Search results for: cationic impurities

Authors: Gule Teri

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The effective validation of analytical methods forms a crucial component of pharmaceutical manufacturing. However, traditional validation techniques can occasionally fail to fully account for inherent variations within datasets, which may result in inconsistent outcomes. This deficiency in validation accuracy is particularly noticeable when quantifying low concentrations of active pharmaceutical ingredients (APIs), excipients, or impurities, introducing a risk to the reliability of the results and, subsequently, the safety and effectiveness of the pharmaceutical products. In response to this challenge, we introduce an enhanced, tolerance-based Design of Experiments (DoE) approach for the validation of analytical methods. This approach distinctly measures variability with reference to tolerance or design margins, enhancing the precision and trustworthiness of the results. This method provides a systematic, statistically grounded validation technique that improves the truthfulness of results. It offers an essential tool for industry professionals aiming to guarantee the accuracy of their measurements, particularly for low-concentration components. By incorporating this innovative method, pharmaceutical manufacturers can substantially advance their validation processes, subsequently improving the overall quality and safety of their products. This paper delves deeper into the development, application, and advantages of this tolerance-based DoE approach and demonstrates its effectiveness using High-Performance Liquid Chromatography (HPLC) data for verification. This paper also discusses the potential implications and future applications of this method in enhancing pharmaceutical manufacturing practices and outcomes.

Keywords: tolerance-based design, design of experiments, analytical method validation, quality control, biopharmaceutical manufacturing

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Authors: Bekan Bogale, Tsegaye Girma Asere, Tilahun Yai, Fekadu Melak

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Aims: To study photocatalytic degradation of methylene blue dye on cuprous oxide/graphene nanocomposite. Background: Cuprous oxide (Cu2O) nanoparticles are among the metal oxides that demonstrated photocatalytic activity. However, the stability of Cu2O nanoparticles due to the fast recombination rate of electron/hole pairs remains a significant challenge in their photocatalytic applications. This, in turn, leads to mismatching of the effective bandgap separation, tending to reduce the photocatalytic activity of the desired organic waste (MB). To overcome these limitations, graphene has been combined with cuprous oxides, resulting in cuprous oxide/graphene nanocomposite as a promising photocatalyst. Objective: In this study, Cu2O/graphene nanocomposite was synthesized and evaluated for its photocatalytic performance of methylene blue (MB) dye degradation. Method: Cu2O/graphene nanocomposites were synthesized from graphite powder and copper nitrate using the facile sol-gel method. Batch experiments have been conducted to assess the applications of the nanocomposites for MB degradation. Parameters such as contact time, catalyst dosage, and pH of the solution were optimized for maximum MB degradation. The prepared nanocomposites were characterized by using UV-Vis, FTIR, XRD, and SEM. The photocatalytic performance of Cu2O/graphene nanocomposites was compared against Cu2O nanoparticles for cationic MB dye degradation. Results: Cu2O/graphene nanocomposite exhibits higher photocatalytic activity for MB degradation (with a degradation efficiency of 94%) than pure Cu2O nanoparticles (67%). This has been accomplished after 180 min of irradiation under visible light. The kinetics of MB degradation by Cu2O/graphene composites can be demonstrated by the second-order kinetic model. The synthesized nanocomposite can be used for more than three cycles of photocatalytic MB degradation. Conclusion: This work indicated new insights into Cu2O/graphene nanocomposite as high-performance in photocatalysis to degrade MB, playing a great role in environmental protection in relation to MB dye.

Keywords: methylene blue, photocatalysis, cuprous oxide, graphene nanocomposite

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Authors: Mouhamadou Diop, Mohamed I. Hassan

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Molten metallic flow in metallurgical plant is highly turbulent and presents a complex coupling with heat transfer, phase transfer, chemical reaction, momentum transport, etc. Molten silicon flow has significant effect in directional solidification of multicrystalline silicon by affecting the temperature field and the emerging crystallization interface as well as the transport of species and impurities during casting process. Owing to the complexity and limits of reliable measuring techniques, computational models of fluid flow are useful tools to study and quantify these problems. The overall objective of this study is to investigate the potential of a traveling magnetic field for an efficient operating control of the molten metal flow. A multidimensional numerical model will be developed for the calculations of Lorentz force, molten metal flow, and the related phenomenon. The numerical model is implemented in a laboratory-scale silicon crystallization furnace. This study presents the potential of traveling magnetic field approach for an efficient operating control of the molten flow. A numerical model will be used to study the effects of magnetic force applied on the molten flow, and their interdependencies. In this paper, coupled and decoupled, steady and unsteady models of molten flow and crystallization interface will be compared. This study will allow us to retrieve the optimal traveling magnetic field parameter range for crystallization furnaces and the optimal numerical simulations strategy for industrial application.

Keywords: multidimensional, numerical simulation, solidification, multicrystalline, traveling magnetic field

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Authors: Srikrishna Pramanik, Sree Chithra, Saurabh Rai, Sameeksha Agrawal, Debanggana Shil, Saptarshi Mukherjee

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The understanding of interactions between organic chromophores and biologically useful luminescent noble metal nanoclusters (NCs) leading to an energy transfer process that has applications in light-harvesting materials is still in its nascent stage. This work describes a photoluminescent supramolecular assembly, made in two stages, employing an energy transfer process between silver (Ag) NCs as the donor and a host-guest system as the acceptor that can find potential applications in diverse fields. Initially, we explored the host-guest chemistry between a cationic guest, Ethidium Bromide and the anionic host Cucurbit[8]uril using spectroscopic and calorimetric techniques to decipher their interaction mechanism in modulating photophysical properties of the chromophore. Next, we synthesized a series of blue-emitting AgNCs using different templates such as protein, peptides, and cyclodextrin. The as-prepared AgNCs were characterized by various spectroscopic techniques. We have established that these AgNCs can be employed as donors in the FRET process with the above acceptor for FRET-based emission color tuning. Our in-depth studies revealed that surface ligands play a key role in modulating FRET efficiency. Overall, by employing a non-covalent strategy, we have tried to develop FRET pairs using blue-emitting NCs and a host-guest complex, which could find potential applications in constructing advanced white light-emitting, anti-counterfeiting materials, and developing biosensors.

Keywords: absorption spectroscopy, cavities, energy transfer, fluorescence, fluorescence resonance energy transfer

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Authors: F. Z. Abir, M. Mesnaoui, Y. Abouliatim, L. Nibou, Y. El Hafiane, A. Smith

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The cement industry has been taking significant steps for years to reduce its carbon footprint by opting for an eco-friendly alternative such as Calcium Sulfoaluminate Cements (CSA). These binders, compared to Ordinary Portland Cements (OPC), have two advantages: reduction of the CO2 emissions and energy-saving because the sintering temperature of CSA cements is between 1250 and 1350 °C, which means 100 to 200 °C less than OPC. The aim of this work is to study the impurities effect, such as iron oxide, on the formation of the ye'elimite phase, which represents the main phase of Calcium Sulfoaluminate Cements and the consequence on its hydration. Several elaborations and characterization techniques were used to study the structure and microstructure of ye'elimite, such as X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), thermal analysis, specific surface area measurement, and electrical conductivity of diluted solutions. This study details the protocol for the solid-state synthesis of ye'elimite containing increasing amounts of iron (general formula: Ca4Al(6-2x)Fe2xSO16 with x = 0.00 to 1.13). Ye'elimite is formed by solid-state reactions between Al2O3, CaO and CaSO4 and the maximum ye'elimite content is reached at a sintering temperature of 1300 °C. The presence of iron promotes the formation of cubic ye'elimite at the expense of the orthorhombic phase. The total incorporation of iron in ye'elimite structure is possible when x < 0.12. Beyond this content, the ferritic phase (CaO)2(Al2O3,Fe2O3) appears as a minor phase and develops two different morphologies during cooling: dendritic crystals and melt morphology. The formation of the ferrous liquid phase affects the evolution of grain size of the ye’elimite and calcium aluminates.

Keywords: calcium sulfoaluminate cement, ferritic phase, sintering, solid-state synthesis, ye’elimite

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Authors: Dawid Stawski, Silviya Halacheva, Dorota Zielińska

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The surface properties of many materials can be readily and predictably modified by the controlled deposition of thin layers containing appropriate functional groups and this research area is now a subject of widespread interest. The layer-by-layer (lbl) method involves depositing oppositely charged layers of polyelectrolytes onto the substrate material which are stabilized due to strong electrostatic forces between adjacent layers. This type of modification affords products that combine the properties of the original material with the superficial parameters of the new external layers. Through an appropriate selection of the deposited layers, the surface properties can be precisely controlled and readily adjusted in order to meet the requirements of the intended application. In the presented paper a variety of anionic (poly(acrylic acid)) and cationic (linear poly(ethylene imine), polymers were successfully deposited onto the polypropylene nonwoven using the lbl technique. The chemical structure of the surface before and after modification was confirmed by reflectance FTIR spectroscopy, volumetric analysis and selective dyeing tests. As a direct result of this work, new materials with greatly improved properties have been produced. For example, following a modification process significant changes in the electrostatic activity of a range of novel nanocomposite materials were observed. The deposition of polyelectrolyte nanolayers was found to strongly accelerate the loss of electrostatically generated charges and to increase considerably the thermal resistance properties of the modified fabric (the difference in T50% is over 20°C). From our results, a clear relationship between the type of polyelectrolyte layer deposited onto the flat fabric surface and the properties of the modified fabric was identified.

Keywords: layer-by-layer technique, polypropylene nonwoven, surface modification, surface properties

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Authors: Ghazi R. Reda Mahmoud Reda

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Among the metal that forms hydride´s, Mg and Ti are known as the most lightweight materials; however, they are covered with a passive layer of oxides and hydroxides and require activation treatment under high temperature ( > 300 C ) and hydrogen pressure ( > 3 MPa) before being used for storage and transport applications. It is well known that small graphite addition to Ti or Mg, lead to a dramatic change in the kinetics of mechanically induced hydrogen sorption ( uptake) and significantly stimulate the Ti-Hydrogen interaction. Many explanations were given by different authors to explain the effect of graphite addition on the performance of Ti as material for hydrogen storage. Not only graphite but also the addition of a polycyclic aromatic compound will also improve the hydrogen absorption kinetics. It will be shown that the function of carbon addition is two-fold. First carbon acts as a vacuum cleaner, which scavenges out all the interstitial oxygen that can poison or slow down hydrogen absorption. It is also important to note that oxygen favors the chemisorption of hydrogen, which is not desirable for hydrogen storage. Second, during scavenging of the interstitial oxygen, the carbon reacts with oxygen in the nano and microchannel through a highly exothermic reaction to produce carbon dioxide and monoxide which provide the necessary heat for activation and thus in the presence of carbon lower heat of activation for hydrogen absorption which is observed experimentally. Furthermore, the product of the reaction of hydrogen with the carbon oxide will produce water which due to ball milling hydrolyze to produce the linear H5O2 + this will reconstruct the primary structure of the nanocarbon to form secondary structure, where the primary structure (a sheet of carbon) are connected through hydrogen bonding. It is the space between these sheets where physisorption or defect mediated sorption occurs.

Keywords: metal forming hydrides, polar molecule impurities, titanium, phase diagram, hydrogen absorption

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Authors: Mari Carmen Reyes Angeles, Dalia Michel Reyes Villeda, Ana María Herrera González

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This work reports the design and synthesis of two composite materials based on physically activated carbon and basic polyelectrolytes useful in the adsorption of textile dyes present in aqueous solutions and wastewater. The synthesis of basic polyelectrolytes poly(2-vinylpyridine) (P2VP) and poly(4-vinylpyridine) (P4VP) was made by means of free radical polymerization. The carbon made from prickly pear peel (CarTunaF) was thermally activated in the presence of combustion gases. Composite materials CarTunaF2VP and CarTunaF4VP were obtained from CarTunaF and polybasic polyelectrolytes P2VP and P4VP with a ratio of 67:33 wt. The structure of each polyelectrolyte, P2VP, and P4VP, was elucidated by means of the FTIR and 1H NMR spectrophotometric techniques. Their thermal stability was evaluated using TGA. The characterization of CarTunaF and composite materials CarTunaF2VP and CarTunaF4VP was made by means of FTIR, TGA, SEM, and N2 adsorption. The adsorptive capacities of the polyelectrolytes and the composite materials were evaluated by adsorption of direct dyes present in aqueous solutions. The polyelectrolytes removed between 90 and 100% of the dyes, and the composite materials removed between 68 and 93% of the dyes. Using the four adsorbents P2VP, P4VP, CarTuna2VP, and CarTuna4VP, it was observed that the dyes studied, Direct Blue 80, Direct Turquoise 86, and Direct Orange 26, were adsorbed in the range between 46.1 and 188.7mg∙g-1 by means of electrostatic interactions between the anionic groups in the dyes with the cationic groups in the adsorbents. By using adsorbent materials in the treatment of wastewater from the textile industry, an improvement in the quality of the water was observed by decreasing its pH, COD, conductivity, and color considerably

Keywords: adsorption, anionic dyes, composite, polyelectrolytes

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Authors: Asavasereerat K., Teacharsripaitoon T., Tungyingyong P., Charupongrat S., Noppiboon S. Hochareon L., Kitsuban P.

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Third generation of vaccines is based on gene therapy where DNA is introduced into patients. The antigenic or therapeutic proteins encoded from transgenes DNA triggers an immune-response to counteract various diseases. Moreover, DNA vaccine offers the customization of its ability on protection and treatment with high stability. The production of DNA vaccines become of interest. According to USFDA guidance for industry, the recommended limits for impurities from host cell are lower than 1%, and the active conformation homogeneity supercoiled DNA, is more than 80%. Thus, the purification strategy using two-steps chromatography has been established and verified for its robustness. Herein, pVax1/lacZ, a pre-approved USFDA DNA vaccine backbone, was used and transformed into E. coli strain DH5α. Three purification process parameters including sample-loading flow rate, the salt concentration in washing and eluting buffer, were studied and the experiment was designed using response surface method with central composite face-centered (CCF) as a model. The designed range of selected parameters was 10% variation from the optimized set point as a safety factor. The purity in the percentage of supercoiled conformation obtained from each chromatography step, AIEX and HIC, were analyzed by HPLC. The response data were used to establish regression model and statistically analyzed followed by Monte Carlo simulation using SAS JMP. The results on the purity of the product obtained from AIEX and HIC are between 89.4 to 92.5% and 88.3 to 100.0%, respectively. Monte Carlo simulation showed that the pVAX1/lacZ purification process is robust with confidence intervals of 0.90 in range of 90.18-91.00% and 95.88-100.00%, for AIEX and HIC respectively.

Keywords: AIEX, DNA vaccine, HIC, puification, response surface method, robustness

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Authors: Anna-Caroline Lavergne-Bril, Jean-François Colin, David Peralta, Pascale Maldivi

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Cobalt is a critical material, widely used in Li-ion batteries. Due to the planned electrification of European vehicles, cobalt needs are expending – and resources are limited. To meet the needs in cobalt to come, it is necessary to develop new efficient ways to recycle cobalt. One of the biggest sources comes from old electrical vehicles batteries (batteries sold in 2019: 500 000 tons of waste to be). A closed loop process of cobalt recycling has been developed and this presentation aims to present the selectivity mechanism of cobalt over manganese and nickel in solution. Cobalt precipitation as a ZIF material (Zeolitic Imidazolate framework) from a starting solution composed of equimolar nickel, manganese and cobalt is studied. A 2-MeIm (2-methylimidazole) linker is introduced in a multimetallic Ni, Mn, Co solution and the resulting ZIF-67 is 100% pure Co among its metallic centers. Selectivity of Co over Ni is experimentally studied and DFT modelisation calculation are conducted to understand the geometry of ligand-metal-solvent complexes in solution. Selectivity of Co over Mn is experimentally studied, and DFT modelisation calcucation are conducted to understand the link between pKa of the ligand and precipitration of Mn impurities within the final material. Those calculation open the way to other ligand being used in the same process, with more efficiency. Experimental material are synthetized from bimetallic (Ni²⁺/Co²⁺, Mn²⁺/Co²⁺, Mn²⁺/Ni²⁺) solutions. Their crystallographic structure is analysed by XRD diffraction (Brüker AXS D8 diffractometer, Cu anticathode). Morphology is studied by scanning electron microscopy, using a LEO 1530 FE-SEM microscope. The chemical analysis is performed by using ICP-OES (Agilent Technologies 700 series ICP-OES). Modelisation calculation are DFT calculation (density functional theory), using B3LYP, conducted with Orca 4.2.

Keywords: MOFs, ZIFs, recycling, closed-loop, cobalt, li-ion batteries

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Authors: Emily Rabe, Stephanie Candelaria, Rachel Malone, Olivia Lenz, Greg Newbloom

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Electrodialysis (ED) is a well-developed technology for ion removal in a variety of applications. However, many industries generate harsh wastewater streams that are incompatible with traditional ion exchange membranes. Membrion® has developed novel ceramic-based ion exchange membranes (IEMs) offering several advantages over traditional polymer membranes: high performance in low pH, chemical resistance to oxidizers, and a rigid structure that minimizes swelling. These membranes are synthesized with our patented silane-based sol-gel techniques. The pore size, shape, and network structure are engineered through a molecular self-assembly process where thermodynamic driving forces are used to direct where and how pores form. Either cationic or anionic groups can be added within the membrane nanopore structure to create cation- and anion-exchange membranes. The ceramic IEMs are produced on a roll-to-roll manufacturing line with low-temperature processing. Membrane performance testing is conducted using in-house permselectivity, area-specific resistance, and ED stack testing setups. Ceramic-based IEMs show comparable performance to traditional IEMs and offer some unique advantages. Long exposure to highly acidic solutions has a negligible impact on ED performance. Additionally, we have observed stable performance in the presence of strong oxidizing agents such as hydrogen peroxide. This stability is expected, as the ceramic backbone of these materials is already in a fully oxidized state. This data suggests ceramic membranes, made using sol-gel chemistry, could be an ideal solution for acidic and/or oxidizing wastewater streams from processes such as semiconductor manufacturing and mining.

Keywords: ion exchange, membrane, silane chemistry, nanostructure, wastewater

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Authors: Mohammed Panthakkal Abdul Muthalif, Shanmugasundaram Kanagaraj, Jumi Park, Hangyu Park, Youngson Choe

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The present study reports the incorporation of calcium ions into the CuS counter electrodes (CEs) in order to modify the photovoltaic performance of quantum dot-sensitized solar cells (QDSSCs). Metal ion-doped CuS thin film was prepared by the chemical bath deposition (CBD) method on FTO substrate and used directly as counter electrodes for TiO₂/CdS/CdSe/ZnS photoanodes based QDSSCs. For the Ca-doped CuS thin films, copper nitrate and thioacetamide were used as anionic and cationic precursors. Calcium nitrate tetrahydrate was used as doping material. The surface morphology of Ca-doped CuS CEs indicates that the fragments are uniformly distributed, and the structure is densely packed with high crystallinity. The changes observed in the diffraction patterns suggest that Ca dopant can introduce increased disorder into CuS material structure. EDX analysis was employed to determine the elemental identification, and the results confirmed the presence of Cu, S, and Ca on the FTO glass substrate. The photovoltaic current density – voltage characteristics of Ca-doped CuS CEs shows the specific improvements in open circuit voltage decay (Voc) and short-circuit current density (Jsc). Electrochemical impedance spectroscopy results display that Ca-doped CuS CEs have greater electrocatalytic activity and charge transport capacity than bare CuS. All the experimental results indicate that 20% Ca-doped CuS CE based QDSSCs exhibit high power conversion efficiency (η) of 4.92%, short circuit current density of 15.47 mA cm⁻², open circuit photovoltage of 0.611 V, and fill factor (FF) of 0.521 under illumination of one sun.

Keywords: Ca-doped CuS counter electrodes, surface morphology, chemical bath deposition method, electrocatalytic activity

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Authors: Yasuyuki Takahashi, Akemi Yoshida, Hirotaka Shimada

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99mTc-2-methoxy-isobutyl-isonitrile (MIBI) and 99mTcmercaptoacetylgylcylglycyl-glycine (MAG3 ) are heat to 368-372K and are labeled with 99mTc-pertechnetate. Quality control (QC) of 99mTc-labeled radiopharmaceuticals is performed at hospitals, using liquid chromatography, which is difficult to perform in general hospitals. We used chromatography strips to simplify QC and investigated the effects of the test procedures on quality control. In this study is 99mTc- MAG3. Solvent using chloroform + acetone + tetrahydrofuran, and the gamma counter was ARC-380CL. The changed conditions are as follows; heating temperature, resting time after labeled, and expiration year for use: which were 293, 313, 333, 353 and 372K; 15 min (293K and 372K) and 1 hour (293K); and 2011, 2012, 2013, 2014 and 2015 respectively were tested. Measurement time using the gamma counter was one minute. A nuclear medical clinician decided the quality of the preparation in judging the usability of the retest agent. Two people conducted the test procedure twice, in order to compare reproducibility. The percentage of radiochemical purity (% RCP) was approximately 50% under insufficient heat treatment, which improved as the temperature and heating time increased. Moreover, the % RCP improved with time even under low temperatures. Furthermore, there was no deterioration with time after the expiration date. The objective of these tests was to determine soluble 99mTc impurities, including 99mTc-pertechnetate and the hydrolyzed-reduced 99mTc. Therefore, we assumed that insufficient heating and heating to operational errors in the labeling. It is concluded that quality control is a necessary procedure in nuclear medicine to ensure safe scanning. It is suggested that labeling is necessary to identify specifications.

Keywords: quality control, tc-99m labeled radio-pharmaceutical, chromatography strip, nuclear medicine

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Authors: Nusaiba Al-Nemrawi, Belal Al-Husein

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Methotrexate (MTX) is a stoichiometric inhibitor of dihydrofolate reductase, which is essential for DNA synthesis. MTX is a chemotherapeutic agent used for treating many types of cancer cells. However, cells’ resistant to MTX is very common and its pharmacokinetic behavior is highly problematic. of MTX within tumor cells, we propose encapsulation of antitumor drugs in nanoparticulated systems. Chitosan (CS) is a naturally occurring polymer that is biocompatibe, biodegradable, non-toxic, cationic and bioadhesive. CS nanoparticles (CS-NPs) have been used as drug carrier for targeted delivery. Titanium dioxide (TiO2), a natural mineral oxide, which is used in biomaterials due to its high stability and antimicrobial and anticorrosive properties. TiO2 showed a potential as a tumor suppressor. In this study a new formulation of MTX loaded in CS NPs (CS-MTX NPs) and coated with Titanium oxide (TiO2) was prepared. The mean particle size, zeta potential, polydispersity index were measured. The interaction between CS NPs and TiO2 NPs was confirmed using FTIR and XRD. CS-MTX NPs was studied in vitro using the tumor cell line MCF-7 (human breast cancer). The results showed that CS-MTX has a size around 169 nm and as they were coated with TiO2, the size ranged between and depending on the ratio of CS-MTX to TiO2 ratio used in the preparation. All NPs (uncoated and coated carried positive charges and were monodispersed. The entrapment efficacy was around 65%. Both FTIR and XRD proved that TiO2 interacted with CS-MTX NPs. The drug invitro release was controlled and sustained over days. Finally, the studied in vitro using the tumor cell line MCF-7 suggested that combining nanomaterials with anticancer drugs CS-MTX NPs may be more effective than free MTX for cancer treatment. In conclusion, the combination of CS-MTX NPs and TiO2 NPs showed excellent time-dependent in vitro antitumor behavior, therefore, can be employed as a promising anticancer agent to attain efficient results towards MCF-7 cells.

Keywords: Methotrexate, Titanium dioxide, Chitosan nanoparticles, cancer

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Authors: Gurlal Singh, Rupinder Singh

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The possible role of the engine brake is to convert a power-producing engine into a power-absorbing retarding mechanism. In this braking system, exhaust gas (EG) from the internal combustion (IC) engines is used to operate air brake in the automobiles. Airbrake is most used braking system in vehicles. In the proposed model, instead of air brake, EG is used to operate the brake lever and stored in a specially designed tank. This pressure of EG is used to operate the pneumatic cylinder and brake lever. Filters used to remove the impurities from the EG, then it is allowed to store in the tank. Pressure relief valve is used to achieve a specific pressure in the tank and helps to avoid further damage to the tank as well as in an engine. The petrol engine is used in the proposed EG braking system. The petrol engine is chosen initially because it produces less impurity in the exhaust than diesel engines. Moreover, exhaust brake system (EBS) for the Diesel engines is composed of gate valve, pneumatic cylinder and exhaust brake valve with the on-off solenoid. Exhaust brake valve which is core component of EBS should have characteristics such as high reliability and long life. In a diesel engine, there is butterfly valve in exhaust manifold connected with solenoid switch which is used to on and off the butterfly valve. When butterfly valve closed partially, then the pressure starts built up inside the exhaust manifold and cylinder that actually resist the movement of piston leads to crankshaft getting stops resulting stopping of the flywheel. It creates breaking effect in a diesel engine. The exhaust brake is a supplementary breaking system to the service brake. It is noted that exhaust brake increased 2-3 fold the life of service brake may be due to the creation of negative torque which retards the speed of the engine. More study may also be warranted for the best suitable design of exhaust brake in a diesel engine.

Keywords: exhaust gas, automobiles, solenoid, airbrake

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Authors: Rahul Jarariya

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The textile industry uses various types of dyes and discharges a lot of highly coloured wastewater. It impacts the environment like allergic reaction, respiratory, skin problems, irritation to a mucous membrane, the upper respiratory tract has to the fore, Intoxicated dye discharges 40 to 50,000 tons with great concern. Spinel ferrites gained a lot of attention due to their wide application area from biomedical to wastewater treatment. Generally, spinel ferrite is known as M-Fe2O4. Spinel type nanoparticles possess high suspension stability. The synthesis method of Microwave solution combustion (MC) method is effective for nanoscale materials, including oxides, metals, alloys, and sulfides, works as fast and energy-efficient during the process. The review focuses on controlling, nanostructure and doping. The influence of the fuel concentration and the post-treatment temperature on the structural and magnetic properties. The effects of amounts of fuel and phase changes, particle size and shape, and magnetic properties can be characterized by various techniques. Urea is the most commonly used fuel. Ethanol or n-butanol is apt for removing impurities. As a result of the materials gives fine purity. Photocatalysis phenomena act with catalyst dosage to degrade dye from wastewater. Visible light responsive produces a large amount of hydroxyl (•OH) radical made the degradation efficiency of Rh21 type dye. It develops a narrow bandgap to make it suitable for enhanced photocatalytic activity.

Keywords: microwave solution combustion method, normal spinel, doped spinels, magnetic property, Rb21

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Authors: Seong Woon Lee, Soo Min Lim, Sung Sik Jeong, Jung Hoon Park

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The atmospheric concentration of greenhouse gas (GHG, Green House Gas) is increasing continuously as a result of the combustion of fossil fuels and industrial development. In response to this trend, many researches have been conducted on the reduction of GHG. Landfill gas (LFG, Land Fill Gas) is one of largest sources of GHG emissions containing the methane (CH₄) as a major constituent and can be considered renewable energy sources as well. In order to use LFG by connecting to the city pipe network, it required a process for removing impurities. In particular, oxygen must be removed because it can cause corrosion of pipes and engines. In this study, methane oxidation was used to eliminate oxygen from LFG and perovskite-type ceramic catalysts of La-Sr-Co-Fe-O composition was selected as a catalyst. Hollow fiber catalysts (HFC, Hollow Fiber Catalysts) have attracted attention as a new concept alternative because they have high specific surface area and mechanical strength compared to other types of catalysts. HFC was prepared by a phase-inversion/sintering technique using commercial La-Sr-Co-Fe-O powder. In order to measure the catalysts' activity, simulated LFG was used for feed gas and complete oxidation reaction of methane was confirmed. Pore structure of the HFC was confirmed by SEM image and perovskite structure of single phase was analyzed by XRD. In addition, TPR analysis was performed to verify the oxygen adsorption mechanism of the HFC. Acknowledgement—The project is supported by the ‘Global Top Environment R&D Program’ in the ‘R&D Center for reduction of Non-CO₂ Greenhouse gases’ (Development and demonstration of oxygen removal technology of landfill gas) funded by Korea Ministry of Environment (ME).

Keywords: complete oxidation, greenhouse gas, hollow fiber catalyst, land fill gas, oxygen removal, perovskite catalyst

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Authors: Alexa Rakoski, Yun Suk Eo, Cagliyan Kurdak, Priscila F. S. Rosa, Zachary Fisk, Monica Ciomaga Hatnean, Geetha Balakrishnan, Boyoun Kang, Myungsuk Song, Byungki Cho

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Samarium hexaboride (SmB6) is a strongly correlated mixed valence material and Kondo insulator. In the resistance-temperature curve, SmB6 exhibits activated behavior from 4-40 K after the Kondo gap forms. However, below 4 K, the resistivity is temperature independent or weakly temperature dependent due to the appearance of a topologically protected surface state. Current research suggests that the surface of SmB6 is conductive while the bulk is truly insulating, different from conventional 3D TIs (Topological Insulators) like Bi₂Se₃ which are plagued by bulk conduction due to impurities. To better understand why the bulk of SmB6 is so different from conventional TIs, this study employed a new method, called inverted resistance, to explore the lowest temperatures, as well as standard Hall measurements for the rest of the temperature range. In the inverted resistance method, current flows from an inner contact to an outer ring, and voltage is measured outside of this outer ring. This geometry confines the surface current and allows for measurement of the bulk resistivity even when the conductive surface dominates transport (below 4 K). The results confirm that the bulk of SmB6 is truly insulating down to 2 K. Hall measurements on a number of samples show consistent bulk behavior from 4-40 K, but widely varying behavior among samples above 40 K. This is attributed to a combination of the growth process and purity of the starting material, and the relationship between the high and low temperature behaviors is still being explored.

Keywords: bulk transport, Hall effect, inverted resistance, Kondo insulator, samarium hexaboride, topological insulator

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Authors: Raviteja Chintala

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Water shortage in many areas of the world have predominantly increased the demand for efficient methods involved in the production of drinking water, So purification of water invoking cost effective and efficient methods is a challenging field of research. In this regard, Reverse osmosis membrane desalination of both seawater and inland brackish water is currently being deployed in various locations around the world. In the present work an attempt is made to integrate these existing technologies with novel method, Wherein carbon nanotubes at the lab scale are prepared which further replace activated carbon tubes being used traditionally. This has proven to enhance the efficiency of the water filter, Effectively neutralising most of the organic impurities. Furthermore, This ensures the reduction in TDS. Carbon nanotubes have wide range in scope of applications such as composite reinforcements, Field emitters, Sensors, Energy storage and energy conversion devices and catalysts support phases, Because of their unusual mechanical, Electrical, Thermal and structural properties. In particular, The large specific surface area, as well as the high chemical and thermal stability, Makes carbon nanotube an attractive adsorbent in waste water treatment. Carbon nanotubes are effective in eliminating these harmful media from water as an adsorbent. In this work, Candle soot method has been incorporated for the preparation of carbon nanotubes and mixed with activated charcoal in different compositions. The effect of composition change is monitored by using TDS measuring meter. As the composition of Nano carbon increases, The TDS of the water gradually decreases. In order to enhance the life time for carbon filter, Nano tubes are provided with larger surface area.

Keywords: TDS (Total Dissolved Solids), carbon nanotubes, water, candle soot

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Authors: Ratnakumar V. Kappagantula, Gordon D. Ingram, Hari B. Vuthaluru

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This paper analyzes a three reactor chemical looping process for hydrogen production from natural gas, allowing for carbon dioxide capture through chemical looping technology. An oxygen carrier is circulated to separate carbon dioxide, to reduce steam for hydrogen production and to supply oxygen for combustion. In this study, the emphasis is placed on the steam conversion in the steam reactor by investigating the hydrogen efficiencies of the complete system at steam conversions of 15.8% and 50%. An Aspen Plus model was developed for a Three Reactor Chemical Looping process to study the effects of operational parameters on hydrogen production is investigated. Maximum hydrogen production was observed under stoichiometric conditions. Different conversions in the steam reactor, which was modelled as a Gibbs reactor, were found when Gibbs-identified products and user identified products were chosen. Simulations were performed for different oxygen carriers, which consist of an active metal oxide on an inert support material. For the same metal oxide mass flowrate, the fuel reactor temperature decreased for different support materials in the order: aluminum oxide (Al2O3) > magnesium aluminate (MgAl2O4) > zirconia (ZrO2). To achieve the same fuel reactor temperature for the same oxide mass flow rate, the inert mass fraction was found to be 0.825 for ZrO2, 0.7 for MgAl2O4 and 0.6 for Al2O3. The effect of poisoning of the oxygen carrier was also analyzed. With 3000 ppm sulfur-based impurities in the feed gas, the hydrogen product energy rate of the process were found to decrease by 0.4%.

Keywords: aspen plus, chemical looping combustion, inert support balls, oxygen carrier

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Authors: Florian Billing, Soren Segan, Meike Jakobi, Elsa Arefaine, Aliki Jerch, Xin Xiong, Matthias Becker, Thomas Joos, Burkhard Schlosshauer, Ulrich Rothbauer, Nicole Schneiderhan-Marra, Hanna Hartmann, Christopher Shipp

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The immune response plays a major role in implant biocompatibility, but an understanding of how to design biomaterials for specific immune responses is yet to be achieved. We aimed to better understand how changing certain material properties can drive immune responses. To this end, we tested immune response to experimental implant coatings that vary in specific characteristics. A layer-by-layer approach was employed to vary surface charge and wettability. Human-based in vitro models (THP-1 macrophages and primary peripheral blood mononuclear cells (PBMCS)) were used to assess immune responses using multiplex cytokine analysis, flow cytometry (CD molecule expression) and microscopy (cell morphology). We observed dramatic differences in immune response due to specific alterations in coating properties. For example altering the surface charge of coating A from anionic to cationic resulted in the substantial elevation of the pro-inflammatory molecules IL-1beta, IL-6, TNF-alpha and MIP-1beta, while the pro-wound healing factor VEGF was significantly down-regulated. We also observed changes in cell surface marker expression in relation to altered coating properties, such as CD16 on NK Cells and HLA-DR on monocytes. We furthermore observed changes in the morphology of THP-1 macrophages following cultivation on different coatings. A correlation between these morphological changes and the cytokine expression profile is ongoing. Targeted changes in biomaterial properties can produce vast differences in immune response. The properties of the coatings examined here may, therefore, be a method to direct specific biological responses in order to improve implant biocompatibility.

Keywords: biomaterials, coatings, immune system, implants

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Authors: Meltem Haktaniyan, Eda Cagli, Irem Erel Goktepe

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Polymers that change their properties in response to different stimuli (e.g. light, temperature, pH, ionic strength or magnetic field) are called ‘smart’ or ‘stimuli-responsive polymers’. These polymers have been widely used in biomedical applications such as sensors, gene delivery, drug delivery or tissue engineering. Temperature-responsive polymers have been studied extensively for controlled drug delivery applications. As regard of pseudo-peptides, poly (2-alky-2-oxazoline)s are considered as good candidates for delivery systems due to their stealth behavior and nontoxicity. In order to build responsive multilayer films for controlled drug release applications from surface, Layer by layer technique (LBL) is a powerful technique with an advantage of nanometer scale control over spatial architecture and morphology. Multilayers can be constructed on surface where non-covalent interactions including electrostatic interactions, hydrogen bonding, and charge-transfer or hydrophobic-hydrophobic interactions. In the present study, hydrogen bounded multilayer films of poly (2-alky-2-oxazoline) s with tannic acid were prepared in order to use as a platform to release Doxorubicin (DOX) from surface with pH and thermal triggers. For this purpose, poly (2-isopropyl-2-oxazoline) (PIPOX) and poly (2-ethyl-2-oxazoline) (PETOX) were synthesized via cationic ring opening polymerization (CROP) with hydroxyl end groups. Two polymeric multilayer systems ((PETOX)/(DOX)-(TA) complexes and (PIPOX)/(DOX)-(TA) complexes) were designed to investigate of controlled release of Doxorubicin (DOX) from surface with pH and thermal triggers. The drug release profiles from the multilayer thin films with alterations of pH and temperature will been examined with UV-Vis Spectroscopy and Fluorescence Spectroscopy.

Keywords: temperature responsive polymers, h-bonded multilayer films, drug release, polyoxazoline

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Authors: Alexey Yu. Postnikov, Nikolay T. Kazakovskiy, Valery V. Mokrushin, Irina A. Tsareva, Andrey A. Potekhin, Valentina N. Golubeva, Yuliya V. Potekhina, Maxim V. Tsarev

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The development of tritium and deuterium targets for neutron tubes and generators is a part of the activities in All-Russia Research Institute of Experimental Physics (RFNC-VNIIEF). These items contain a metal substrate (for example, copper) with a titanium film with a few microns thickness deposited on it. Then these metal films are saturated with tritium, deuterium or their mixtures. The significant problem in neutron tubes and neutron generators is the characterization of substrate surface before a deposition of titanium film on it, and analysis of the deposited titanium film’s surface before hydrogenation and after a saturation of the film with hydrogen isotopes. The performance effectiveness of neutron tube and generator also depends on upon the quality parameters of the surface of the initial substrate, deposited metal film and hydrogenated target. The objective of our work is to study the target prototype samples, that have differ by various approaches to the preliminary chemical processing of a copper substrate, and to analyze the integrity of titanium film after its saturation with deuterium. The research results of copper substrate and the surface of deposited titanium film with the use of electron microscopy, X-ray spectral microanalysis and laser-spark methods of analyses are presented. The causes of surface defects appearance have been identified. The distribution of deuterium and some impurities (oxygen and nitrogen) along the surface and across the height of the hydrogenated film in the target has been established. This allows us to evaluate the composition homogeneity of the samples and consequently to estimate the quality of hydrogenated samples. As the result of this work the propositions on the advancement of production technology and characterization of target’s surface have been presented.

Keywords: tritium and deuterium targets, titanium film, laser-spark methods, electron microscopy

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Authors: Mumtaz Khan, Adeel Shahid, Waqas Khan

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Heavy metals presence in water streams is a big danger for aquatic life and ultimately effects human health. Removal of copper (Cu) by ispaghula husk, maize fibre, and maize oil cake from synthetic solution in batch conditions was studied. Different experimental parameters such as contact time, initial solution pH, agitation rate, initial Cu concentration, biosorbent concentration, and biosorbent particle size has been studied to quantify the Cu biosorption. The rate of adsorption of metal ions was very fast at the beginning and became slow after reaching the saturation point, followed by a slower active metabolic uptake of metal ions into the cells. Up to a certain point, (pH=4, concentration of Cu = ~ 640 mg/l, agitation rate = ~ 400 rpm, biosorbent concentration = ~ 0.5g, 3g, 3g for ispaghula husk, maize fiber and maize oil cake, respectively) increasing the pH, concentration of Cu, agitation rate, and biosorbent concentration, increased the biosorption rate; however the sorption capacity increased by decreasing the particle size. At optimized experimental parameters, the maximum Cu biosorption by ispaghula husk, maize fibre and maize oil cake were 86.7%, 59.6% and 71.3%, respectively. Moreover, the results of the kinetics studies demonstrated that the biosorption of copper on ispaghula husk, maize fibre, and maize oil cake followed pseudo-second order kinetics. The results of adsorption were fitted to both the Langmuir and Freundlich models. The Langmuir model represented the sorption process better than Freundlich, and R² value ~ 0.978. Optimizations of physical and environmental parameters revealed, ispaghula husk as more potent copper biosorbent than maize fibre, and maize oil cake. The sorbent is cheap and available easily, so this study can be applied to remove Cu impurities on pilot and industrial scale after certain modifications.

Keywords: biosorption, copper, ispaghula husk, maize fibre, maize oil cake, purification

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Authors: Hamideh Hamedi, Nima Rezaei, Sohrab Zendehboudi

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Separating emulsified oil contaminations from waste- or produced water is of interest to various industries. Magnetic particles (MPs) application for separating dispersed and emulsified oil from wastewater is becoming more popular. Stabilization of MPs is required through developing a coating layer on their surfaces to prevent their agglomeration and enhance their dispersibility. In this research, we study the effects of coating material, size, and concentration of iron oxide MPs on oil separation efficiency, using oil adsorption capacity measurements. We functionalize both micro-and nanoparticles of Fe3O4 using sodium dodecyl sulfate (SDS) as an anionic surfactant, cetyltrimethylammonium bromide (CTAB) as a cationic surfactant, and stearic acid (SA). The chemical structures and morphologies of these particles are characterized using Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), and Energy Dispersive X-ray (EDX). The oil-water separation results indicate that a low dosage of the coated magnetic nanoparticle with CTAB (0.5 g/L MNP-CTAB) results the highest oil adsorption capacity (nearly 100%) for 1000 ppm dodecane-in-water emulsion, containing ultra-small droplets (250–300 nm). While separation efficiency of the same dosage of bare MNPs is around 57.5%. Demulsification results of magnetic microparticles (MMPs) also reveal that the functionalizing particles with CTAB increase oil removal efficiency from 86.3% for bare MMP to 92% for MMP-CTAB. Comparing the results of different coating materials implies that the major interaction reaction is an electrostatic attraction between negatively charged oil droplets and positively charged MNP-CTAB and MMP-CTAB. Furthermore, the synthesized nanoparticles could be recycled and reused; after ten cycles the oil adsorption capacity slightly decreases to near 95%. In conclusion, functionalized magnetic particles with high oil separation efficiency could be used effectively in treatment of oily wastewater. Finally, optimization of the adsorption process is required by considering the effective system variables, and fluid properties.

Keywords: oily wastewater treatment, emulsions, oil-water separation, adsorption, magnetic nanoparticles

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Authors: Samane Maroufi, Rasoul Khayyam Nekouei, Sajjad Sefimofarah, Veena Sahajwalla

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The present work details a three-stage strategy based on selective purification of rare earth oxide (REOs) isolated from end-of-life nickel-metal hydride (Ni-MH) batteries leading to high-yield fabrication of defect-rich Mn1-x-y(CeₓLaᵧ)O2-δ film. In step one, major impurities (Fe and Al) were removed from a REE-rich solution. In step two, the resulting solution with trace content of Mn was further purified through electrodeposition which resulted in the synthesis of a non-stoichiometric Mn₋₁₋ₓ₋ᵧ(CeₓLaₓᵧ)O2-δ ultra-thin film, with controllable thicknesses (5-650 nm) and transmittance (~29-100%)in which Ce4+/3+ and La3+ ions were dissolved in MnO2-x lattice. Due to percolation impacts on the optoelectronic properties of ultrathin films, a representative Mn1-x-y(CexLay)O2-δ film with 86% transmittance exhibited an outstanding areal capacitance of 3.4 mF•cm-2, mainly attributed to the intercalation/de-intercalation of anionic O2- charge carriers through the atomic tunnels of the stratified Mn1-x-y(CexLay)O2-δ crystallites. Furthermore, the Mn1-x-y(CexLay)O2-δ exhibited excellent capacitance retention of ~90% after 16,000 cycles. Such stability was shown to be associated with intervalence charge transfers occurring among interstitial Ce/La cations and Mn oxidation states within the Mn₋₁₋ₓ₋ᵧ(CexLay)O2-δ structure. The energy and power densities of the transparent flexible Mn₋₁₋ₓ₋ᵧ(CexLay)O2-δ full-cell pseudocapacitor device with a solid-state electrolyte was measured to be 0.088 µWh.cm-2 and 843 µW.cm-2, respectively. These values showed insignificant changes under vigorous twisting and bending to 45-180˚, confirming these materials are intriguing alternatives for size-sensitive energy storage devices. In step three, the remaining solution purified further, that led to the formation of REOs (La, Ce, and Nd) nanospheres with ~40-50 nm diameter.

Keywords: spent Ni-MH batteries, green energy, flexible pseudocapacitor, rare earth elements

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Authors: Ji-Hoon Byeon, Kwon-Hee Lee

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Strainer filter serves to block the inflow of impurities while mixed fluid is entering or exiting the piping. The filter of the strainer has a perforated structure, so that the pressure drop and the velocity change necessarily occur when the mixed fluid passes through the filter. It is possible to predict the pressure drop and velocity change of the strainer by numerical analysis by implementing all the perforated plates. However, if the size of the perforated plate exceeds a certain size, it is difficult to perform the numerical analysis, and sometimes we cannot guarantee its accuracy. In this study, we tried to predict the pressure drop and velocity change by using the porous media technique to obtain the equivalent resistance without actual implementation of the perforation shape of the strainer. Ansys-CFX, a commercial software, is used to perform the numerical analysis. The analysis procedure is as follows. Firstly, the unit pattern of the perforated plate is modeled, and the pressure drop is analyzed by varying the velocity by symmetry of the wall surface. Secondly, since the equation for obtaining resistance is a quadratic equation of pressure having unknown velocity, the viscous resistance and the inertia resistance of the perforated plate are obtained from the relationship between pressure and speed. Thirdly, by using the calculated resistance values, the values are substituted into the flat plate implemented as a two-dimensional porous media, and the accuracy is verified by comparing the pressure drop and the velocity change. Fourthly, the pressure drop and velocity change in the whole strainer are analyzed by using the resistance values obtained on the perforated plate in the actual whole strainer model. Using the porous media technique, it is found that pressure drop and velocity change can be predicted in relatively short time without modeling the overall shape of the filter. Acknowledgements: This work was supported by the Valve Center from the Regional Innovation Center(RIC) Program of Ministry of Trade, Industry & Energy (MOTIE).

Keywords: strainer, porous media, CFD, numerical analysis

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Authors: Chandra Shekhar Verma, Umesh Chandra Mishra

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Blast Furnace performance mainly depends on the quality of sinter as a major portion of iron-bearing material occupies by it hence its quality w.r.t. Tumbler Index (TI), Reducibility Index (RI) and Reduction Degradation Index (RDI) are the key performance indicators of sinter plant. Now it became very tough to maintain the desired quality with the increasing alumina (Al₂O₃) content in iron fines and study is focused on it. Alumina is a refractory material and required more heat input to fuse thereby affecting the desired sintering temperature, i.e. 1300°C. It goes in between the grain boundaries of the bond and makes it weaker. Sinter strength decreases with increasing alumina content, and weak sinter generates more fines thereby reduces the net sinter production as well as plant productivity. Presence of impurities beyond the acceptable norm: such as LOI, Al₂O₃, MnO, TiO₂, K₂O, Na₂O, Hydrates (Goethite & Limonite), SiO₂, phosphorous and zinc, has led to greater challenges in the thrust areas such as productivity, quality and cost. The ultimate aim of this study is maintaining the sinter strength even with high Al₂O without hampering the plant productivity. This study includes mineralogy test of iron fines to find out the fraction of different phases present in the ore and phase analysis of product sinter to know the distribution of different phases. Corrections were done focusing majorly on varying Al₂O₃/SiO₂ ratio, basicity: B2 (CaO/SiO₂), B3 (CaO+MgO/SiO₂) and B4 (CaO+MgO/SiO₂+Al₂O₃). The concept of Alumina / Silica ratio, B3 & B4 found to be useful. We used to vary MgO, Al₂O₃/SiO₂, B2, B3 and B4 to get the desired sinter strength even at high alumina (4.2 - 4.5%) in sinter. The study concludes with the establishment of B4, and Al₂O₃/SiO₂ ratio in between 1.53-1.60 and 0.63- 0.70 respectively and have achieved tumbler index (Drum Index) 76 plus with the plant productivity of 1.58-1.6 t/m2/hr. at JSPL, Raigarh. Study shows that despite of high alumina in sinter, its physical quality can be controlled by maintaining the above-mentioned parameters.

Keywords: Basicity-2, Basicity-3, Basicity-4, Sinter

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Authors: Haiming Wen

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Grain growth is an important and consequential phenomenon that generally occurs in the presence of thermal and/or stress/strain fields. Thermally activated grain growth has been extensively studied and similarly, there are numerous experimental and theoretical studies published describing stress-induced grain growth in single-phase materials. However, studies on grain growth during the simultaneous presence of an elevated temperature and an external stress are very limited, and moreover, grain growth phenomena in materials containing second-phase particles and solute segregation at GBs have received limited attention. This lecture reports on a study of grain growth in the presence of second-phase particles and solute/impurity segregation at grain boundaries (GBs) during high-temperature deformation of an ultra-fine grained (UFG) Al alloy synthesized via consolidation of mechanically milled powders. The mechanisms underlying the grain growth were identified as GB migration and grain rotation, which were accompanied by dynamic recovery and geometric dynamic recrystallization, while discontinuous dynamic recrystallization was not operative. A theoretical framework that incorporates the influence of second-phase particles and solute/impurity segregation at GBs on grain growth in presence of both elevated temperature and external stress is formulated and discussed. The effect of second-phase particles and solute/impurity segregation at GBs on GB migration and grain rotation was quantified using the proposed theoretical framework, indicating that both second-phase particles and solutes/impurities segregated GBs reduce the velocities of GB migration and grain rotation as compared to those in commercially pure Al. Our results suggest that grain growth predicted by the proposed theoretical framework is in agreement with experimental results. Hence, the developed theoretical framework can be applied to quantify grain growth in simultaneous presence of external stress, elevated temperature, GB segregation and second-phase particles, or in presence of one or more of the aforementioned factors.

Keywords: nanocrystalline materials, ultra-fine grained materials, grain growth, grain boundary migration, grain rotation

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Authors: Ben Yahia Nouha, Sebei Abdelaziz, Boussen Slim, Chaabani Fredj

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The present work aims to determine mineralogical and geochemical characteristics of siliceous rock levels and to clarify the origin through geochemical arguments. This study was performed on the deposit of Tabarka-Babouch, which belongs to the northwestern of Tunisia; they spread out the later Miocene. Investigations were carried out to study mineralogical structure by XRD and chemical analysis by ICP-AES. The X-ray diffraction (XRD) patterns of the powdered natural rocks show that the Babouchite is composed mainly of quartz and clay minerals (smectite, illite, and kaolinite). Siliceous rocks contain quartz as a major silica mineral, which is characterized by two broad reflections at the vicinity of 4.26Å and 3.34 Å, respectively, with a total lack of opal-CT. That confirms that these siliceous rocks are quartz-rich (can reach 90%). Indeed, the amounts of all clay minerals (ACM), constituted essentially by smectite marked by a close association with illite and kaolinite, are relatively high, where their percentages vary from 7 to 46%. Chemical analyses show that the major oxide contents are consistent with mineralogical observations. It reveals that the siliceous rocks of the Babouchite formation are rich in SiO₂. The data of whole-rock chemical analyses indicate that the SiO₂ content is generally in the range 73-91 wt.%; (average: 80.43 wt.%). The concentration of Al₂O₃, which represent the detrital fractions in the studied samples, varies from 3.99 to 10.55 wt. % and Fe₂O₃ from 0.73 to 4.41wt. %. The low levels recorded in CaO (%) show that the carbonate is considered impurities. However, these rocks contain a low amount of some others oxides, such as the following: Na₂O, MgO, K₂O, and TiO₂. The trace elemental distributions also vary with high Sr (up to 84.55 ppm), Cu (5–127 ppm), and Zn (up to 124 ppm), with a relatively lower concentration of Co (2.43-25.54 ppm), Cr (10–61 ppm) and Pb (8-22ppm). The Babouchite siliceous rocks of northwestern of Tunisia have generally high Al/ (Al+Fe+Mn) values (0.63-0.83). The majority of Al/ (Al+Fe+Mn) values are nearly of 0.6, which is the biogenic end-member. Thus, Al/ (Al+Fe+Mn) values revealed the biogenic origin of silica.

Keywords: siliceous rocks, Babouchite formation, XRD, chemical analysis, biogenic silica, Northwestern of Tunisia

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