Search results for: spectrometer

Authors: Giovanni Meloni

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Recent results are presented from experiments carried out at the Advanced Light Source (ALS) at the Chemical Dynamics Beamline of Lawrence Berkeley National Laboratory using multiplexed synchrotron photoionization mass spectrometry. The reaction mixture and a buffer gas (He) are introduced through individually calibrated mass flow controllers into a quartz slow flow reactor held at constant pressure and temperature. The gaseous mixture effuses through a 650 μm pinhole into a 1.5 mm skimmer, forming a molecular beam that enters a differentially pumped ionizing chamber. The molecular beam is orthogonally intersected by a tunable synchrotron radiation produced by the ALS in the 8-11 eV energy range. Resultant ions are accelerated, collimated, and focused into an orthogonal time-of-flight mass spectrometer. Reaction species are identified by their mass-to-charge ratios and photoionization (PI) spectra. Comparison of experimental PI spectra with literature and/or simulated curves is routinely done to assure the identity of a given species. With the aid of electronic structure calculations, potential energy surface scans are performed, and Franck-Condon spectral simulations are obtained. Examples of these experiments are discussed, ranging from new intermediates characterization to reaction mechanisms elucidation and biofuels oxidation pathways identification.

Keywords: mass spectrometry, reaction intermediates, synchrotron photoionization, oxidation reactions

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Authors: Rongzhou Wang

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Research on designing nano-antibacterial agent with potent and long-lasting antibacterial property is demanding and provoking work. In this study, a core-shell AgBr/cationic polymer nanocomposite (AgBr/NPVP-H10) were synthesized and its structure confirmed by Fourier Transform Infrared Spectrometer (FT-IR), Nuclear Magnetic Resonance (1H NMR) and X-ray diffraction (XRD), and the cationic polymer contents were determined with Thermal Gravimetric Analyzer (TGA). The morphology was directly observed by Transmission Electron Microscope (TEM) which showed that the nanoparticle contains single core and organic shell and had an average diameter of 30.1 nm. The antibacterial test against Gram-positive Staphylococcus aureus and Gram-negative Escherichia coli illuminated that this nanocomposite had potent bactericidal activity, which can be attributed to the contact-killing of cationic polymers and releasing-killing of Ag+ ions. In addition, cationic polymer encapsulating AgBr cores gave the resin discs sustained release of Ag+ ions, which may result in long-lasting bactericidal activity. The AgBr/NPVP-H10 nanoparticle with the dual bactericidal capability and long term antimicrobial effect is a promising material aimed at preventing bacterial infection.

Keywords: core-shell nanocomposite, cationic polymer, dual antibacterial capability, long-lasting antibacterial activity

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Authors: Rehan Siddiqui, Brendan Quine

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The Radiance Enhancement (RE) and integrated absorption technique is applied to develop a synthetic model to determine the enhancement in radiance due to cloud scene and Shortwave upwelling Radiances (SHupR) by O2, H2O, CO2 and CH4. This new model is used to estimate the magnitude variation for RE and SHupR over spectral range of 900 nm to 1700 nm by varying surface altitude, mixing ratios and surface reflectivity. In this work, we employ satellite real observation of space orbiting Argus 1000 especially for O2, H2O, CO2 and CH4 together with synthetic model by using line by line GENSPECT radiative transfer model. All the radiative transfer simulations have been performed by varying over a different range of percentages of water vapor contents and carbon dioxide with the fixed concentration oxygen and methane. We calculate and compare both the synthetic and real measured observed data set of different week per pass of Argus flight. Results are found to be comparable for both approaches, after allowing for the differences with the real and synthetic technique. The methodology based on RE and SHupR of the space spectral data can be promising for the instant and reliable classification of the cloud scenes.

Keywords: radiance enhancement, radiative transfer, shortwave upwelling radiative flux, cloud reflectivity, greenhouse gases

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Authors: M. P. Raju, P. D. Safai, P. S. P. Rao, P. C. S. Devara, C. V. Naidu

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In order to study the Physical and chemical characteristics of aerosols, samples of Total Suspended Particulates (TSP) were collected using a high volume sampler at Pune, a semi-urban location in SW India during March 2009 to February 2010. TSP samples were analyzed for water soluble components like F, Cl, NO3, SO4, NH4, Na, K, Ca, and Mg and acid soluble components like Al, Zn, Fe and Cu using Ion-Chromatograph and Atomic Absorption Spectrometer. Analysis of the data revealed that the monthly mean TSP concentrations varied between 471.3 µg/m3 and 30.5 µg/m3 with an annual mean value of 159.8 µg/m3. TSP concentrations were found to be less during post-monsoon and winter (October through February), compared to those in summer and monsoon (March through September). Anthropogenic activities like vehicular emissions and dust particles originated from urban activities were the major sources for TSP. TSP showed good correlation with all the major ionic components, especially with SO4 (R= 0.62) and NO3 (R= 0.67) indicating the impact of anthropogenic sources over the aerosols at Pune. However, the overall aerosol nature was alkaline (Ave pH = 6.17) mainly due to the neutralizing effects of Ca and NH4. SO4 contributed more (58.8%) to the total acidity as compared to NO3 (41.1%) where as, Ca contributed more (66.5%) to the total alkalinity than NH4 (33.5%). Seasonality of acid soluble component Al, Fe and Cu showed remarkable increase, indicating the dominance of soil source over the man-made activities. Overall study on TSP indicated that aerosols at Pune were mainly affected by the local sources.

Keywords: chemical composition, acidic and neutralization potential, radiative forcing, urban station

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Authors: Temesgen Geremew

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ZnS/glass and CdS/glass single layers and ZnS/CdS and CdS/ZnS heterojunction thin films were deposited by the chemical bath deposition method using zinc acetate and cadmium acetate as the metal ion sources and thioacetamide as a nonmetallic ion source in acidic medium. Na2EDTA was used as a complexing agent to control the free cation concentration. +e single layer and heterojunction thin films were characterized with X-ray diffraction (XRD), a scanning electron microscope (SEM), energy dispersive X-ray (EDX), and a UV-VIS spectrometer. +e XRD patterns of the CdS/glass thin film deposited on the soda lime glass substrate crystalized in the cubic structure with a single peak along the (111) plane. +e ZnS/CdS heterojunction and ZnS/glass single layer thin films were crystalized in the hexagonal ZnS structure. +e CdS/ZnS heterojunction thin film is nearly amorphous.The optical analysis results confirmed single band gap values of 2.75 eV and 2.5 eV for ZnS/CdS and CdS/ZnS heterojunction thin films, respectively. +e CdS/glass and CdS/ZnS thin films have more imaginary dielectric components than the real part. The optical conductivity of the single layer and heterojunction films is in the order of 1015 1/s. +e optical study also confirmed refractive index values between 2 and 2.7 for ZnS/glass, ZnS/CdS, and CdS/ZnS thin films for incident photon energies between 1.2 eV and 3.8 eV. +e surface morphology studies revealed compacted spherical grains covering the substrate surfaces with few cracks on ZnS/glass, ZnS/CdS, and CdS/glass and voids on CdS/ZnS thin films. +e EDX result confirmed nearly 1 :1 metallic to nonmetallic ion ratio in the single-layered thin films and the dominance of Zn ion over Cd ion in both ZnS/CdS and CdS/ZnS heterojunction thin films.

Keywords: SERS, sensor, Hg2+, water detection, polythiophene

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Authors: Eunmi Koh, Bogyoung Choi, Dayeon Ryu, Jee-Yeon Lee, Sungok Kwon, Cho-Il Kim

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Ethyl carbamate(EC) is a probable human carcinogen (Group 2A) found in alcoholic beverages and fermented foods. A total of 351 samples including fermented foods and alcoholic beverages were chosen from 734 foods appeared in the pooled intake data of 2008, 2009, 2010, and 2011 Korea National Health & Nutrition Examination Survey (KNHANES). Sampling was carried out from September 2013 to July 2016 in 18 supermarkets of 9 metropolitan cities in Korea. The samples were pooled, prepared according to various cooking methods, and analyzed. A total of 1245 samples were analyzed using gas chromatograph-mass spectrometer. EC was detected in 13 items (1.0%), which ranged from not-detected to 151 g/kg. Alcoholic beverages (maesilju, whisky, and bokbunjaju) and fermented soy products (soy sauce and soybean paste) were the food items with relatively higher EC levels. Dietary intake of EC in the Korean population was estimated to be 2.11 ng/kg body weight (bw) per day for average population and 8.42 ng/kg bw per day for high consumers (the 97.5th percentile). When the estimated average dietary exposure to EC was compared with the Benchmark Dose Lower Confidence Limit 10% (BMDL10) of 0.3 mg/kg bw per day, margin of exposure (MOE) values of 1420000 to 28000000 were observed. This indicates that there is no health concern for the Korean population.

Keywords: ethyl carbamate, total diet study, dietary exposure, margin of exposure

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Authors: Joshua N. Edokpayi, John O. Odiyo, Patience P. Shikwambana

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Water is a very rare natural resource in South Africa. Ga-Selati River is used for both domestic and industrial purposes. This study was carried out in order to assess the quality of Ga-Selati River in a mining area of Limpopo Province-Phalaborwa. The pH, Electrical Conductivity (EC) and Total Dissolved Solids (TDS) were determined using a Crinson multimeter while turbidity was measured using a Labcon Turbidimeter. The concentrations of Al, Ca, Cd, Cr, Fe, K, Mg, Mn, Na and Pb were analysed in triplicate using a Varian 520 flame atomic absorption spectrometer (AAS) supplied by PerkinElmer, after acid digestion with nitric acid in a fume cupboard. The average pH of the river from eight different sampling sites was 8.00 and 9.38 in wet and dry season respectively. Higher EC values were determined in the dry season (138.7 mS/m) than in the wet season (96.93 mS/m). Similarly, TDS values were higher in dry (929.29 mg/L) than in the wet season (640.72 mg/L) season. These values exceeded the recommended guideline of South Africa Department of Water Affairs and Forestry (DWAF) for domestic water use (70 mS/m) and that of the World Health Organization (WHO) (600 mS/m), respectively. Turbidity varied between 1.78-5.20 and 0.95-2.37 NTU in both wet and dry seasons. Total hardness of 312.50 mg/L and 297.75 mg/L as the concentration of CaCO3 was computed for the river in both the wet and the dry seasons and the river water was categorised as very hard. Mean concentration of the metals studied in both the wet and the dry seasons are: Na (94.06 mg/L and 196.3 mg/L), K (11.79 mg/L and 13.62 mg/L), Ca (45.60 mg/L and 41.30 mg/L), Mg (48.41 mg/L and 44.71 mg/L), Al (0.31 mg/L and 0.38 mg/L), Cd (0.01 mg/L and 0.01 mg/L), Cr (0.02 mg/L and 0.09 mg/L), Pb (0.05 mg/L and 0.06 mg/L), Mn (0.31 mg/L and 0.11 mg/L) and Fe (0.76 mg/L and 0.69 mg/L). Results from this study reveal that most of the metals were present in concentrations higher than the recommended guidelines of DWAF and WHO for domestic use and the protection of aquatic life.

Keywords: contamination, mining activities, surface water, trace metals

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Authors: J. Bahrawi, M. Elhag

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Estimation of evapotranspiration is always a major component in water resources management. Traditional techniques of calculating daily evapotranspiration based on field measurements are valid only for local scales. Earth observation satellite sensors are thus used to overcome difficulties in obtaining daily evapotranspiration measurements on regional scale. The Surface Energy Balance System (SEBS) model was adopted to estimate daily evapotranspiration and relative evaporation along with other land surface energy fluxes. The model requires agro-climatic data that improve the model outputs. Advance Along Track Scanning Radiometer (AATSR) and Medium Spectral Resolution Imaging Spectrometer (MERIS) imageries were used to estimate the daily evapotranspiration and relative evaporation over the entire Nile Delta region in Egypt supported by meteorological data collected from six different weather stations located within the study area. Daily evapotranspiration maps derived from SEBS model show a strong agreement with actual ground-truth data taken from 92 points uniformly distributed all over the study area. Moreover, daily evapotranspiration and relative evaporation are strongly correlated. The reliable estimation of daily evapotranspiration supports the decision makers to review the current land use practices in terms of water management, while enabling them to propose proper land use changes.

Keywords: daily evapotranspiration, relative evaporation, SEBS, AATSR, MERIS, Nile Delta

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Authors: G. Ozturk, B. Demirci

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It is well known that essential oils used for therapeutic purposes for many years. In this study, five different Pharmacopoeia grade essential oils (Achillea millefolium L., Pimpinella anisum L., Matricaria recutita L., Eucalyptus globulus L., Salvia officinalis L.) which obtained from commercial sources were evaluated for chemical compositions, synergistic antimicrobial activities, and lipoxygenase enzyme inhibitions. Volatile components were determined by gas chromatography/flame ionization detector and gas chromatography/mass spectrometer, simultaneously. The potential antimicrobial activity of essential oils was tested against oral pathogenic standard strains such as Streptococcus mutans, Streptococcus sanguinis, Staphylococcus aureus, Corynebacterium striatum, Candida albicans and Candida krusei by broth microdilution methods. Ciprofloxacin and ketoconazole were used positive controls. It has been observed that the essential oils tested have average inhibitory antimicrobial activity against oral pathogens with a Minimum Inhibition Concentration of 20-0.625 mg/mL. The active essential oils have been combined with antibiotics and synergistic effects have been evaluated by Checkerboard method. ƩFIC values were determined. In combination with antibiotics M. recutita essential oil has been shown to have a synergistic effect against S. aureus in combination with tetracycline (ƩFIC 0.46). In addition, 5-LOX inhibitory activity was measured by modifying the spectrophotometric method developed by Baylac and Racine. As a result, 5-LOX % inhibition of S. officinalis, E. globulus and M. recutita were calculated as 34.0 ± 6.66, 72.7 ± 2.78 and 27.7 ± 0.60, respectively.

Keywords: antimicrobial activity, essential oils, synergistic activity, 5-lipoxygenase inhibition

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Authors: Tie-Gang Wang, De-Qiang Meng, Yan-Mei Liu

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Ternary AlCrN coatings were widely used to prolong cutting tool life because of their high hardness and excellent abrasion resistance. However, the friction between the workpiece and cutter surface was increased remarkably during machining difficult-to-cut materials (such as superalloy, titanium, etc.). As a result, a lot of cutting heat was generated and cutting tool life was shortened. In this work, an appropriate amount of solid lubricant MoS₂ was added into the AlCrN coating to reduce the friction between the tool and the workpiece. A series of Al-Cr-N/MoS₂ self-lubricating coatings with different MoS₂ contents were prepared by high power impulse magnetron sputtering (HiPIMS) and pulsed direct current magnetron sputtering (Pulsed DC) compound system. The MoS₂ content in the coatings was changed by adjusting the sputtering power of the MoS₂ target. The composition, structure and mechanical properties of the Al-Cr-N/MoS2 coatings were systematically evaluated by energy dispersive spectrometer, scanning electron microscopy, X-ray photoelectron spectroscopy, X-ray diffractometer, nano-indenter tester, scratch tester, and ball-on-disk tribometer. The results indicated the lubricant content played an important role in the coating properties. As the sputtering power of the MoS₂ target was 0.1 kW, the coating possessed the highest hardness 14.1GPa, the highest critical load 44.8 N, and the lowest wear rate 4.4×10−3μm2/N.

Keywords: self-lubricating coating, Al-Cr-N/MoS₂ coating, wear rate, friction coefficient

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Authors: Maisarah Jaafar, Neil I. Ward

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Volcanic and geothermal activity can result in the release of arsenic (As), manganese (Mn), iron, selenium (Se), molybdenum (Mo) and uranium (U) into natural waters. Several studies have reported high levels of these elements in surface and groundwater in Argentina. The main focus has been on As associated with volcanic ash deposits. This study reports the trace element levels of groundwater from an agricultural region of south-eastern La Pampa and southern Buenos Aires provinces, Argentina which have reported high levels of human health problems (bone/teeth disorders, depression, arthritis, etc). Fifty-eight groundwater samples were collected from wells adjacent to Ruta 35 and an Agilent 7700x inductively coupled plasma mass spectrometer (ICP-MS) were used for total elemental analysis. Physicochemical analysis confirmed pH range of 7.05-8.84 and variable conductivity (988-3880 µS/cm) with total dissolved solid content of 502-1989 mg/l. The majority water samples are in an oxidizing environment (Eh= 45-146 mV). Total As levels ranged from (µg/l): 13.08 – 319.4 for La Pampa (LP) and 39.6 – 189.4 for Buenos Aires (BA); all above the WHO Guideline for Drinking Water, 10 µg/l As. Interestingly, Mo (LP: 1.85 – 85.39 µg/l; BA: 4.61– 55.55 µg/l;), Se (LP: 1.2 – 16.59 µg/l; BA: 0.3– 6.94 µg/l;) and U (LP: 1.85 – 85.39 µg/l; BA: 4.61– 55.55 µg/l;) levels are lower than reported values for northern La Pampa. Inter-elemental correlation displayed positive statistically significant between As-Mo, A-Se, As-U while negative statistically significant between As-Mn and As-Fe. This confirms that the source of the trace element is similar to that reported for other region of Argentina, namely volcanic ash deposition.

Keywords: Argentina, groundwater, trace element, volcanic activity

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Authors: Diana La Forgia, Jean Baptiste Thibord, François Verheggen

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Volatiles Organic Compound (VOCs) are one of the many features of defense used by plants in their eternal fight against pests. Their main role is to attract the natural enemies of the herbivores. But on another hand, they can be used by the same herbivores to locate plants while foraging. In an attempt to fill a gap of knowledge in a complex web of interactions, we focused on wireworms (Coleoptera:Elateridae). Wireworms whose larvae feed on roots are one of the most spread pests of valuable crops such as maize and potatoes, causing important economical damage. Little is known about the root compounds that are playing a role in the attraction of the larvae. In order to know more about these compounds, we compared four different maize varieties (Zea mays mays) that are known to have different levels of attraction, from weak to strong, for wireworms in fields. We tested the attraction of larvae in laboratory conditions in dual-choice olfactometer assays where they were offered all possible combinations of the four maize varieties. Contemporary, we collected the VOCs of each variety during 24h using a push-and-pull system. The collected samples were then analyzed by gas chromatography coupled with a mass spectrometer (GC-MS) to identify their molecular profiles. The choice of the larvae was dependent on the offered combination and some varieties were preferred to others. Differences were also observed in terms of quantitative and qualitative emissions of volatile profiles between the maize varieties. Our aim is to develop traps based on VOCs from maize roots to open a new frontier in wireworms management.

Keywords: integrated pest management, maize roots, plant defense, volatile organic compounds, wireworms

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Authors: Hossein Navid, Maryam Adeli Khadem, Shahin Oustan, Mahmoud Zareie

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Among the nutrients needed by the plants, three elements containing nitrate, phosphorus and potassium are more important. The objective of this research was measuring these nutrient amounts in soil using Fourier transform infrared spectroscopy in range of 400- 4000 cm-1. Soil samples for different soil types (sandy, clay and loam) were collected from different areas of East Azerbaijan. Three types of fertilizers in conventional farming (urea, triple superphosphate, potassium sulphate) were used for soil treatment. Each specimen was divided into two categories: The first group was used in the laboratory (direct measurement) to extract nitrate, phosphorus and potassium uptake by colorimetric method of Olsen and ammonium acetate. The second group was used to measure drug absorption spectrometry. In spectrometry, the small amount of soil samples mixed with KBr and was taken in a small pill form. For the tests, the pills were put in the center of infrared spectrometer and graphs were obtained. Analysis of data was done using MINITAB and PLSR software. The data obtained from spectrometry method were compared with amount of soil nutrients obtained from direct drug absorption using EXCEL software. There were good fitting between these two data series. For nitrate, phosphorus and potassium R2 was 79.5%, 92.0% and 81.9%, respectively. Also, results showed that the range of MIR (mid-infrared) is appropriate for determine the amount of soil nitrate and potassium and can be used in future research to obtain detailed maps of land in agricultural use.

Keywords: nitrate, phosphorus, potassium, soil nutrients, spectroscopy

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Authors: Akshita Jindal, Renu Chadha, Maninder Karan

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Supramolecular chemistry has gained recent eminence in a flurry of research documents demonstrating the formation of new crystalline forms with potentially advantageous characteristics. Mesalamine (5-amino salicylic acid) belongs to anti-inflammatory class of drugs, is used to treat ulcerative colitis and Crohn’s disease. Unfortunately, mesalamine suffer from poor solubility and therefore very low bioavailability. This work is focused on preparation and characterization of cocrystal of mesalamine with nicotinamide (MNIC) a coformer of GRAS status. Cocrystallisation was achieved by solvent drop grinding in stoichiometric ratio of 1:1 using acetonitrile as solvent and was characterized by various techniques including DSC (Differential Scanning Calorimetry), PXRD (X-ray Powder Diffraction), and FTIR (Fourier Transform Infrared Spectrometer). The co-crystal depicted single endothermic transitions (254°C) which were different from the melting peaks of both drug (288°C) and coformer (128°C) indicating the formation of a new solid phase. Different XRPD patterns and FTIR spectrums for the co-crystals from those of individual components confirms the formation of new phase. Enhancement in apparent solubility study and intrinsic dissolution study showed effectiveness of this cocrystal. Further improvement in pharmacokinetic profile has also been observed with 2 folds increase in bioavailability. To conclude, our results show that application of nicotinamide as a coformer is a viable approach towards the preparation of cocrystals of potential drug molecule having limited solubility.

Keywords: cocrystal, mesalamine, nicotinamide, solvent drop grinding

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Authors: Ram Prasad Baral

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A large number of herb materials contain Essential Oils with extensive bioactivities. Acknowledging the importance of plants and its medicinal value, extraction of Essential Oil had been done using Steam Distillation method. In this project, Steam Distillation was used to extract oil from different plant materials like Chamomilla recutita (L.) Rauschert, Artemisia Vulgaris L, Rhododendron anthopogon D. Don, Cymbopogon nardus L, Andropogon nardus, Cinnamomum tamala, Juniperus spp, Cymbopohonflexuosus flexuous, Mantha Arvensia, Nardostachys Jatamansi, Wintergreen Essential Oil, and Valeriana Officinalis. Research has confirmed centuries of practical use of essential oils, and we now know that the 'fragrant pharmacy' contains compounds with an extremely broad range of biochemical effects. Essential oils are so termed as they are believed to represent the very essence of odor and flavor. The recovery of Essential Oil from the raw botanical starting material is very important since the quality of the oil is greatly influenced during this step. There is a variety of methods for obtaining volatile oils from plants. Steam distillation method was found to be one of the promising techniques for the extraction of essential oil from plants as reputable distiller will preserve the original qualities of the plant. The distillation was conducted in Clevenger apparatus in which boiling, condensing, and decantation was done. Analysis of essential oil was done using Gas Chromatography-Mass Spectrometer apparatus, which gives evaluates essential oil qualitatively and quantitatively. The volume of essential oil obtained was changing with respect to temperature and time of heating.

Keywords: Chamomilla recutita (L.) Rauschert, Artemisia Vulgaris L, Rhododendron anthopogon D. Don, Cymbopogon nardus L, Andropogon nardus, Cinnamomum tamala, Juniperus spp, Cymbopohonflexuosus flexuous, Mantha

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Authors: Akhila Konala, Jagadeeswara Reddy Vennapusa, Sujay Chattopadhyay

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The energy consumption of humankind is growing day by day due to an increase in the population, industrialization and their needs for living. Fossil fuels are the major source of energy to satisfy energy needs, which are non-renewable energy resources. So, there is a need to develop green resources for energy production and storage. Phase change materials (PCMs) derived from plants (green resources) are well known for their capacity to store the thermal energy as latent heat during their phase change from solid to liquid. This property of PCM could be used for storage of thermal energy. In this study, a composite with fatty acid (caprylic acid; M.P 15°C, Enthalpy 179kJ/kg) as a phase change material and expanded perlite as support porous matrix was prepared through direct impregnation method for thermal energy storage applications. The prepared composite was characterized using Differential scanning calorimetry (DSC), Field Emission Scanning Electron Microscope (FESEM), Thermal Gravimetric Analysis (TGA), and Fourier Transform Infrared (FTIR) spectrometer. The melting point of the prepared composite was 15.65°C, and the melting enthalpy was 82kJ/kg. The surface nature of the perlite was observed through FESEM. It was observed that there are micro size pores in the perlite surface, which were responsible for the absorption of PCM into perlite. In TGA thermogram, the PCM loss from composite was started at ~90°C. FTIR curves proved there was no chemical interaction between the perlite and caprylic acid. So, the PCM composite prepared in this work could be effective to use in temperature maintenance of buildings.

Keywords: caprylic acid, composite, phase change materials, PCM, perlite, thermal energy

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Authors: Harikrishna Yadav Nanganuru, Narasimhulu Korrapati

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The demand for the lead (Pb) in the battery industry has been growing for last twenty years. On an average about 2.35 million tons of lead is used in the battery industry. According to the survey of supply and demand battery industry is using 75% of lead produced every year. Due to the increase in battery scrap, secondary lead production has been increasing in this decade. Europe and USA together account for 75% of the world’s secondary lead production. The effluent from used battery scrap consists of high concentrations of lead. Unauthorized disposal of spent batteries, which contain intolerable concentration of lead, into landfills or municipal water canals causes release of Pb into the environment. Lead is one of the toxic heavy metals that have large damaging effects on the human health. Due to its persistence and toxicity, the presence of Pb in drinking water is considered as a special concern. Accumulation of Pb in the human body for long period of time can result in the malfunctioning of some organs. Many technologies have been developed for the removal of lead using microorganisms. In this paper, effluent was taken from the spent battery scrap and was characterized by inductively coupled plasma atomic emission spectrometer. Microorganisms play an important role in removal of lead from the contaminated sites. So, the bacteria were isolated from the effluent. Optimum conditions for the microbial growth and applied for the lead removal. These bacterial cells were immobilized and used for the removal of Pb from the known concentration of metal solution. Scanning electron microscopic (SEM) studies were shown that the Pb was efficiently adsorbed by the immobilized bacteria. From the results of Atomic Absorption Spectroscopy (AAS), 83.40 percentage of Pb was removed in a batch culture.

Keywords: adsorption, effluent, immobilization, lead (Pb)

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Authors: Kalpana Rajouriya, Ajay Taneja

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Particulates are ubiquitous in the air environment and cause serious threats to human beings, such as lung cancer, COPD, and Asthma. Particulates mainly arise from industrial effluent, vehicular emission, and other anthropogenic activities. In the glass industrial city Firozabad, real-time monitoring of size segregated Particulate Matter (PM) and black carbon was done by Aerosol Black Carbon Detector (ABCD) and GRIMM portable aerosol Spectrometer at two different sites in which one site is urban and another is rural. The average mass concentration of size segregated PM during the study period (March & April 2022) was recorded as PM10 (223.73 g/m⁻³), PM5.0 (44.955 g/m⁻³), PM2.5 (59.275 g/m⁻³), PM1.0 (33.02 g/m⁻³), PM0.5 (2.05 g/m⁻³), and PM0.25 (2.99 g/m⁻³). The highest concentration of BC was found in Urban due to the emissions from diesel engines and wood burning, while NO2 was highest at the rural sites. The average concentrations of PM10 (6.08 and 2.73 times) PM2.5 exceeded the NAAQS and WHO guidelines. Particulate Matter deposition and health risk assessment was done by MPPD and USEPA model to know about the particulate matter toxicity in industrial residents. Health risk assessment results showed that Children are most likely to be affected by exposure of PM10 and PM2.5 and may have various non-carcinogenic and carcinogenic diseases. Deposition results inferred that the sensitive exposed population, especially 9 years old children, have high PM deposition as well as visualization and may be at risk of developing health-related problems from exposure to size-segregated PM. They will be discussed during presentation.

Keywords: particulate matter, black carbon, NO2, deposition of PM, health risk

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Authors: M. Mathuthu, N. N. Gaxela, R. Y. Olobatoke

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A study was carried out to assess the heavy metal and radionuclide concentrations of water from the waste water treatment plant in Mafikeng Local Municipality to evaluate treatment efficiency. Ten water samples were collected from various stages of water treatment which included sewage delivered to the plant, the two treatment stages and the effluent and also the community. The samples were analyzed for heavy metal content using Inductive Coupled Plasma Mass Spectrometer. Gross α/β activity concentration in water samples was evaluated by Liquid Scintillation Counting whereas the concentration of individual radionuclides was measured by gamma spectroscopy. The results showed marked reduction in the levels of heavy metal concentration from 3 µg/L (As)–670 µg/L (Na) in sewage into the plant to 2 µg/L (As)–170 µg/L (Fe) in the effluent. Beta activity was not detected in water samples except in the in-coming sewage, the concentration of which was within reference limits. However, the gross α activity in all the water samples (7.7-8.02 Bq/L) exceeded the 0.1 Bq/L limit set by World Health Organization (WHO). Gamma spectroscopy analysis revealed very high concentrations of 235U and 226Ra in water samples, with the lowest concentrations (9.35 and 5.44 Bq/L respectively) in the in-coming sewage and highest concentrations (73.8 and 47 Bq/L respectively) in the community water suggesting contamination along water processing line. All the values were considerably higher than the limits of South Africa Target Water Quality Range and WHO. However, the estimated total doses of the two radionuclides for the analyzed water samples (10.62 - 45.40 µSv yr-1) were all well below the reference level of the committed effective dose of 100 µSv yr-1 recommended by WHO.

Keywords: gross α/β activity, heavy metals, radionuclides, 235U, 226Ra, water sample

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Authors: Anıl Dinçer, Dilek Duranoğlu

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Ketones, which are widely used as solvent and chemical intermediates in chemical process industry, are commercially produced by using catalytic dehydrogenation of secondary alcohols at higher temperature (300-500ºC), and pressure (1-5 bar). Although it is possible to obtain high conversion values (60-87%) via gas phase catalytic dehydrogenation, working high temperature and pressure can result in side reactions and shorten the catalyst life. In order to overcome these challenges, catalytic dehydrogenation in the presence of an appropriate liquid solvent has been started to use. Hence, secondary alcohols can be converted to respective ketones at relatively low temperature (150-200ºC) under atmospheric pressure. In this study, methyl ethyl ketone and acetone was produced via catalytic dehydrogenation of appropriate secondary alcohols (isopropyl alcohol and sec-butyl alcohol) in the presence of liquid solvent at 160-190ºC. Obtained methyl ethyl ketone and acetone were analyzed by using FTIR and GC spectrometer. Effects of temperature, amount of catalyst and solvent on conversion and reaction rate were investigated. Optimum process conditions, which gave high conversion and reaction rate, were determined. According to GC results, 70% of secondary butyl alcohol and 42% of isopropyl alcohol was converted to related ketone (methyl ethyl ketone and acetone, respectively) at optimum process conditions. After distillation, 99.13% methyl ethyl ketone and 99.20% acetone was obtained. Consequently, liquid phase dehydrogenation process, which can compete with commercial gas phase process, was developed.

Keywords: dehydrogenation, liquid phase, methyl ethyl ketone, secondary alcohol

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Authors: M. Pilar Valles-gonzalez, Alejandro Gonzalez Meije, Ana Pastor Muro, Maria Garcia-Martinez, Beatriz Gonzalez Caballero

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This paper studies a failure case of a fuel pressure supply tube from an aircraft engine. Multiple fracture cases of the fuel pressure control tube from aircraft engines have been reported. The studied set was composed of the mentioned tube, a welded connecting pipe, where the fracture has been produced, and a union nut. The fracture has been produced in one most critical zones of the tube, in a region next to the supporting body of the union nut to the connector. The tube material was X6CrNiTi18-10, an austenitic stainless steel. Chemical composition was determined using an X-Ray fluorescence spectrometer (XRF) and combustion equipment. Furthermore, the material has been mechanical, by hardness test, and microstructural characterized using a stereomicroscope and an optical microscope. The results confirmed that it is within specifications. To determine the macrofractographic features, a visual examination and a stereo microscope of the tube fracture surface have been carried out. The results revealed a tube plastic macrodeformation, surface damaged, and signs of a possible corrosion process. Fracture surface was also inspected by scanning electron microscopy (FE-SEM), equipped with a microanalysis system by X-ray dispersive energy (EDX), to determine the microfractographic features in order to find out the failure mechanism involved in the fracture. Fatigue striations, which are typical from a progressive fracture by a fatigue mechanism, have been observed. The origin of the fracture has been placed in defects located on the outer wall of the tube, leading to a final overload fracture.

Keywords: aircraft engine, fatigue, FE-SEM, fractography, fracture, fuel tube, microstructure, stainless steel

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Authors: Muhammad Mohsin, Mir Md Abdus Salam, Pertti Pulkkinen, Ari Pappinen

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Soil and water contamination by heavy metals is a major challenging issue for the environment. Phytoextraction is an emerging, environmentally friendly and cost-efficient technology in which plants are used to eliminate pollutants from the soil and water. We aimed to assess the copper (Cu) and zinc (Zn) removal efficiency by two willow varieties such as Klara (S. viminalis x S. schwerinii x S. dasyclados) and Karin ((S.schwerinii x S. viminalis) x (S. viminalis x S.burjatica)) under different soil treatments (control/unpolluted, polluted, lime with polluted, wood ash with polluted). In 180 days of pot experiment, these willow varieties were grown in a highly polluted soil collected from Pyhasalmi mining area in Finland. The lime and wood ash were added to the polluted soil to improve the soil pH and observe their effects on metals accumulation in plant biomass. The Inductively Coupled Plasma Optical Emission Spectrometer (ELAN 6000 ICP-EOS, Perkin-Elmer Corporation) was used in this study to assess the heavy metals concentration in the plant biomass. The result shows that both varieties of willow have the capability to accumulate the considerable amount of Cu and Zn varying from 36.95 to 314.80 mg kg⁻¹ and 260.66 to 858.70 mg kg⁻¹, respectively. The application of lime and wood ash substantially affected the stimulation of the plant height, dry biomass and deposition of Cu and Zn into total plant biomass. Besides, the lime application appeared to upsurge Cu and Zn concentrations in the shoots and leaves in both willow varieties when planted in polluted soil. However, wood ash application was found more efficient to mobilize the metals in the roots of both varieties. The study recommends willow plantations to rehabilitate the Cu and Zn polluted soils.

Keywords: heavy metals, lime, phytoextraction, wood ash, willow

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Authors: Emmanuel Ekpa, Adaji Andrew, Queen Opaluwa, Isreal Daraobong

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Three (3) indigenous bacteria species (Bacillus spp, Acinectobacter spp and Moraxella spp) previously isolated from contaminated soil of some auto mechanic workshops were used for bioremediation studies on some irrigation water used at Sarkin-noma Fadama farms located in Lokoja Kogi State, Nigeria. This was done in order to investigate their bioremediation potentials using a simple pour plate method. The physicochemical parameters and heavy metal analysis (using AAS iCE 3000) of the irrigation water were performed before and after inoculation of the isolated organisms. Nitrate and phosphate concentration were found to be 10.56mg/L and 12.63mg/L prior to inoculation while iron and zinc were 0.9569mg/L and 0.2245mg/L respectively. Other physicochemical parameters were also observed to be high prior to inoculation. After the bioremediation test (inoculation with the isolated organisms), a nitrate and phosphate content of 2.53mg/L and 2.61mg/L were recorded respectively, iron and zinc gave 0.1694mg/L and 0.0174mg/L concentrations while other physicochemical parameters measured were also found to be lower in their respective values. The implication of this present study is that a number of carefully isolated indigenous bacteria species are capable of reducing the amount of heavy metal concentrations in water. Also, non-metallic contaminants like nitrate and phosphate are susceptible to bioremediation in the presence of such efficient system.

Keywords: bioremediation, heavy metals, physicochemical parameters, Bacillus spp, Acinectobacter spp and Moraxella spp, AAS, spectrometer 3000

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Authors: Changde Zhang, Qiang Zhang, Shilong Zheng, Jiawang Liu, Shanchun Guo, Qiu Zhong, Guangdi Wang

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Fulvestrant was approved by FDA to treat breast cancer as a selective estrogen receptor downregulator (SERD) with intramuscular injection administration. ZB716, a fulvestarnt-3 boronic acid, is an SERD with comparable anticancer effect to fulvestrant, but could produce good pharmacokinetic properties under oral administration with mice or rat models. To understand why ZB716 produced much better oral bioavailability, it was proposed that the boronic acid blocked the phase II direct biotransformation with the hydroxyl group on the 3 position of the aromatic ring on fulvestrant. In this study, ZB716 or fulvestrant was incubated with human liver microsome and oxidation cofactor NADPH in vitro. Their metabolites after oxidation were profiled with the Q-Exactive, a high-resolution mass spectrometer. The result showed that ZB716 blocked the forming of hydroxyl groups on its benzene ring except for the oxidation of C-B bond forming fulvestrant in its metabolites, and the concentration of fulvestrant with one more hydroxyl group found in the metabolites from incubation with fulvestrant was about 34 fold high as that formed from incubation with ZB716. Compared to fulvestrant, ZB716 is expected to be much difficult to be further bio-transformed into more hydrophilic compounds, to be difficult excreted out of blood system, and to have longer residence time in blood, which can lead to higher oral bioavailability. This study provided evidence to explain the high bioavailability of ZB716 after oral administration from the perspective of its difficulty of oxidation, a phase I biotransformation, on positions on its aromatic ring.

Keywords: biotransformation, fulvestrant, metabolite profiling, ZB716

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Authors: Paballo M. Moshupya, Tamiru A. Abiye, Ian Korir

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Mining and processing of naturally occurring radioactive materials could result in elevated levels of natural radionuclides in the environment. The aim of this study was to evaluate the radioactivity levels on a large scale in the West Rand District in South Africa, which is dominated by abandoned gold mine tailings and the consequential radiological exposures to members of the public. The activity concentrations of ²³⁸U, ²³²Th and 40K in mine tailings, soil and rocks were assessed using the BGO Super-Spec (RS-230) gamma spectrometer. The measured activity concentrations for ²³⁸U, ²³²Th and 40K in the studied mine tailings were found to range from 209.95 to 2578.68 Bq/kg, 19.49 to 108.00 Bq/kg and 31.30 to 626.00 Bq/kg, respectively. In surface soils, the overall average activity concentrations were found to be 59.15 Bq/kg, 34.91 and 245.64 Bq/kg for 238U, ²³²Th and 40K, respectively. For the rock samples analyzed, the mean activity concentrations were 32.97 Bq/kg, 32.26 Bq/kg and 351.52 Bg/kg for ²³⁸U, ²³²Th and 40K, respectively. High radioactivity levels were found in mine tailings, with ²³⁸U contributing significantly to the overall activity concentration. The external gamma radiation received from surface soil in the area is generally low, with an average of 0.07 mSv/y. The highest annual effective doses were estimated from the tailings dams and the levels varied between 0.14 mSv/y and 1.09 mSv/y, with an average of 0.51 mSv/y. In certain locations, the recommended dose constraint of 0.25 mSv/y from a single source to the average member of the public within the exposed population was exceeded, indicating the need for further monitoring and regulatory control measures specific to these areas to ensure the protection of resident members of the public.

Keywords: activity concentration, gold mine tailings, in-situ gamma spectrometry, radiological exposures

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Authors: Mark-Adam Kellerman

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Proteins are capable of exploring vast mutational spaces. This makes it difficult for protein engineers to devise rational methods to improve stability and function via mutagenesis. Deciding which residues to mutate requires knowledge of the characteristics they elicit. We probed the characteristics of residues in granulocyte-colony stimulating factor (G-CSF) using a thermal melt (from 295K to 323K) to denature it in a 700 MHz Bruker spectrometer. These characteristics included dynamics, micro-environmental changes experienced/ induced during denaturing and structure-function relationships. 15N-1H HSQC experiments were performed at 2K increments along with this thermal melt. We observed that dynamic residues that also undergo a lot of change in their microenvironment were predominantly in unstructured regions. Moreover, we were able to identify four residues (G4, A6, T133 and Q134) that we class as high priority targets for mutagenesis, given that they all appear in both the top 10% of measures for environmental changes and dynamics (∑Δ and ∆PI). We were also able to probe these NMR observables and combine them with molecular dynamics (MD) to elucidate what appears to be an opening motion of G-CSFs binding site III. V48 appears to be pivotal to this opening motion, which also seemingly distorts the loop region between helices A and B. This observation is in agreement with previous findings that the conformation of this loop region becomes altered in an aggregation-prone state of G-CSF. Hence, we present here an approach to profile the characteristics of residues in order to highlight their potential as rational mutagenesis targets and their roles in important conformational changes. These findings present not only an opportunity to effectively make biobetters, but also open up the possibility to further understand epistasis and machine learn residue behaviours.

Keywords: protein engineering, rational mutagenesis, NMR, molecular dynamics

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Authors: Violina Angelova, Stefan Krustev

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The aim of this work was to evaluate the effectiveness of different soil test extractants for the determination of available soil phosphorus in five internationally certified standard soils, sludge and clay (NCS DC 85104, NCS DC 85106, ISE 859, ISE 952, ISE 998). The certified samples were extracted with the following methods/extractants: CaCl₂, CaCl₂ and DTPA (CAT), double lactate (DL), ammonium lactate (AL), calcium acetate lactate (CAL), Olsen, Mehlich 3, Bray and Kurtz I, and Morgan, which are commonly used in soil testing laboratories. The phosphorus in soil extracts was measured colorimetrically using Spectroquant Pharo 100 spectrometer. The methods used in the study were evaluated according to the recovery of available phosphorus, facility of application and rapidity of performance. The relationships between methods are examined statistically. A good agreement of the results from different soil test was established for all certified samples. In general, the P values extracted by the nine extraction methods significantly correlated with each other. When grouping the soils according to pH, organic carbon content and clay content, weaker extraction methods showed analogous trends; also among the stronger extraction methods, common tendencies were found. Other factors influencing the extraction force of the different methods include soil: solution ratio, as well as the duration and power of shaking the samples. The mean extractable P in certified samples was found to be in the order of CaCl₂ < CAT < Morgan < Bray and Kurtz I < Olsen < CAL < DL < Mehlich 3 < AL. Although the nine methods extracted different amounts of P from the certified samples, values of P extracted by the different methods were strongly correlated among themselves. Acknowledgment: The financial support by the Bulgarian National Science Fund Projects DFNI Н04/9 and DFNI Н06/21 are greatly appreciated.

Keywords: available soil phosphorus, certified samples, determination, soil test extractants

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Authors: Olanrewaju Rotimi Bodede, Akinlabi Oyetunji

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Modeling the dry compressive strength of sodium silicate bonded kaolin refractory bricks was studied. The materials used for this research work included refractory clay obtained from Ijero-Ekiti kaolin deposit on coordinates 7º 49´N and 5º 5´E, sodium silicate obtained from the open market in Lagos on coordinates 6°27′11″N 3°23′45″E all in the South Western part of Nigeria. The mineralogical composition of the kaolin clay was determined using the Energy Dispersive X-Ray Fluorescence Spectrometer (ED-XRF). The clay samples were crushed and sieved using the laboratory pulveriser, ball mill and sieve shaker respectively to obtain 100 μm diameter particles. Manual pipe extruder of dimension 30 mm diameter by 43.30 mm height was used to prepare the samples with varying percentage volume of sodium silicate 5 %, 7.5 % 10 %, 12.5 %, 15 %, 17.5 %, 20% and 22.5 % while kaolin and water were kept at 50 % and 5 % respectively for the comprehensive test. The samples were left to dry in the open laboratory atmosphere for 24 hours to remove moisture. The samples were then were fired in an electrically powered muffle furnace. Firing was done at the following temperatures; 700ºC, 750ºC, 800ºC, 850ºC, 900ºC, 950ºC, 1000ºC and 1100ºC. Compressive strength test was carried out on the dried samples using a Testometric Universal Testing Machine (TUTM) equipped with a computer and printer, optimum compression of 4.41 kN/mm2 was obtained at 12.5 % sodium silicate; the experimental results were modeled with MATLAB and Origin packages using polynomial regression equations that predicted the estimated values for dry compressive strength and later validated with Pearson’s rank correlation coefficient, thereby obtaining a very high positive correlation value of 0.97.

Keywords: dry compressive strength, kaolin, modeling, sodium silicate

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Authors: Ozlem Temiz Arpaci, Meryem Tasci, Hakan Goker

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Benzimidazole, a structural isostere of indol and purine nuclei that can interact with biopolymers, can be identified as master key. So that benzimidazole compounds are important fragments in medicinal chemistry because of their wide range of biological activities including antimicrobial activity. We planned to synthesize some benzimidazole compounds for developing new antimicrobial drug candidates. In this study, we put some heterocyclic rings on second position and an amidine group on the fifth position of benzimidazole ring and synthesized them using a multiple step procedure. For the synthesis of the compounds, as the first step, 4-chloro-3-nitrobenzonitrile was reacted with cyclohexylamine in dimethyl formamide. Imidate esters (compound 2) were then prepared with absolute ethanol saturated with dry HCl gas. These imidate esters which were not too stable were converted to compound 3 by passing ammonia gas through ethanol. At the Pd / C catalyst, the nitro group is reduced to the amine group (compound 4). Finally, various aldehyde derivatives were reacted with sodium metabisulfite addition products to give compound 5-20. Melting points were determined on a Buchi B-540 melting point apparatus in open capillary tubes and are uncorrected. Elemental analyses were done a Leco CHNS 932 elemental analyzer. 1H-NMR and 13C-NMR spectra were recorded on a Varian Mercury 400 MHz spectrometer using DMSO-d6. Mass spectra were acquired on a Waters Micromass ZQ using the ESI(+) method. The structures of them were supported by spectral data. The 1H-NMR, 13C NMR and mass spectra and elemental analysis results agree with those of the proposed structures. Antimicrobial activity studies of the synthesized compounds are under the investigation.

Keywords: benzimidazoles, synthesis, structure elucidation, antimicrobial

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Authors: Li Maksym, Prabhakar M. N., Jung-Il Song

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In this study, a flame retardant and hydrophobic cotton textile were prepared by utilizing a renewable halogen-free bio-based solution based on chitosan, urea, and phytic acid, named bio-flame retardant liquid (BFL), through facile dip-coating technology. Deposition of BFL on the surface of the cotton was confirmed by Fourier-transform infrared spectroscopy and scanning electron microscope coupled with energy-dispersive X-ray spectrometer. Thermal and flame retardant properties of the cottons were studied with thermogravimetric analysis, differential scanning calorimetry, vertical flame test, cone calorimeter test. Only with 8.8% of dry weight gain treaded cotton showed self-extinguish properties during fire test. Cone calorimeter test revealed a reduction of peak heat release rate from 203.2 to 21 kW/m2 and total heat release from 20.1 to 2.8 MJ/m2. Incidentally, BFL remarkably improved the thermal stability of flame retardant cotton from expressed in an enhanced amount of char at 700 °C (6.7 vs. 33.5%). BFL initiates the formation of phosphorous and silica contain char layer whichrestrains the propagation of heat and oxygen to unburned materialstrengthen by the liberation of non-combustible gases, which reduce the concentration of flammable volatiles and oxygen hence reducing the flammability of cotton. In addition, hydrophobicity and specific ignition test for upholstery application were performed. In conjunction, the proposed flame retardant cotton is potentially translatable to be utilized as upholstery materials in public transport.

Keywords: cotton farbic, flame retardancy, surface coating, intumescent mechanism

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