant offset elimination, first derivative and second derivative preprocessing method which were found to be most appropriate for models development.

Keywords: FT-NIR, mechanical properties, pre-processing, PLS

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Authors: Philip Edinger, Christian Ludwig

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The formation and control of tars remain one of the major challenges in the implementation of biomass gasification technologies. Robust, on-line analytical methods are needed to investigate the fate of tar compounds when different measures for their reduction are applied. This work establishes an on-line UV-Vis method, based on a liquid quench sampling system, to monitor tar compounds in biomass gasification processes. Recorded spectra from the liquid phase were analyzed for their tar composition by means of a classical least squares (CLS) and partial least squares (PLS) approach. This allowed for the detection of UV-Vis active tar compounds with detection limits in the low part per million by volume (ppmV) region. The developed method was then applied to two case studies. The first involved a lab-scale reactor, intended to investigate the decomposition of a limited number of tar compounds across a catalyst. The second study involved a gas scrubber as part of a pilot scale wood gasification plant. Tar compound quantification results showed good agreement with off-line based reference methods (GC-FID) when the complexity of tar composition was limited. The two case studies show that the developed method can provide rapid, qualitative information on the tar composition for the purpose of process monitoring. In cases with a limited number of tar species, quantitative information about the individual tar compound concentrations provides an additional benefit of the analytical method.

Keywords: biomass gasification, on-line, tar, UV-Vis

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Authors: Mairaj Ahmad, L. Paglia, F. Marra, V. Genova, G. Pulci

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This study employed Rene N4 and FSX 414 superalloys, which are used in numerous turbine engine components due of their high strength, outstanding fatigue, creep, thermal, and corrosion-resistant properties. An in-depth examination of corrosion mechanisms with vapor present at high temperature is necessary given the industrial trend toward introducing increasing amounts of hydrogen into combustion chambers in order to boost power generation and minimize pollution in contrast to conventional fuels. These superalloys were oxidized in recent tests for 500, 1000, 2000, 3000 and 4000 hours at 982±5°C temperatures with a steady airflow at a flow rate of 10L/min and 1.5 bar pressure. These superalloys were also examined for wet corrosion for 500, 1000, 2000, 3000, and 4000 hours in a combination of air and water vapor flowing at a 10L/min rate. Weight gain, X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive x-ray spectroscopy (EDS) were used to assess the oxidation and heat corrosion resistance capabilities of these alloys before and after 500, 1000, and 2000 hours. The oxidation/corrosion processes that accompany the formation of these oxide scales are shown in the graph of mass gain vs time. In both dry and wet oxidation, oxides like Al2O3, TiO2, NiCo2O4, Ni3Al, Ni3Ti, Cr2O3, MnCr2O4, CoCr2O4, and certain volatile compounds notably CrO2(OH)2, Cr(OH)3, Fe(OH)2, and Si(OH)4 are formed.

Keywords: hot corrosion, oxidation, turbine materials, high temperature corrosion, super alloys

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Authors: Samia Khadhar, Anis Chekirbene, Nouha Khiari, Amira Mabrouki

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The persistent organic pollutants (POPs) in aquatic environments are one of the most worrying problems for environmental sustainability and human health because of their carcinogenic and toxic characteristics. Human anthropogenic actions (wastewater discharges, agricultural and industrial activities) without prior treatment are the main cause of this organic pollution. Oued Madjerda is considered the most important river in Tunisia, hence the importance of assessing the level of organic pollution of water and sediments, taking into account the anthropogenic stress exerted on this river. Water and sediment samples were taken from the middle and lower valley of the Medjerda to determine the state of contamination by 7PCBs, priority 15PAHs, and pesticides. The analysis was performed by gas chromatography (GC) and liquid phase coupled to HPLC MS-MS mass spectroscopy. The results showed that for the waters, the total PAH and PCB contents vary respectively from 0.0023 to 7.72 mg/l and from 0.0001 to 0.179 mg/l. In surface sediments 0 to 15 cm, 7PCB levels vary from 1,112 to 110,062 µg/kg-1. In this study, we tried to determine the concentration of 96 pesticides in surface sediments; analyzes showed the presence of Buprofezin, propamocarb-HCl, hexaconazole, flutriafol, quinalphos, and tebufenpyrad with concentrations varying from 1.06 to 2.388 µg/kg-1. The pace of the spatial variation confirms the impact of wastewater discharged on the quality of water and sediments despite the perennial aspect of the river.

Keywords: Wadi Madjerda, organic pollution, water and sediments surface, anthropics stress

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Authors: Asif Jamal, Samia Sakindar, Ramla Rehman

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Biosurfactants are amphiphilic surface active compounds obtained from natural resources such as plants and microorganisms. Because of their diverse physicochemical characteristics biosurfactant are replacing synthetic compounds in various commercial applications. In present study, a strain of P. aeruginosa was isolated from crude oil contaminated soil as efficient biosurfactant producers. The biosurfactant production was analyzed as a function of surface tension reduction, oil spreading capacity, emulsification index and hemolysis assay. This bacterial strain showed excellent emulsion activity of EI24 85%, surface tension reduction up to 28.6 mNm-1 and 7.0 mm oil displacement zone. Physicochemical and biological properties of extracted rhamnolipid were also investigated in current study. The chemical composition of product from strain PSS was analyzed by FTIR spectroscopy. The results revealed that extracted biosurfactant was rhamnolipid type in nature having RL-1 and RL-2 homologues. The surface behavior of rhamnolipid in aqueous phase was investigated varying extreme pH, temperature, salt conditions and with various hydrocarbons. The results indicated that biosurfactant produced by strain PSS Which showed stability during high temperature up to 121 C, salt concentrations up to 20% and pH range between (4—14). The emulsification activity with different hydrocarbons was also remarkable. It was concluded that rhamnolipid biosurfactant produced by strain PSS has excellent potential as emulsifying/remediation agent for broad range of hydrophobic pollutants.

Keywords: P. aeruginosa, bioremediation, rhamnolipid, surfactants

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Authors: Nurlan Akhmetov, Abilmansur Yeshmuratov, Aliya Kurbanova, Gulnar Sugurbekova, Murat Baisariyev

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Extraction of the vanadium and nickel compounds is complex due to the high stability of porphyrin, nickel is catalytic poison which deactivates catalysis during the catalytic cracking of the oil, while vanadyl is abrasive and valuable metal. Thus, high concentration of the Ni and V in the crude oil makes their removal relevant. Two methods of the demetallization of crude oil were tested, therefore, the present research is conducted for comparative analysis of the deasphalting with organic solvents (cyclohexane, carbon tetrachloride, chloroform) and electrochemical method. Percentage of Ni extraction reached maximum of approximately 55% by using the electrochemical method in electrolysis cell, which was developed for this research and consists of three sections: oil and protonating agent (EtOH) solution between two conducting membranes which divides it from two capsules of 10% sulfuric acid and two graphite electrodes which cover all three parts in electrical circuit. Ions of metals pass through membranes and remain in acid solutions. The best result was obtained in 60 minutes with ethanol to oil ratio 25% to 75% respectively, current fits in to the range from 0.3A to 0.4A, voltage changed from 12.8V to 17.3V. Maximum efficiency of deasphalting, with cyclohexane as the solvent, in Soxhlet extractor was 66.4% for Ni and 51.2% for V. Thus, applying the voltammetry, ICP MS (Inductively coupled plasma mass spectrometry) and AAS (atomic absorption spectroscopy), these mentioned types of metal extraction methods were compared in this paper.

Keywords: electrochemistry, deasphalting of crude oil, demetallization of crude oil, petrolium engineering

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Authors: Tadahiro Wada, Hiroyuki Hanyu

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In this study, to clarify the effectiveness of an aluminum/chromium/tungsten-based-coated tool for cutting sintered steel, tool wear was experimentally investigated. The sintered steel was turned with the (Al60,Cr25,W15)N-, (Al60,Cr25,W15)(C,N)- and (Al64,Cr28,W8)(C,N)-coated cemented carbide tools according to the physical vapor deposition (PVD) method. Moreover, the tool wear of the aluminum/chromium/tungsten-based-coated item was compared with that of the (Al,Cr)N coated tool. Furthermore, to clarify the tool wear mechanism of the aluminum/chromium/tungsten-coating film for cutting sintered steel, Scanning Electron Microscope observation and Energy Dispersive x-ray Spectroscopy mapping analysis were conducted on the abraded surface. The following results were obtained: (1) The wear progress of the (Al64,Cr28,W8)(C,N)-coated tool was the slowest among that of the five coated tools. (2) Adding carbon (C) to the aluminum/chromium/tungsten-based-coating film was effective for improving the wear-resistance. (3) The main wear mechanism of the (Al60,Cr25,W15)N-, the (Al60,Cr25,W15)(C,N)- and the (Al64,Cr28,W8)(C,N)-coating films was abrasive wear.

Keywords: cutting, physical vapor deposition coating method, tool wear, tool wear mechanism, (Al, Cr, W)N-coating film, (Al, Cr, W)(C, N)-coating film, sintered steel

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Authors: Noureddine Ramdani

Abstract:

In recent years, extensive attention has been given to the study of conductive nanocomposites due to their unique properties, which are dependent on their size and shape. The potential applications of these materials include electromagnetic interference shielding, energy storage, photovoltaics, and others. These outstanding properties have led to increased interest and research in this field. In this work, a conductive poly benzoxazine nanocomposite, PBZ/Gr-Cu, was synthesized through a compression molding technique to achieve a high-performance material suitable for electromagnetic interference (EMI) shielding applications. The microstructure of the nanocomposites was analyzed using scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR). The thermal stability, electrical conductivity, and EMI shielding properties of the nanocomposites were evaluated using thermogravimetric analysis, a four-point probe, and a VNA analyzer, respectively. The TGA results revealed that the thermal stability and electrical conductivity of the nanocomposites were significantly enhanced by the incorporation of Gr/Cu nanoparticles. The nanocomposites exhibited a low percolation threshold of about 3.5 wt.% and an increase in carrier concentration and mobility of the carriers with increasing hybrid nanofiller content, causing the composites to behave as n-type semiconductors. These nanocomposites also displayed a high dielectric constant and a high dissipation factor in the frequency range of 8-12 GHz, resulting in higher EMI shielding effectiveness (SE) of 25-44 dB. These characteristics make them promising candidates for lightweight EMI shielding materials in aerospace and radar evasion applications.

Keywords: polybenzoxazine matrix, conductive nanocomposites, electrical conductivity, EMI shielding

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Authors: Gehan El-Sayed Sharaf El-Deen

Abstract:

In this study, super paramagnetic iron-oxide nano- materials (SPMIN) were investigated for removal of toxic heavy metals from aqueous solution. The magnetic nanoparticles of 12 nm were synthesized using a co-precipitation method and characterized by transmission electron microscopy (TEM), transform infrared spectroscopy (FTIR), x-ray diffraction (XRD) and vibrating sample magnetometer (VSM). Batch experiments carried out to investigate the influence of different parameters such as contact time, initial concentration of metal ions, the dosage of SPMIN, desorption,pH value of solutions. The adsorption process was found to be highly pH dependent, which made the nanoparticles selectively adsorb these three metals from wastewater. Maximum sorption for all the studies cations obtained at the first half hour and reached equilibrium at one hour. The adsorption data of heavy metals studied were well fitted with the Langmuir isotherm and the equilibrium data show the percent removal of Ni2+, Zn2+ and Cd2+ were 96.5%, 80% and 75%, respectively. Desorption studies in acidic medium indicate that Zn2+, Ni2+ and Cd2+ were removed by 89%, 2% and 18% from the first cycle. Regeneration studies indicated that SPMIN nanoparticles undergoing successive adsorption–desorption processes for Zn2+ ions retained original metal removal capacity. The results revealed that the most prominent advantage of the prepared SPMIN adsorbent consisted in their separation convenience compared to the other adsorbents and SPMIN has high efficiency for removal the investigated metals from aqueous solution.

Keywords: heavy metals, magnetic nanoparticles, removal efficiency, Batch technique

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