Search results for: chemical synthesis

Authors: Zainab Bibi, Afsheen Aman, Shah Ali Ul Qader

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Endo-β-1,4-xylanases [EC 3.2.1.8] are one of the major groups of enzymes that are involved in degradation process of xylan and have several applications in food, textile and paper processing industries. Due to broad utility of endo-β-1,4-xylanase, researchers are focusing to increase the productivity of this hydrolase from various microbial species. Harsh industrial condition, faster reaction rate and efficient hydrolysis of xylan with low risk of contamination are critical requirements of industry that can be fulfilled by synthesizing the enzyme with efficient properties. In the current study, a newly isolated thermophile Geobacillus stearothermophilus KIBGE-IB29 was used in order to attain the maximum production of endo-1,4-β-xylanase. Bacterial culture was isolated from soil, collected around the blast furnace site of a steel processing mill, Karachi. Optimization of various nutritional and physical factors resulted the maximum synthesis of endo-1,4-β-xylanase from a thermophile. High production yield was achieved at 60°C and pH-6.0 after 24 hours of incubation period. Various nitrogen sources viz. peptone, yeast extract and meat extract improved the enzyme synthesis with 0.5%, 0.2% and 0.1% optimum concentrations. Dipotassium hydrogen phosphate (0.25%), potassium dihydrogen phosphate (0.05%), ammonium sulfate (0.05%) and calcium chloride (0.01%) were noticed as valuable salts to improve the production of enzyme. The thermophilic nature of isolate, with its broad pH stability profile and reduced fermentation time indicates its importance for effective xylan saccharification and for large scale production of endo-1,4-β-xylanase.

Keywords: geobacillus, optimization, production, xylanase

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Authors: Anna Kolanowska, Anna Kuziel, Sławomir Boncel

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Carbon nanotubes (CNTs) represent a combination of lightness and nanoscopic size with high tensile strength, excellent thermal and electrical conductivity. By now, CNTs have been used as a support in heterogeneous catalysis (CuCl anchored to pre-functionalized CNTs) in the Ullmann-type coupling with aryl halides toward formation of C-N and C-O bonds. The results indicated that the stability of the catalyst was much improved and the elaborated catalytic system was efficient and recyclable. However, CNTs have not been considered as the substrate itself in the Ullmann-type reactions. But if successful, this functionalization would open new areas of CNT chemistry leading to enhanced in-solvent/matrix nanotube individualization. The copper-catalyzed Ullmann-type reaction is an attractive method for the formation of carbon-heteroatom and carbon-carbon bonds in organic synthesis. This condensation reaction is usually conducted at temperature as high as 200 oC, often in the presence of stoichiometric amounts of copper reagent and with activated aryl halides. However, a small amount of organic additive (e.g. diamines, amino acids, diols, 1,10-phenanthroline) can be applied in order to increase the solubility and stability of copper catalyst, and at the same time to allow performing the reaction under mild conditions. The copper (pre-)catalyst is prepared by in situ mixing of copper salt and the appropriate chelator. Our research is focused on the application of Ullmann-type reaction for the covalent functionalization of CNTs. Firstly, CNTs were chlorinated by using iodine trichloride (ICl3) in carbon tetrachloride (CCl4). This method involves formation of several chemical species (ICl, Cl2 and I2Cl6), but the most reactive is the dimer. The fact (that the dimer is the main individual in CCl4) is the reason for high reactivity and possibly high functionalization levels of CNTs. This method, indeed, yielded a notable amount of chlorine onto the MWCNT surface. The next step was the reaction of CNT-Cl with three substrates: aniline, iodobenzene and phenol for the formation C-N, C-C and C-O bonds, respectively, in the presence of 1,10-phenanthroline and cesium carbonate (Cs2CO3) as a base. As the CNT substrates, two multi-wall CNT (MWCNT) types were used: commercially available Nanocyl NC7000™ (9.6 nm diameter, 1.5 µm length, 90% purity) and thicker MWCNTs (in-house) synthesized in our laboratory using catalytic chemical vapour deposition (c-CVD). In-house CNTs had diameter ranging between 60-70 nm and length up to 300 µm. Since classical Ullmann reaction was found as suffering from poor yields, we have investigated the effect of various solvents (toluene, acetonitrile, dimethyl sulfoxide and N,N-dimethylformamide) on the coupling of substrates. Owing to the fact that the aryl halides show the reactivity order of I>Br>Cl>F, we have also investigated the effect of iodine presence on CNT surface on reaction yield. In this case, in first step we have used iodine monochloride instead of iodine trichloride. Finally, we have used the optimized reaction conditions with p-bromophenol and 1,2,4-trihydroxybenzene for the control of CNT dispersion.

Keywords: carbon nanotubes, coupling reaction, functionalization, Ullmann reaction

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Authors: Laura Elena De León Prado, Dora Alicia Cortés Hernández, Javier Sánchez

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Among the different cancer treatments that are currently used, hyperthermia has a promising potential due to the multiple benefits that are obtained by this technique. In general terms, hyperthermia is a method that takes advantage of the sensitivity of cancer cells to heat, in order to damage or destroy them. Within the different ways of supplying heat to cancer cells and achieve their destruction or damage, the use of magnetic nanoparticles has attracted attention due to the capability of these particles to generate heat under the influence of an external magnetic field. In addition, these nanoparticles have a high surface area and sizes similar or even lower than biological entities, which allow their approaching and interaction with a specific region of interest. The most used magnetic nanoparticles for hyperthermia treatment are those based on iron oxides, mainly magnetite and maghemite, due to their biocompatibility, good magnetic properties and chemical stability. However, in order to fulfill more efficiently the requirements that demand the treatment of magnetic hyperthermia, there have been investigations using ferrites that incorporate different metallic ions, such as Mg, Mn, Co, Ca, Ni, Cu, Li, Gd, etc., in their structure. This paper reports the synthesis of nanosized Mg_xMn_1-xFe₂O₄ (x = 0.3 and 0.4) ferrites by sol-gel method and their evaluation in terms of heating capability and in vitro hemolysis to determine the potential use of these nanoparticles as thermoseeds for the treatment of cancer by magnetic hyperthermia. It was possible to obtain ferrites with nanometric sizes, a single crystalline phase with an inverse spinel structure and a behavior near to that of superparamagnetic materials. Additionally, at concentrations of 10 mg of magnetic material per mL of water, it was possible to reach a temperature of approximately 45°C, which is within the range of temperatures used for the treatment of hyperthermia. The results of the in vitro hemolysis assay showed that, at the concentrations tested, these nanoparticles are non-hemolytic, as their percentage of hemolysis is close to zero. Therefore, these materials can be used as thermoseeds for the treatment of cancer by magnetic hyperthermia.

Keywords: ferrites, heating capability, hemolysis, nanoparticles, sol-gel

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Authors: Nadjiba Meziou-Chebouti, Amel Merabet, Yahia Chebouti, Nassima Behidj, Salahedine Doumandji

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Among the Anacardiaceae, the fruit (Pistacia vera L.) is the only species that produces edible fruits. The introduction of real pistachio was made in the early sixties by an FAO program in Algeria in several regions in the northern part of Algeria: Tlemcen, Sidi Bel Abbes, Batna, Bouira M'sila. Chemical analyzes of seeds pistachios were made on seeds from an orchard that localizes to Bechloul (Bouira) located in bioclimatic sub-humid temperate winter floor. Analyzes reveal dry matter content of 3.60±0.45%, the water rate is 7.21±0.36%. However, the fat content is 46.00±0.90%, in average blood sugar, it is 4.02±0.47%, the protein reached 29.88±0.76%. Given the very interesting that high-fat food nutritional values, culture pistachio must be considered for its extension in Algeria.

Keywords: pistachio, dry matter, fat, sugar, protein

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Authors: Kyriaki Kalaitzidou, Athanasia Tolkou, Christina Raptopoulou, Manassis Mitrakas, Anastasios Zouboulis

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Phosphate rock is the main source of phosphorous (P) in fertilizers and is essential for high crop yield in agriculture; currently, it is considered as a critical element, phasing scarcity. Chemical precipitation, which is a commonly used method of phosphorous removal from wastewaters, finds its significance in that phosphates may be precipitated in appropriate chemical forms that can be reused-recovered. Most often phosphorous is removed from wastewaters in the form of insoluble phosphate salts, by using salts (coagulants) of multivalent metal ions, most frequently iron, aluminum, calcium, or magnesium. The removal degree is affected by various factors, such as pH, chemical agent dose, temperature, etc. In this study, phosphate precipitation from the secondary (biologically treated) effluent of a municipal wastewater treatment plant is examined. Using chlorosulfate (FeClSO4) it was attempted to either remove and/or recover PO43-. Results showed that the use of Fe3+ can achieve residual concentrations lower than the commonly applied legislation limit of PO43- (i.e. 3 mg PO43-/L) by adding 7.5 mg/L Fe3+ in the secondary effluent with an initial concentration of about 10 mg PO43-/L and at pH range between 6 to 9. In addition, the formed sediment has a percentage of almost 24% PO43- content. Therefore, simultaneous removal and recovery of PO43- as ferric phosphate can be achieved, making it possible for the ferric phosphate to be re-used as a possible (secondary) fertilizer source.

Keywords: ferric phosphate, phosphorus recovery, phosphorus removal, wastewater treatment

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Authors: Fang Lian, Zefang Chenli, Laijun Ma, Lei Mao

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Up to now, electrolytic process is a popular way to prepare Mn and MnO2 (EMD) with high purity. However, the conventional preparation process of manganese oxide such as Mn3O4 with high purity from electrolytic manganese metal is characterized by long production-cycle, high-pollution discharge and high energy consumption especially initially from low-grade rhodochrosite, the main resources for exploitation and applications in China. Moreover, Mn3O4 prepared from electrolytic manganese shows large particles, single morphology beyond the control and weak chemical activity. On the other hand, hydrometallurgical method combined with thermal decomposition, hydrothermal synthesis and sol-gel processes has been widely studied because of its high efficiency, low consumption and low cost. But the key problem in direct preparation of manganese oxide series from low-grade rhodochrosite is to remove completely the multiple impurities such as iron, silicon, calcium and magnesium. It is urgent to develop a sustainable approach to high pure manganese oxide series with character of short process, high efficiency, environmentally friendly and economical benefit. In our work, the preparation technique of high pure Mn3O4 directly from low-grade rhodochrosite ore (13.86%) was studied and improved intensively, including the effective leaching process and the short purifying process. Based on the same ion effect, the repeated leaching of rhodochrosite with sulfuric acid is proposed to improve the solubility of Mn2+ and inhibit the dissolution of the impurities Ca2+ and Mg2+. Moreover, the repeated leaching process could make full use of sulfuric acid and lower the cost of the raw material. With the aid of theoretical calculation, Ba(OH)2 was chosen to adjust the pH value of manganese sulfate solution and BaF2 to remove Ca2+ and Mg2+ completely in the process of purifying. Herein, the recovery ratio of manganese and removal ratio of the impurity were evaluated via chemical titration and ICP analysis, respectively. Comparison between conventional preparation technique from electrolytic manganese and a sustainable approach directly from low-grade rhodochrosite have also been done herein. The results demonstrate that the extraction ratio and the recovery ratio of manganese reached 94.3% and 92.7%, respectively. The heavy metal impurities has been decreased to less than 1ppm, and the content of calcium, magnesium and sodium has been decreased to less than 20ppm, which meet standards of high pure reagent for energy and electronic materials. In compare with conventional technique from electrolytic manganese, the power consumption has been reduced to ≤2000 kWh/t(product) in our short-process approach. Moreover, comprehensive recovery rate of manganese increases significantly, and the wastewater generated from our short-process approach contains low content of ammonia/ nitrogen about 500 mg/t(product) and no toxic emissions. Our study contributes to the sustainable application of low-grade manganese ore. Acknowledgements: The authors are grateful to the National Science and Technology Support Program of China (No.2015BAB01B02) for financial support to the work.

Keywords: leaching, high purity, low-grade rhodochrosite, manganese oxide, purifying process, recovery ratio

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Authors: Om Kalthoum Sallem, Saidakilani, Kamiliya Ounaissa, Abdelmajid Abid

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Introduction and purposes: Olive oil is the main oil used in the Mediterranean diet. Virgin olive oil is valued for its organoleptic and nutritional characteristics and is resistant to oxidation due to its high monounsaturated fatty acid content (MUFAs), and low polyunsaturates (PUFAs) and the presence of natural antioxidants such as phenols, tocopherols and carotenoids. The fatty acid composition, especially the MUFA content, and the natural antioxidants provide advantages for health. The aim of the present study was to examine the impact of method of extraction on the chemical profiles of ‘Chemchali’ olive oil variety, which is cultivated in the city of Gafsa, and to compare it with chetoui and chemchali varieties. Methods: Our study is a qualitative prospective study that deals with ‘Chemchali’ olive oil variety. Analyses were conducted during three months (from December to February) in different oil mills in the city of Gafsa. We have compared ‘Chemchali’ olive oil obtained by continuous method to this obtained by superpress method. Then we have analyzed quality index parameters, including free fatty acid content (FFA), acidity, and UV spectrophotometric characteristics and other physico-chemical data [oxidative stability, ß-carotene, and chlorophyll pigment composition]. Results: Olive oil resulting from super press method compared with continuous method is less acid(0,6120 vs. 0,9760), less oxydazible(K232:2,478 vs. 2,592)(k270:0,216 vs. 0,228), more rich in oleic acid(61,61% vs. 66.99%), less rich in linoleic acid(13,38% vs. 13,98 %), more rich in total chlorophylls pigments (6,22 ppm vs. 3,18 ppm ) and ß-carotene (3,128 mg/kg vs. 1,73 mg/kg). ‘Chemchali’ olive oil showed more equilibrated total content in fatty acids compared with the varieties ’Chemleli’ and ‘Chetoui’. Gafsa’s variety ’Chemlali’ have significantly less saturated and polyunsaturated fatty acids. Whereas it has a higher content in monounsaturated fatty acid C18:2, compared with the two other varieties. Conclusion: The use of super press method had benefic effects on general chemical characteristics of ‘Chemchali’ olive oil, maintaining the highest quality according to the ecocert legal standards. In light of the results obtained in this study, a more detailed study is required to establish whether the differences in the chemical properties of oils are mainly due to agronomic and climate variables or, to the processing employed in oil mills.

Keywords: olive oil, extraction method, fatty acids, chemchali olive oil

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Authors: J. O. Yeboah, K Aboraa, K. Kodom

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The chemical and physical characteristics of rainwater harvested from a typical rooftop were progressively studied. The samples of rainwater collected were analyzed for pH, major ion concentrations, TDS, turbidity, conductivity. All the physicochemical constituents fell within the WHO guideline limits at some points as rainfall progresses except the pH. All the components of rainwater quality measured during the study showed higher concentrations during the early stages of rainfall and reduce as time progresses. There was a downward trend in terms of pH as rain progressed, with 18% of the samples recording pH below the WHO limit of 6.5-8.0. It was observed that iron concentration was above the WHO threshold value of 0.3 mg/l on occasions of heavy rains. The results revealed that most of physicochemical characteristics of rainwater samples were generally below the WHO threshold, as such, the rainwater characteristics showed satisfactory conditions in terms of physicochemical constituents.

Keywords: conductivity, pH, physicochemical, rainwater quality, TDS

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Authors: Hanen Filali, Mohamed Hachicha

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Treated grey water (TGW) reuse emerged as an alternative resource to meet the growing demand for water for agricultural irrigation and reduce the pressure on limited existing fresh water. However, this reuse needs adapted management in order to avoid environmental and health risks. In this work, the treatment of grey water (GW) was studied from a cyclic treatment system that we designed and implemented in the greenhouse of National Research Institute for Rural Engineering, Water and Forests (INRGREF). This system is composed of three levels for treatment (TGW 1, TGW 2, and TGW 3). Each level includes a sandy soil box. The use of grey water was moderated depending on the chemical and microbiological quality obtained. Different samples of soils and treated grey water were performed and analyzed for 14 irrigation cycles. TGW through cyclic treatment showed physicochemical parameters like pH, electrical conductivity (EC), chemical oxygen demand (COD), biological oxygen demand (BOD5) in the range of 7,35-7,91, 1,69-5,03 dS/m, 102,6-54,2 mgO2/l, and 31,33-15,74 mgO2/l, respectively. Results showed a reduction in the pollutant load with a significant effect on the three treatment levels; however, an increase in salinity was observed during all irrigation cycles. Microbiological results showed good grey water treatment with low health risk on irrigated soil. Treated water quality was below permissible Tunisian standards (NT106.03), and treated water is suitable for non-potable options.

Keywords: treated grey water, irrigation, cyclic treatment, soils, physico-chemical parameters, microbiological parameters

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Authors: Hafizan Junoh, Kumaran Palanisamy, Yip Chan Heng, Pua Fei Ling

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This study investigates the influence of low temperature thermo-chemical pretreatment of organic food waste on the performance of COD solubilisation. Both temperature and alkaline agent were reported to have an effect on solubilizing any possible biomass including organic food waste. The three independent variables considered in this pretreatment were temperature (50-90oC), pretreatment time (30-120 minutes) and alkaline concentration, sodium hydroxide, NaOH (0.7-15 g/L). The optimal condition obtained were 90oC, 15 g/L NaOH for 2 hours. Solubilisation has potential in enhancing methane production by providing a high amount of soluble components at an early stage during anaerobic digestion.

Keywords: food waste, pretreatments, respond surface methodology, ANOVA, anaerobic digestion

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Authors: Stephen Daniel Iduh, Evans Chidi Egwin, Oluwatosin Kudirat Shittu

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The process for the development of reliable and eco-friendly metallic Nanoparticles is an important step in the field of Nanotechnology for biomedical application. To achieve this, use of natural sources like biological systems becomes essential. In the present work, extracellular biosynthesis of gold Nanoparticles using aqueous leave and stembark extracts of K. senegalensis has been attempted. The gold Nanoparticles produced were characterized using High Resolution scanning electron microscopy, Ultra Violet–Visible spectroscopy, zeta-sizer Nano, Energy-Dispersive X-ray (EDAX) Spectroscopy and Fourier Transmission Infrared (FTIR) Spectroscopy. The cytotoxicity of the synthesized gold nanoparticles on MCF-7 cell line was evaluated using MTT assay. The result showed a rapid development of Nano size and shaped particles within 5 minutes of reaction with Surface Plasmon Resonance at 520 and 525nm respectively. An average particle size of 20-90nm was confirmed. The amount of the extracts determines the core size of the AuNPs. The core size of the AuNPs decreases as the amount of extract increases and it causes the shift of Surface Plasmon Resonance band. The FTIR confirms the presence of biomolecules serving as reducing and capping agents on the synthesised gold nanoparticles. The MTT assay shows a significant effect of gold nanoparticles which is concentration dependent. This environment-friendly method of biological gold Nanoparticle synthesis has the potential and can be directly applied in cancer therapy.

Keywords: biosynthesis, gold nanoparticles, characterization, calotropis procera, cytotoxicity

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Authors: L. Amjad, M. Torki, F. Yazdani

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The genus Achillea belongs to Asteraceae family. This plant is widely found in different regions of Iran and used for treatment of different diseases. The aim of this study was to evaluate the chemical composition of Achillea wilhelmsii in Iran. The aerial parts of A. wilhelmsii collected from Shahrekord and Mazandaran Province, Iran and they were analyzed by using GC/MS. The 23, 13 compounds were identified in dried aerial parts of A. wilhelmsii from Shahrekord and Mazandaran, respectively. The major components in Shahrekord were: 1,8-Cineole (35.532%), α-pinene (22.885%), Camphor (12.238%), Camphene (8.691%), Piperitol (3.748%), Ethanone (2.274%) and The major components in Mazandaran were: 1,8-Cineole (52.951%), α-pinene (13.985%), Camphor (11.824%), Camphene (8.531%), Terpineol (2.533%), α-Thujone (2.330%). According to the results, difference in essential oil components of Achillea species in different regions may be due to the several factors that leads to change in compositions of plant.

Keywords: achillea wilhelmsii, essential oils, GC/MS

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Authors: Hina Verma, Karine Le Guen, Renaud Dalaunay, Iyas Ismail, Vita Ilakovac, Jean Pascal Rueff, Yunlin Jacques Zheng, Philippe Jonnard

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To the extent of our knowledge, X-ray emission spectroscopy (XES) has been applied in the soft x-ray region (photon energy ≤ 2 keV) to study the buried layers and interfaces of stacks of nanometer-thin films. Now we extend the methodology to study the buried interfaces in the hard X-ray region (i.e., ≥ five keV). The emission spectra allow us to study the interactions between elements in the buried layers from the analysis of their valence states, thereby providing sensitive information about the physical-chemical environment of the emitting element in multilayers. We exploit the chemical sensitivity of XES to study the interfaces between Fe and Si layers in the Fe/Si multilayer from the Fe Kβ₂,₅ emission spectra (7108 eV). The Fe Kβ₅ emission line results from the electronic transition from occupied 3d to 1s levels (i.e., valence to core transition) and is hence sensitive to the chemical state of emitting Fe atoms. The comparison of emission spectra recorded for Fe/Si multilayer with Fe and FeSi₂ references reveal the formation of FeSi₂ at the Fe-Si interfaces inside the multilayer stack. The interfacial thickness was calculated to be 1.4 ± 0.2 nm by taking into consideration the intensity of Fe atoms emitted from the interface and the Fe layer. The formation of FeSi₂ at the interface was further confirmed by the X-ray diffraction and X-ray photoelectron spectroscopy done on the Fe/Si multilayer. Hence, we can conclude that the XES in the hard X-ray range could be used to study multilayers and their interfaces and obtain information both qualitatively and quantitatively.

Keywords: buried interfaces, hard X-ray emission spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy

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Authors: Norah Al Hokbany, Ibrahim Al Jammaz, Basem Al Otaibi, Yousif Al Malki, Subhani M. Okarvi

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Objective: The folate receptor is over-expressed in a wide variety of human tumors. Conjugates of folate have been shown to be selectively taken up by tumor cells via the folate receptor. In an attempt to develop new folate radiotracers with favorable biochemical properties for detecting folate receptor-positive cancers. Methods: we synthesized ⁶⁴Cu-NOTA- and ⁶⁴Cu-NOTAM-folate conjugates using a straightforward and simple one-step reaction. Radiochemical yields were greater than 95% (decay-corrected) with a total synthesis time of less than 20 min. Results: Radiochemical purities were always greater than 98% without high-performance liquid chromatography (HPLC) purification. These synthetic approaches hold considerable promise as a rapid and simple method for ⁶⁴Cu-folate conjugate preparation with high radiochemical yield in a short synthesis time. In vitro tests on the KB cell line showed that significant amounts of the radio conjugates were associated with cell fractions. Bio-distribution studies in nude mice bearing human KB xenografts demonstrated a significant tumor uptake and favorable bio-distribution profile for ⁶⁴Cu-NOTA- and ⁶⁴Cu-NOTAM-folate conjugate. The uptake in the tumors was blocked by the excess injection of folic acid, suggesting a receptor-mediated process. Conclusion: These results demonstrate that the ⁶⁴Cu-NOTAM-folate conjugate may be useful as a molecular probe for the detection and staging of folate receptor-positive cancers, such as ovarian cancer and their metastasis, as well as monitoring tumor response to treatment.

Keywords: folate, receptor, tumor imaging, ⁶⁴Cu-NOTA-folate, PET

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Authors: D. Geringswald, B. Hintze

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The miniaturization of circuits is advancing. During chip manufacturing, structures are filled for example by metal organic chemical vapor deposition (MOCVD). Since this process reaches its limits in case of very high aspect ratios, the use of alternatives such as the atomic layer deposition (ALD) is possible, requiring the extension of existing coating systems. However, it is an unsolved question to what extent MOCVD can achieve results similar as an ALD process. In this context, this work addresses the characterization of a metal organic vapor deposition of titanium nitride. Based on the current state of the art, the film properties coating thickness, sheet resistance, resistivity, stress and chemical composition are considered. The used setting parameters are temperature, plasma gas ratio, plasma power, plasma treatment time, deposition time, deposition pressure, number of cycles and TDMAT flow. The derived process instructions for unstructured wafers and inside a structure with high aspect ratio include lowering the process temperature and increasing the number of cycles, the deposition and the plasma treatment time as well as the plasma gas ratio of hydrogen to nitrogen (H₂:N₂). In contrast to the current process configuration, the deposited titanium nitride (TiN) layer is more uniform inside the entire test structure. Consequently, this paper provides approaches to employ the MOCVD for structures with increasing aspect ratios.

Keywords: ALD, high aspect ratio, PE-MOCVD, TiN

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Authors: Renata L. C. Leão, João E. Nascimento, Natalia C. E. S. Nascimento, Elaine S. Vasconcelos, Mércia L. Oliveira

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The quality control procedures of a radiopharmaceutical include the assessment of its chemical purity. The method suggested by international pharmacopeias consists of a thin layer chromatographic run. In this paper, the method proposed by the United States Pharmacopeia (USP) is compared to a direct method to determine the final concentration of aminopolyether in Fludeoxyglucose (¹⁸F-FDG) preparations. The approach (no chromatographic run) was achieved by placing the thin-layer chromatography (TLC) plate directly on an iodine vapor chamber. Both methods were validated and they showed adequate results to determine the concentration of aminopolyether in ¹⁸F-FDG preparations. However, the direct method is more sensitive, faster and simpler when compared to the reference method (with chromatographic run), and it may be chosen for use in routine quality control of ¹⁸F-FDG.

Keywords: chemical purity, Kryptofix 222, thin layer chromatography, validation

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Authors: Adrien Cornille, Sylvain Caillol, Bernard Boutevon

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The development of polyurethanes began in 1937 at I. G. Farbenindustrie where Bayer with coworkers discovered the addition polymerization reaction between diisocyanates and diols. Since their discovery, the demand in PU has continued to increase and it will attain in 2016 a production of 18 million tons. However, isocyanates compounds are harmful to human and environment. Methylene diphenyl 4,4’-diisocyanate (MDI) and toluene diisocyanate (TDI), the most widely used isocyanates in PU industry, are classified as CMR (Carcinogen, Mutagen, and Reprotoxic). In order to design isocyanate-free materials, an interesting alternative is the use of Polyhydroxyurethanes (PHUs) by reaction between cyclic carbonate and polyfunctional amines. The main problem concerning PHUs synthesis relates to the low reactivity of carbonate/amine reaction. To solve this issue, many studies in the literature have been conducted to design PHU from more reactive cyclic-carbonates, bearing electro-withdrawing substituent or by using six-membered, seven-membered or thio-cyclic carbonate. The main drawback of all these systems remains the low molar masses obtained for the synthesized PHUs, which hinders their use for material applications. Therefore, we developed another strategy to afford new hybrid PHU with high conversion. This very innovative two-step approach consists in the first step in the synthesis of aminotelechelic PHU oligomers with different chain length from bis-cyclic carbonate with different excess of primary amine functions. In the second step, these aminotelechelic PHU oligomers were used in formulation with biobased epoxy monomers (from cashew nut shell liquid and tannins) to synthesize hybrid polyepoxyurethane polymers. These materials were then characterized by thermal and mechanical analyses.

Keywords: polyurethane, polyhydroxyurethane, aminotelechelic NIPU oligomers, carbonates, epoxy, amine, epoxyurethane polymers, hybrid polymers

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Authors: Meera A. Albloushi, Adel B. Gougam

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The development in the field of piezoelectrics has led to a renewed interest in ZnO nanowires (NWs) as a promising material in the nanogenerator devices category. It can be used as a power source for self-powered electronic systems with higher density, higher efficiency, longer lifetime, as well as lower cost of fabrication. Highly aligned ZnO nanowires seem to exhibit a higher performance compared with nonaligned ones. The purpose of this study was to develop ZnO nanowires and to investigate their electrical and chemical properties for various applications. They were grown on silicon (100) and glass substrates. We have used a low temperature and non-hazardous method: aqueous chemical growth (ACG). ZnO (non-doped) and AZO (Aluminum doped) seed layers were deposited using RF magnetron sputteringunder Argon pressure of 3 mTorr and deposition power of 180 W, the times of growth were selected to obtain thicknesses in the range of 30 to 125 nm. Some of the films were subsequently annealed. The substrates were immersed tilted in an equimolar solution composed of zinc nitrate and hexamine (HMTA) of 0.02 M and 0.05 M in the temperature range of 80 to 90 ᵒC for 1.5 to 2 hours. The X-ray diffractometer shows strong peaks at 2Ө = 34.2ᵒ of ZnO films which indicates that the films have a preferred c-axis wurtzite hexagonal (002) orientation. The surface morphology of the films is investigated by atomic force microscope (AFM) which proved the uniformity of the film since the roughness is within 5 nm range. The scanning electron microscopes(SEM) (Quanta FEG 250, Quanta 3D FEG, Nova NanoSEM 650) are used to characterize both ZnO film and NWs. SEM images show forest of ZnO NWs grown vertically and have a range of length up to 2000 nm and diameter of 20-300 nm. The SEM images prove that the role of the seed layer is to enhance the vertical alignment of ZnO NWs at the pH solution of 5-6. Also electrical and optical properties of the NWs are carried out using Electrical Force Microscopy (EFM). After growing the ZnO NWs, developing the nano-generator is the second step of this study in order to determine the energy conversion efficiency and the power output.

Keywords: ZnO nanowires(NWs), aqueous chemical growth (ACG), piezoelectric NWs, harvesting enery

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Authors: Teimuraz Manjapharashvili, Ketevani Manjaparashvili

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Fuzzy logic is a modeling method for complex or ill-defined systems and is a relatively new mathematical approach. Its basis is to consider overlapping cases of parameter values and define operations to manipulate these cases. Fuzzy logic can successfully create operative automatic management or appropriate advisory systems. Fuzzy logic techniques in various operational control technologies have grown rapidly in the last few years. Fuzzy logic is used in many areas of human technological activity. In recent years, fuzzy logic has proven its great potential, especially in the automation of industrial process control, where it allows to form of a control design based on the experience of experts and the results of experiments. The engineering of chemical technological processes uses fuzzy logic in optimal management, and it is also used in process control, including the operational control of continuous cycle chemical industrial, technological processes, where special features appear due to the continuous cycle and correct management acquires special importance. This paper discusses how intelligent systems can be developed, in particular, how fuzzy logic can be used to build knowledge-based expert systems in chemical process engineering. The implemented projects reveal that the use of fuzzy logic in technological process control has already given us better solutions than standard control techniques. Fuzzy logic makes it possible to develop an advisory system for decision-making based on the historical experience of the managing operator and experienced experts. The present paper deals with operational control and management systems of continuous cycle chemical technological processes, including advisory systems. Because of the continuous cycle, many features are introduced in them compared to the operational control of other chemical technological processes. Among them, there is a greater risk of transitioning to emergency mode; the return from emergency mode to normal mode must be done very quickly due to the impossibility of stopping the technological process due to the release of defective products during this period (i.e., receiving a loss), accordingly, due to the need for high qualification of the operator managing the process, etc. For these reasons, operational control systems of continuous cycle chemical technological processes have been specifically discussed, as they are different systems. Special features of such systems in control and management were brought out, which determine the characteristics of the construction of control and management systems. To verify the findings, the development of an advisory decision-making information system for operational control of a lime kiln using fuzzy logic, based on the creation of a relevant expert-targeted knowledge base, was discussed. The control system has been implemented in a real lime production plant with a lime burn kiln, which has shown that suitable and intelligent automation improves operational management, reduces the risks of releasing defective products, and, therefore, reduces costs. The special advisory system was successfully used in the said plant both for the improvement of operational management and, if necessary, for the training of new operators due to the lack of an appropriate training institution.

Keywords: chemical process control systems, continuous cycle industrial technological processes, fuzzy logic, lime kiln

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Authors: Mireille Vonlanthen, Pasquale Porcu, Ernesto Rivera

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Dendritic macromolecules are presenting unique physical and chemical properties. One of them is the faculty of transferring energy from a donor moiety introduced at the periphery to an acceptor moiety at the core, mimicking the antenna effect of the process of photosynthesis. The mechanism of energy transfer is based on the Förster resonance energy exchange and requires some overlap between the emission spectrum of the donor and the absorption spectrum of the acceptor. Since it requires a coupling of transition dipole but no overlap of the physical wavefunctions, the energy transfer by Förster mechanism can occur over quite long distances from 1 to a maximum of 10 nm. However, the efficiency of the transfer depends strongly on distance. The Förster radius is the distance at which 50% of the donor’s emission is deactivated by FRET. In this work, we synthesized and characterized a novel series of dendrimers bearing pyrene moieties at the periphery and a Ru (II) complex at the core. The optical and photophysical properties of these compounds were studied by absorption and fluorescence spectroscopy. Pyrene is a well-studied chromophore that has the particularity to present monomer as well as excimer fluorescence emission. The coordination compounds of Ru (II) are red emitters with low quantum yield and long excited lifetime. We observed an efficient singulet to singulet energy transfer in such constructs. Moreover, it is known that the energy of the MLCT emitting state of Ru (II) can be tuned to become almost isoenegetic with respect to the triplet state of pyrene, leading to an extended phosphorescence lifetime. Using dendrimers bearing pyrene moieties as ligands for Ru (II), we could combine the antenna effect of dendrimers as well as its protection effect to the quenching by dioxygen with lifetime increase due to triplet-triplet equilibrium.

Keywords: dendritic molecules, energy transfer, pyrene, ru-trisbipyridine complex

Procedia PDF Downloads 276

Authors: Rewadee Anuwattana, Pattamaphorn Phuangngamphan, Narumon Soparatana, Supinya Sutthima, Worapong Pattayawan, Saroj Klangkongsub, Songkiat Roddang, Pluek Wongpanich

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The leachate wastewater is high contaminant water; hence it needs to be treated. The objective of this research was to determine the Chemical Oxygen Demand (COD) concentration, Phosphate (PO₄³⁻), Ammonia (NH₃) and color in leachate wastewater in the landfill area. The experiments were carried out in the optimum condition by pH, the Fenton reagent dosage (concentration of dosing Fe²⁺ and H₂O₂). The optimum pH is 3, the optimum [Fe²⁺]/[COD] and [H₂O₂]/[COD₀] = 0.03 and 0.03, respectively. The Biochemical Oxygen Demand (BOD₅)/Chemical Oxygen Demand (COD) ratio can be adjusted to 1 for landfill leachate wastewater (BOD₅/COD = 0.11). From the results, the Fenton process shall be investigated further to achieve the removal of phosphates in addition to COD and color.

Keywords: landfill leachate treatment, open dumpsite, Fenton process, wastewater treatment

Procedia PDF Downloads 261

Authors: Muhammad R. Islam, Mohammad Dalour H. Beg, Saidatul S. Jamari

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Considering palm oil as non-drying oil owing to its low iodine value, an attempt was taken to increase the unsaturation in the fatty acid chains of palm oil for the preparation of alkyds. To increase the unsaturation in the palm oil, sulphuric acid (SA) and para-toluene sulphonic acid (PTSA) was used prior to alcoholysis for the dehydration process. The iodine number of the oil samples was checked for the unsaturation measurement by Wijs method. Alkyd resin was prepared using the dehydrated palm oil by following alcoholysis and esterification reaction. To improve the film properties 0.5 wt% multi-wall carbon nano tubes (MWCNTs) were used to manufacture polymeric film. The properties of the resins were characterized by various physico-chemical properties such as density, viscosity, iodine value, acid value, saponification value, etc. Structural elucidation was confirmed by Fourier transform of infrared spectroscopy and proton nuclear magnetic resonance; surfaces of the cured films were observed by scanning electron microscopy. In addition, pencil hardness and chemical resistivity was also measured by using standard methods. The effect of enhancement of the unsaturation in the fatty acid chain found significant and motivational. The resin prepared with dehydrated palm oil showed improved properties regarding hardness and chemical resistivity testing. The incorporation of MWCNTs enhanced the thermal stability and hardness of the films as well.

Keywords: alkyd resin, nano-coatings, dehydration, palm oil

Procedia PDF Downloads 309

Authors: Thandeka Y. S. Jwara, Paul Musonge

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Traditionally, the complexity associated with implementing and controlling biological nutrient removal (BNR) in wastewater works (WWW) has been primarily in terms of balancing competing requirements for nitrogen and phosphorus removal, particularly with respect to the use of influent chemical oxygen demand (COD) as a carbon source for the microorganisms. Successful BNR optimization and modelling using WEST (Worldwide Engine for Simulation and Training) depend largely on the accurate fractionation of the influent COD. The different COD fractions have differing effects on the BNR process, and therefore, the influent characteristics need to be well understood. This study presents the fractionation results of primary wastewater effluent COD at one of South Africa’s wastewater works treating 65ML/day of mixed industrial and domestic effluent. The method used for COD fractionation was the oxygen uptake rate/respirometry method. The breakdown of the results of the analysis is as follows: 70.5% biodegradable COD (bCOD) and 29.5% of non-biodegradable COD (iCOD) in terms of the total COD. Further fractionation led to a readily biodegradable soluble fraction (SS) of 75%, a slowly degradable particulate fraction (XS) of 24%, a particulate non-biodegradable fraction (XI) of 50.8% and a non-biodegradable soluble fraction (SI) of 49.2%. The fractionation results demonstrate that the primary effluent has good COD characteristics, as shown by the high level of the bCOD fraction with Ss being higher than Xs. This means that the microorganisms have sufficient substrate for the BNR process and that these components can now serve as inputs to the WEST Model for the plant under study.

Keywords: chemical oxygen demand, COD fractionation, wastewater modelling, wastewater optimization

Procedia PDF Downloads 142

Authors: Azad Khalid, Sifa Dogan

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Because of its persistence in conventional treatment plants and broad prevalence in water bodies, the pharmaceutical chemical carbamazepine (CBZ) has been suggested as an anthropogenic marker to evaluate water quality. This study provides a thorough examination of the origins and occurrences of CBZ in water bodies, as well as the drug's toxicological effects and laws. Given CBZ's well-documented negative consequences on the human body when used medicinally, cautious monitoring in water is advised. CBZ residues in drinking water may enter embryos and newborns via intrauterine exposure or breast-feeding, causing congenital abnormalities and/or neurodevelopmental issues over time. The insufficiency of solo solutions was shown after an in-depth technical study of traditional and sophisticated treatment technologies. Nanofiltration and reverse osmosis membranes are more successful at removing CBZ than traditional activated sludge and membrane bioreactor techniques. Recent research has shown that severe chemical cleaning, which is essential to prevent membrane fouling, may lower long-term removal efficiency. Furthermore, despite the efficacy of activated carbon adsorption and advanced oxidation processes, a few issues such as chemical cost and activated carbon renewal must be carefully examined. Individual technology constraints lead to the benefits of combined and hybrid systems, namely the heterogeneous advanced oxidation process.

Keywords: carbamazepine, occurrence, toxicity, conventical treatment, advanced oxidation process (AOPs)

Procedia PDF Downloads 95

Authors: Motahar Reza, Rajni Chahal, Neha Sharma

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This article addresses the boundary layer flow and heat transfer of Casson fluid over a nonlinearly permeable stretching surface with chemical reaction in the presence of variable magnetic field. The effect of thermal radiation is considered to control the rate of heat transfer at the surface. Using similarity transformations, the governing partial differential equations of this problem are reduced into a set of non-linear ordinary differential equations which are solved by finite difference method. It is observed that the velocity at fixed point decreases with increasing the nonlinear stretching parameter but the temperature increases with nonlinear stretching parameter.

Keywords: boundary layer flow, nonlinear stretching, Casson fluid, heat transfer, radiation

Procedia PDF Downloads 398

Authors: Ouahiba Bechiri, Mostefa Abbessi

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In recent year, polyoxometallates are intensely being explored because of their applications as new materiels, structural aesthetics, catalysts, and biologically active compounds. heteropolyanions of general formulae [X2M18O62] n- (X= heteroatom, e.g. P, Si) and (M=W, Mo), known as Dawson-type anions, constitue a special class of polyoxometallate compounds. In this present work, cobalt substituted heteropolyanion Dawson-type [HP2W15Mo3CoO61] were synthesized and characterized by IR spectroscopy, 31 P NMR, cyclic voltammetry.

Keywords: heteropolyanions, nanomaterials, Dawson-type, characterization

Procedia PDF Downloads 248

Authors: Shahla Hajializadeh, Maryam Hamedanlou

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Multiwall carbon nanotubes were chemically modified with amide groups for the purpose of enhancing their chemical affinity with waterborne polyurethane. In this study, a thermoplastic nanocomposite containing functionalized multiwall carbon nanotube/waterborne polyurethane (WBPU/MWNT) via in situ polymerization has been prepared. The impacts of MWNT addition on the morphology and electrical properties of nanocomposites were investigated. Micrographs of Scanning Electron Microscopy (SEM) prove that functionalized CNT can be effectively dispersed in WBPU matrix. The electrical conductivity of nanocomposites increased with the CNT contents in as such the nanocomposites containing 1 wt% of MWNT exhibited a conductivity nearly five orders of magnitude higher than the WBPU film.

Keywords: chemical functionalization, electrical properties, in situ polymerization, morphology, multiwall carbon nanotubes, waterborne polyurethane

Procedia PDF Downloads 263

Authors: S. N. Turkmen Koc, A. S. Kipcak, M. B. Piskin, E. Moroydor Derun, N. Tugrul

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Active carbon can be obtained from agricultural sources. Due to the high surface area, the production of activated carbon from cheap resources is very important. Since the surface area of 1 g activated carbon is approximately between 300 and 2000 m², it can be used to remove both organic and inorganic impurities. In this study, the adsorption of Zn metal was studied with the product of activated carbon, which is obtained from pomegranate peel by microwave and chemical activation methods. The microwave process of pomegranate peel was carried out under constant microwave power of 800 W and 1 to 4 minutes. After the microwave process, samples were treated with H₂SO₄ for 3 h. Then prepared product was used in synthetic waste water including 40 ppm Zn metal. As a result, removal of waste Zn in waste water ranged from 91% to 93%.

Keywords: activated carbon, chemical activation, H₂SO₄, microwave, pomegranate peel

Procedia PDF Downloads 166

Authors: Kiran Abdullah, Yanli Chen

Abstract:

An amphiphilic mixed (phthalocyaninato) (porphyrinato) europium triple-decker complex Eu₂(Pc)₂(TPyP) has been synthesized and characterized. Introducing electron-withdrawing pyridyl substituents onto the meso-position of porphyrin ring in the triple-decker to ensure the sufficient hydrophilicity and suitable HOMO and LUMO energy levels and thus successfully realize amphiphilic ambipolar organic semiconductor. Importantly, high sensitive, reproducible p-type and n-type responses towards NH₃ andNO₂ respectively, based on the self-assembled film of the Eu₂(Pc)₂(TPyP) fabricated by a simple solution-based Quasi–Langmuir–Shäfer (QLS) method, have been first revealed. The good conductivity and crystallinity for the QLS film of Eu₂(Pc)₂(TPyP) render it excellent sensing property. This complex is sensitive to both electron-donating NH₃ gas in 5–30 ppm range and electron-accepting NO₂ gas 400–900 ppb range. Due to uniform nano particles there exist effective intermolecular interaction between triple decker molecules. This is the best result of Phthalocyanine–based chemical sensors at room temperature. Furthermore, the responses of the QLS film are all linearly correlated to both NH₃ and NO₂ with excellent sensitivity of 0.04% ppm⁻¹ and 31.9 % ppm⁻¹, respectively, indicating the great potential of semiconducting tetrapyrrole rare earth triple-decker compounds in the field of chemical sensors.

Keywords: ambipolar semiconductor, gas sensing, mixed (phthalocyaninato) (porphyrinato) rare earth complex, Self-assemblies

Procedia PDF Downloads 197

Authors: Dharmana Pradeep, Chandan Kumar Patnaikuni, N. V. S. Venugopal

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Rice Husk Ash (RHA) is a green product contains carbon and also loaded with silica. For the development of durability and strength of any concrete, curing phenomenon shall be very important. In this communication, we reported the exposure of partial replacement of cement with RHA at different percentages of 0%, 5%, 7.5%, 10%, 12.5% and 15% by weight under sodium phosphate curing atmosphere. The mix is designed for M40 grade concrete with the proportions of 1:2.2:3.72. The tests conducted on concrete was a compressive strength, and the specimens were cured in normal water & exposed to the chemical solution for 7, 28 & 56 days. For chemical curing 0.5% & 1% concentrated sodium phosphates were used and were compared with normal concrete strength results. The strength of specimens of 1% sodium phosphate exposure showed that the compressive strength decreased with increase in RHA percentages.

Keywords: rice husk ash, compressive strength, sodium phosphate, curing

Procedia PDF Downloads 343