Search results for: pesticide mixture

Authors: Salah Brahim Belakhdar, Tari Mohammed Amin, Rafai Abderrahmen, Amalsi Bilal

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Shear strength of sandy soils has been considered as the important parameter to study the stability of different civil engineering structures when subjected to monotonic, cyclic, and earthquake loading conditions. The proposed research investigated the effect of grading characteristics on the shear strength and mechanical behaviour of granular classes of sands mixed with salt in loose and dense states (Dr=15% and 90%). The laboratory investigation aimed at understanding the extent or degree at which shear strength of sand-silt mixture soil is affected by its gradation under static loading conditions. For the purpose of clarifying and evaluating the shear strength characteristics of sandy soils, a series of Casagrande shear box tests were carried out on different reconstituted samples of sand-silt mixtures with various gradations. The soil samples were tested under different normal stresses (100, 200, and 300 kPa). The results from this laboratory investigation were used to develop insight into the shear strength response of sand and sand-silt mixtures under monotonic loading conditions. The analysis of the obtained data revealed that the grading characteristics (D10, D50, Cu, ESR, and MGSR) have a significant influence on the shear strength response. It was found that shear strength can be correlated to the grading characteristics for the sand-silt mixture. The effective size ratio (ESR) and mean grain size ratio (MGSR) appear as pertinent parameters to predict the shear strength response of the sand-silt mixtures for soil gradation under study.

Keywords: mechanical behavior, silty sand, friction angle, cohesion, fines content

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Authors: Rupa Rani, Vipin Kumar

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Endosulfan, an organochlorine pesticide is of environmental concern due to its apparent persistence and toxicity. It has been reported as contaminants in soil, air, and water and is bioaccumulated and magnified in ecosystems. The combined use of microorganisms and plants has great potential for remediating soil contaminated with organic compounds such as pesticides. The objective of this study was to evaluate whether the bacterial inoculation influences plant growth promotion, endosulfan degradation in soil and endosulfan accumulation in different plant parts. Lycopersicon esculentum L. (Tomato) was grown in endosulfan spiked soil and inoculated with endosulfan tolerant bacterial strains. Endosulfan residues from different parts of plants and soil were extracted and estimated by using gas chromatograph equipped with 63Ni electron capture detector (GC-ECD). The inoculation of bacterial strains into the soil with plants showed a beneficial effect on endosulfan degradation and plant biomass production. Maximum endosulfan (90%) degradation was observed after 120 days of bacterial inoculation in the soil. Furthermore, there was significantly less endosulfan accumulation in roots and shoots of bacterial strains inoculated plants as compared to uninoculated plants. The results show the effectiveness of inoculated endosulfan tolerant bacterial strains to increase the remediation of endosulfan contaminated soil.

Keywords: organochlorine pesticides, endosulfan, degradation, plant-bacteria partnerships

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Authors: Mulugeta K. Tefera, Xiaolong Yang, Jian Liu

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Detection and tracking of moving objects are very important in many application contexts such as detection and recognition of people, visual surveillance and automatic generation of video effect and so on. However, the task of detecting a real shape of an object in motion becomes tricky due to various challenges like dynamic scene changes, presence of shadow, and illumination variations due to light switch. For such systems, once the moving object is detected, tracking is also a crucial step for those applications that used in military defense, video surveillance, human computer interaction, and medical diagnostics as well as in commercial fields such as video games. In this paper, an object presents in dynamic background is detected using adaptive mixture of Gaussian based analysis of the video sequences. Then the detected moving object is tracked using the region based moving object tracking and inter-frame differential mechanisms to address the partial overlapping and occlusion problems. Firstly, the detection algorithm effectively detects and extracts the moving object target by enhancing and post processing morphological operations. Secondly, the extracted object uses region based moving object tracking and inter-frame difference to improve the tracking speed of real-time moving objects in different video frames. Finally, the plotting method was applied to detect the moving objects effectively and describes the object’s motion being tracked. The experiment has been performed on image sequences acquired both indoor and outdoor environments and one stationary and web camera has been used.

Keywords: background modeling, Gaussian mixture model, inter-frame difference, object detection and tracking, video surveillance

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Authors: Mudawi M. Nour

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Background: Now a days, the multidisciplinary scientific research conception in the field of nanotechnology has witnessed development with regard to the numerous applications and synthesis of nanomaterials. Objective: The current investigation has been conducted with the main focus on the green synthesis of silver nanoparticles from the leaves of Salvadora persica and its antibacterial activity against MDR pathogens E. coli and S. aureus. Methodology: Silver nanoparticles (AgNPs) were prepared after addition of aqueous extract of Salvadora persica leaves. The UV-Vis spectrophotometer, Transmission Electron Microscopy (TEM), zeta potential and Scanning Electron Microscopy (SEM) were employed to detect the particle size and morphology, besides Fourier transform infra-red spectrometer (FTIR) analysis was performed to determine the capping and stabilizing agents in the extract. Antibacterial assay for the biogenic AgNPs was conducted against E. coli and S. aureus. Results: Color change of the mixture from yellow to dark brown is the first indication to AgNPs formation. Furthermore, 420 nm was the peak value for UV-Vis spectroscopy absorption of the mixture. Besides, TEM and SEM micrographs showed wide variability in the diameter of smaller NPs aggregated together with spherical shapes, and zeta sizer showed about 153.3 nm as an average size of nanoparticles. Microbial suppression was noticed for the tested microorganisms. Furthermore, with the help of FTIR analysis, the biomolecules that act as capping and stabilizing agents of AgNPs are proteins and phenols present in the plant extract. Conclusion: Salvadora persica leaves extract act as a reducing and stabilizing agent for the synthesis of AgNPs, keeping its ability to suppress the MDR pathogen.

Keywords: green synthesis, FTIR, MDR pathogen, salvadora persica

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Authors: Tomas Drevinskas, Ruta Mickiene, Audrius Maruska, Nicola Tiso, Algirdas Salomskas, Raimundas Lelesius, Agneta Karpovaite, Ona Ragazinskiene, Loreta Kubiliene

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Antiviral effect of substances accumulated by plants and natural products is known to ethno-pharmacy and modern day medicine. Antiviral properties are usually assigned to volatile compounds and polyphenols. This research work is divided into several parts and the task of this part was to investigate potential plants, potential substances and potential preparation conditions that can be used for the preparation of antiviral agents. Sixteen different medicinal plants, their parts and two types of propolis were selected for screening. Firstly, extraction conditions of non-volatile compounds were investigated: 3 pre-selected plants were extracted with 5 different ethanol – water mixtures (96%, 75%, 60%, 40%, 20 %, vol.) and bidistilled water. Total phenolic content, total flavonoid content and radical scavenging activity was determined. The results indicated that optimal extrahent is 40%, vol. of ethanol – water mixture. Further investigations were performed with the extrahent of 40%, vol. ethanol – water mixture. All 16 of selected plants, their parts and two types of propolis were extracted using selected extrahent. Determined total phenolic content, total flavonoid content and radical scavenging activity indicated that extracts of Origanum Vulgare L., Mentha piperita L., Geranium macrorrhizum L., Melissa officinalis L. and Desmodium canadence L. contains highest amount of extractable phenolic compounds (7.31, 5.48, 7.88, 8.02 and 7.16 rutin equivalents (mg/ ml) respectively), flavonoid content (2.14, 2.23, 2.49, 0.79 and 1.51 rutin equivalents (mg/ml) respectively) and radical scavenging activity (11.98, 8.72, 13.47, 13.22 and 12.22 rutin equivalents (mg/ml) respectively). Composition of the extracts is analyzed using HPLC.

Keywords: antiviral effect, plants, propolis, phenols

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Authors: F. Portet-Koltalo, Y. Tian, I. Berger, C. Boulanger-Lecomte, A. Benamar, N. Machour

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Sediments are complex environments which can accumulate a great variety of persistent toxic contaminants such as polychlorobiphenyles (PCBs), polycyclic aromatic hydrocarbons (PAHs) and some of their more toxic degradation metabolites such as hydroxylated PAHs (OH-PAHs). Owing to their composition, fine clayey sediments can be more difficult to extract than soils using conventional solvent extraction processes. So this study aimed to compare the potential of MSPD (matrix solid phase dispersive extraction) to extract PCBs, PAHs and OH-PAHs, in comparison with microwave assisted extraction (MAE). Methodologies: MAE extraction with various solvent mixtures was used to extract PCBs, PAHs and OH-PAHs from sediments in two runs, followed by two GC-MS analyses. MSPD consisted in crushing the dried sediment with dispersive agents, introducing the mixture in cartridges and eluting the target compounds with an appropriate volume of selected solvents. So MSPD combined with cartridges containing MIPs (molecularly imprinted polymers) designed for OH-PAHs was used to extract the three families of target compounds in only one run, followed by parallel analyses in GC-MS for PAHs/PCBs and HPLC-FLD for OH-PAHs. Results: MAE extraction was optimized to extract from clayey sediments, in two runs, PAHs/PCBs in one hand and OH-PAHs in the other hand. Indeed, the best conditions of extractions (mixtures of extracting solvents, temperature) were different if we consider the polarity and the thermodegradability of the different families of target contaminants: PAHs/PCBs were better extracted using an acetone/toluene 50/50 mixture at 130°C whereas OH-PAHs were better extracted using an acetonitrile/toluene 90/10 mixture at 100°C. Moreover, the two consecutive GC-MS analyses contributed to double the total analysis time. A matrix solid phase dispersive (MSPD) extraction procedure was also optimized, with the first objective of increasing the extraction recovery yields of PAHs and PCBs from fine-grained sediment. The crushing time (2-10 min), the nature of the dispersing agents added for purifying and increasing the extraction yields (Florisil, octadecylsilane, 3-chloropropyle, 4-benzylchloride), the nature and the volume of eluting solvents (methylene chloride, hexane, hexane/acetone…) were studied. It appeared that in the best conditions, MSPD was a better extraction method than MAE for PAHs and PCBs, with respectively, mean increases of 8.2% and 71%. This method was also faster, easier and less expensive. But the other advantage of MSPD was that it allowed to introduce easily, just after the first elution process of PAHs/PCBs, a step permitting the selective recovery of OH-PAHs. A cartridge containing MIPs designed for phenols was coupled to the cartridge containing the dispersed sediment, and various eluting solvents, different from those used for PAHs and PCBs, were tested to selectively concentrate and extract OH-PAHs. Thereafter OH-PAHs could be analyzed at the same time than PAHs and PCBs: the OH-PAH extract could be analyzed with HPLC-FLD, whereas the PAHs/PCBs extract was analyzed with GC-MS, adding only few minutes more to the total duration of the analytical process. Conclusion: MSPD associated to MIPs appeared to be an easy, fast and low expensive method, able to extract in one run a complex mixture of toxic apolar and more polar contaminants present in clayey fine-grained sediments, an environmental matrix which is generally difficult to analyze.

Keywords: contaminated fine-grained sediments, matrix solid phase dispersive extraction, microwave assisted extraction, molecularly imprinted polymers, multi-pollutant analysis

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Authors: Mahacine Amrani

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A simple and rapid method for the determination of alcohol in gasoline-alcohol mixtures using density measurements is described. The method can determine a minimum of 1% of alcohol by volume. The precision of the method is ± 3%.The method is more useful for field test in the quality assessment of alcohol blended fuels.

Keywords: gasoline-alcohol, mixture, alcohol determination, density, measurement, Morocco

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Authors: I. Berger, N. Machour, F. Portet-Koltalo

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Polycyclic aromatic hydrocarbons (PAHs) are toxic and carcinogenic pollutants produced in majority by incomplete combustion processes in industrialized and urbanized areas. After being emitted in atmosphere, these persistent contaminants are deposited to soils or sediments. Even if persistent, some can be partially degraded (photodegradation, biodegradation, chemical oxidation) and they lead to oxygenated metabolites (oxy-PAHs) which can be more toxic than their parent PAH. Oxy-PAHs are less measured than PAHs in sediments and this study aims to compare different analytical tools in order to extract and quantify a mixture of four hydroxylated PAHs (OH-PAHs) and four carbonyl PAHs (quinones) in sediments. Methodologies: Two analytical systems – HPLC with on-line UV and fluorescence detectors (HPLC-UV-FLD) and GC coupled to a mass spectrometer (GC-MS) – were compared to separate and quantify oxy-PAHs. Microwave assisted extraction (MAE) was optimized to extract oxy-PAHs from sediments. Results: First OH-PAHs and quinones were analyzed in HPLC with on-line UV and fluorimetric detectors. OH-PAHs were detected with the sensitive FLD, but the non-fluorescent quinones were detected with UV. The limits of detection (LOD)s obtained were in the range (2-3)×10-4 mg/L for OH-PAHs and (2-3)×10-3 mg/L for quinones. Second, even if GC-MS is not well adapted to the analysis of the thermodegradable OH-PAHs and quinones without any derivatization step, it was used because of the advantages of the detector in terms of identification and of GC in terms of efficiency. Without derivatization, only two of the four quinones were detected in the range 1-10 mg/L (LODs=0.3-1.2 mg/L) and LODs were neither very satisfying for the four OH-PAHs (0.18-0.6 mg/L). So two derivatization processes were optimized, comparing to literature: one for silylation of OH-PAHs, one for acetylation of quinones. Silylation using BSTFA/TCMS 99/1 was enhanced using a mixture of catalyst solvents (pyridine/ethyle acetate) and finding the appropriate reaction duration (5-60 minutes). Acetylation was optimized at different steps of the process, including the initial volume of compounds to derivatize, the added amounts of Zn (0.1-0.25 g), the nature of the derivatization product (acetic anhydride, heptafluorobutyric acid…) and the liquid/liquid extraction at the end of the process. After derivatization, LODs were decreased by a factor 3 for OH-PAHs and by a factor 4 for quinones, all the quinones being now detected. Thereafter, quinones and OH-PAHs were extracted from spiked sediments using microwave assisted extraction (MAE) followed by GC-MS analysis. Several mixtures of solvents of different volumes (10-25 mL) and using different extraction temperatures (80-120°C) were tested to obtain the best recovery yields. Satisfactory recoveries could be obtained for quinones (70-96%) and for OH-PAHs (70-104%). Temperature was a critical factor which had to be controlled to avoid oxy-PAHs degradation during the MAE extraction process. Conclusion: Even if MAE-GC-MS was satisfactory to analyze these oxy-PAHs, MAE optimization has to be carried on to obtain a most appropriate extraction solvent mixture, allowing a direct injection in the HPLC-UV-FLD system, which is more sensitive than GC-MS and does not necessitate a previous long derivatization step.

Keywords: derivatizations for GC-MS, microwave assisted extraction, on-line HPLC-UV-FLD, oxygenated PAHs, polluted sediments

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Authors: Supatra Karnjanapratum, Soottawat Benjakul

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Gelatin hydrolysate, especially from marine resource, has been known to possess antioxidative activity. Nevertheless, the activity is still lower in comparison with the commercially available antioxidant. Maillard reactions can be use to increase antioxidative activity of gelatin hydrolysate, in which the numerous amino group could be involved in glycation. In the present study, gelatin hydrolysate (GH) from unicorn leatherjacket skin prepared using glycyl endopeptidase with prior autolysis assisted process was used for preparation of Maillard reaction products (MRPs) under dry condition. The impacts of different factors including, types of saccharides, GH to saccharide ratio, incubation temperatures, relative humidity (RH) and times on antioxidative activity of MRPs were investigated. MRPs prepared using the mixture of GH and galactose showed the highest antioxidative activity as determined by both ABTS radical scavenging activity and ferric reducing antioxidant power during heating (0-48 h) at 60 °C with 65% RH, compared with those derived from other saccharide tested. GH to galactose ratio at 2:1 (w/w) yielded the MRPs with the highest antioxidative activity, followed by the ratios of 1:1 and 1:2, respectively. When the effects of incubation temperatures (50, 60, 70 °C) and RH (55, 65, 75%) were examined, the highest browning index and the absorbance at 280 nm were found at 70 °C, regardless of RH. The pH and free amino group content of MRPs were decreased with the concomitant increase in antioxidative activity as the reaction time increased. Antioxidative activity of MRPs generally increased with increasing temperature and the highest antioxidative activity was found when RH of 55% was used. Based on electrophoresis of MRP, the polymerization along with the formation of high molecular weight material was observed. The optimal condition for preparing antioxidative MRPs was heating the mixture of GH and galactose (2:1) at 70 °C and 55% RH for 36 h. Therefore, antioxidative activity of GH was improved by Maillard reaction and the resulting MRP could be used as natural antioxidant in food products.

Keywords: antioxidative activity, gelatin hydrolysate, maillard reaction, unicorn leatherjacket

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Authors: Ling Xu, Giuseppe Loprencipe, Antonio D'Andrea

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Asphalt pavement with recycled and sustainable materials has become the most commonly adopted strategy for road construction, including reclaimed asphalt pavement (RAP) and crumb rubber (CR) from waste tires. However, the adhesion and cohesion characteristics of rubberized reclaimed asphalt pavement were still ambiguous, resulting in deteriorated adhesion behavior and life performance. This research investigated the effect of bonding characteristics on rutting resistance and moisture susceptibility of rubberized reclaimed asphalt pavement in terms of two RAP sources with different oxidation levels and two tire rubber with different particle sizes. Firstly, the binder bond strength (BBS) test and bonding failure distinguishment were conducted to analyze the surface behaviors of binder-aggregate interaction. Then, the compatibility and penetration grade of rubberized RAP binder were evaluated by rotational viscosity test and penetration test, respectively. Hamburg wheel track (HWT) test with high-temperature viscoelastic deformation analysis was adopted, which illustrated the rutting resistance. Additionally, a water boiling test was employed to evaluate the moisture susceptibility of the mixture and the texture features were characterized with the statistical parameters of image colors. Finally, the colloid structure model of rubberized RAP binder with surface interaction was proposed, and statistical analysis was established to release the correlation among various indexes. This study concluded that the gel-phase colloid structure and molecular diffusion of the free light fraction would affect the surface interpretation with aggregate, determining the bonding characteristic of rubberized RAP asphalt.

Keywords: bonding characteristics, reclaimed asphalt pavement, rubberized asphalt, sustainable material

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Authors: T. Varazi, M. Pruidze, M. Kurashvili, N. Gagelidze, M. Sutton

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The complex phytoremediation approach given in the presented work implies joint application of natural sorbents, microorganisms, natural biosurfactants and plants. The approach is based on using the natural mineral composites, microorganism strains with high detoxification abilities, plants-phytoremediators and natural biosurfactants for enhancing the uptake of intermediates of pollutants by plant roots. In this complex strategy of phytoremediation technology, the sorbent serves to uptake and trap the pollutants and thus restrain their emission in the environment. The role of microorganisms is to accomplish the first stage biodegradation of organic contaminants. This is followed by application of a phytoremediation technology through purposeful planting of selected plants. Thus, using of different tools will provide restoration of polluted environment and prevention of toxic compounds’ dissemination from hotbeds of pollution for a considerable length of time. The main idea and novelty of the carried out work is the development of a new approach for the ecological safety. The wide spectrum of contaminants: Organochlorine pesticide – DDT, heavy metal –Cu, oil hydrocarbon (hexadecane) and wax have been used in this work. The presented complex biotechnology is important from the viewpoint of prevention, providing total rehabilitation of soil. It is unique to chemical pollutants, ecologically friendly and provides the control of erosion of soils.

Keywords: bioremediation, phytoremediation, pollutants, soil contamination

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Authors: Luísa P. Cruz-Lopes, Hugo Costa e Silva, Idalina Domingos, José Ferreira, Luís Teixeira de Lemos, Bruno Esteves

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The liquefaction process of cork based tree barks has led to an increase of interest due to its potential innovation in the lumber and wood industries. In this particular study the bark of Quercus cerris (Turkish oak) is used due to its appreciable amount of cork tissue, although of inferior quality when compared to the cork provided by other Quercus trees. This study aims to optimize alkaline catalysis liquefaction conditions, regarding several parameters. To better comprehend the possible chemical characteristics of the bark of Quercus cerris, a complete chemical analysis was performed. The liquefaction process was performed in a double-jacket reactor heated with oil, using glycerol and a mixture of glycerol/ethylene glycol as solvents, potassium hydroxide as a catalyst, and varying the temperature, liquefaction time and granulometry. Due to low liquefaction efficiency resulting from the first experimental procedures a study was made regarding different washing techniques after the filtration process using methanol and methanol/water. The chemical analysis stated that the bark of Quercus cerris is mostly composed by suberin (ca. 30%) and lignin (ca. 24%) as well as insolvent hemicelluloses in hot water (ca. 23%). On the liquefaction stage, the results that led to higher yields were: using a mixture of methanol/ethylene glycol as reagents and a time and temperature of 120 minutes and 200 ºC, respectively. It is concluded that using a granulometry of <80 mesh leads to better results, even if this parameter barely influences the liquefaction efficiency. Regarding the filtration stage, washing the residue with methanol and then distilled water leads to a considerable increase on final liquefaction percentages, which proves that this procedure is effective at liquefying suberin content and lignocellulose fraction.

Keywords: liquefaction, Quercus cerris, polyalcohol liquefaction, temperature

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Authors: D. Nkazi, S. E. Iyuke, J. Mulopo

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Increasing global energy demand as well as air quality concerns have in recent years led to the search for alternative clean fuels to replace fossil fuels. One such alternative is the blending of petrol with ethanol, which has numerous advantages such ethanol’s ability to act as oxygenate thus reducing the carbon monoxide emissions from the exhaust of internal combustion engines of vehicles. However, the hygroscopic nature of ethanol is a major concern in obtaining a perfectly homogenized petrol-ethanol fuel. This problem has led to the study of ways of homogenizing the petrol-ethanol mixtures. During the blending process, volumes fraction of ethanol and petrol were studied with respect to the depth within the storage container to confirm homogenization of the blend and time of storage. The results reveal that the density of the mixture was constant. The binodal curve of the ternary diagram shows an increase of homogeneous region, indicating an improved of interaction between water and petrol. The concentration distribution in the reactor showed proof of cavitation formation since in both directions, the variation of concentration with both time and distance was found to be oscillatory. On comparing the profiles in both directions, the concentration gradient, diffusion flux, and energy and diffusion rates were found to be higher in the vertical direction compared to the horizontal direction. It was therefore concluded that ultrasonication creates cavitation in the mixture which enhances mass transfer and mixing of ethanol and petrol. The horizontal direction was found to be the diffusion rate limiting step which proposed that the blender should have a larger height to diameter ratio. It is, however, recommended that further studies be done on the rate-limiting step so as to have actual dimensions of the reactor.

Keywords: ultrasonication, petrol, ethanol, concentration

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Authors: Nthabiseng Portia Mahumapelo, Andre van Niekerk, Ndabenhle Sosibo, Nirdesh Singh

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The foundry industry generates large quantities of solid waste in the form of waste foundry sand. The ever-increasing quantities of this type of industrial waste put pressure on land-filling space and its proper management has become a global concern. The South African foundry industry is not different when it comes to this solid waste generation. Utilizing the foundry waste sand in other applications has become an attractive avenue to deal with this waste stream. In the present paper, an evaluation was done on the suitability of foundry waste sand as an additive in clay masonry products. Purchased clay was added to the foundry waste sand sample in a 50/50 ratio. The mixture was named FC sample. The FC sample was mixed with water in a pan mixer until the mixture was consistent and suitable for extrusion. The FC sample was extruded and cut into briquettes. Water absorption, shrinkage and modulus of rupture tests were conducted on the resultant briquettes. Foundry waste sand and FC samples were respectively characterized mineralogically using X-Ray Diffraction, and the major and trace elements were determined using Inductively Coupled Plasma Optical Emission Spectroscopy. Adding purchased clay to the foundry waste sand positively influenced the workability of the test sample. Another positive characteristic was the low linear shrinkage, which indicated that products manufactured from the FC sample would not be susceptible to cracking. The water absorption values were acceptable and the unfired and fired strength values of the briquette’s samples were acceptable. In conclusion, tests showed that foundry waste sand can be used as an additive in masonry clay bricks, provided it is blended with good quality clay.

Keywords: foundry waste sand, masonry clay bricks, modulus of rupture, shrinkage

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Authors: Normah Sulaiman, Yong Zhi Kang, Nor Hayati Hussain, Abdul Rehman Khalid

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Segara Ninda owned by Din Ku Meh, the governor of the province Satul, a Malay man with a big role liaising with Thailand. This mansion is part of the legacy he left behind among other properties in George Town, Penang, besides his family. The island’s geographical location is strategic which has benefitted it through important trade routes for Europe, Middle, East, India, and China in the past. Due to this reasoning, various architectural styles were introduced in Penang; Late Straits Eclectic style is one of the forms of the Colonial Architectural style widely spread as vernacular shophouses in George Town. Segara Ninda is located among the mixture of nouveau-riche, historical and heritage sites at the most important street; Penang Road, which dated back to the late 18th century. This paper examines the strait eclectic style that Segara Ninda encompasses. Acknowledging the mixture of colonial architecture in Georgetown, we argue that the mansion faces challenging issues in conservation processes to be vindicated. This is reflected by analysing the spatial layout, visual elements quality, and its activity through interviews with the occupants of the mansion. The focus will be on the understanding of building form, features, and functions; respecting the architectural spaces and their activity. The methodology applied is to promote our understanding of the mix of culture that the mansion holds through documentation, observation and measuring exercises. This offers a positional interpretation of the mix of culture that the mansion holds. This conservation effort will further contribute exposure to the public and recognize it in the society as its essence is a deficiency character to the existing built environment.

Keywords: eclectic, heritage, spatial organization, culture

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Authors: Tomas Makaras

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Sticklebacks (Gasterosteiformes) are increasingly used in ecological and evolutionary research and become well-established role as model species for biologists. However, ecotoxicology studies concerning behavioural effects in sticklebacks regarding stress responses, mainly induced by chemical mixtures, have hardly been addressed. Moreover, although many authors in their studies emphasised the similarity between three-spined and nine-spined stickleback in morphological, neuroanatomical and behavioural adaptations to environmental changes, several comparative studies have revealed considerable differences between these species in and their susceptibility and resistance to variousstressors in laboratory experiments. The hypothesis of this study was that three-spined and nine-spined stickleback species will demonstrate apparent differences in response patterns and sensitivity to metal-based chemicals stimuli. For this purpose, we investigated the swimming behaviour (including mortality rate based on 96-h LC50 values) of two ecologically similar three-spined (Gasterosteusaculeatus) and nine-spined sticklebacks (Pungitiuspungitius) to short-term (up to 24 h) metal mixture (MIX) exposure. We evaluated the relevance and efficacy of behavioural responses of test species in the early toxicity assessment of chemical mixtures. Fish exposed to six (Zn, Pb, Cd, Cu, Ni and Cr) metals in the mixture were either singled out by the Water Framework Directive as priority or as relevant substances in surface water, which was prepared according to the environmental quality standards (EQSs) of these metals set for inland waters in the European Union (EU) (Directive 2013/39/EU). Based on acute toxicity results, G. aculeatus found to be slightly (1.4-fold) more tolerant of MIX impact than those of P. pungitius specimens. The performed behavioural analysis showed the main effect on the interaction between time, species and treatment variables. Although both species exposed to MIX revealed a decreasing tendency in swimming activity, these species’ responsiveness to MIX was somewhat different. Substantial changes in the activity of G. aculeatus were established after 3-h exposure to MIX solutions, which was 1.43-fold lower, while in the case of P. pungitius, 1.96-fold higher than established 96-h LC50 values for each species. This study demonstrated species-specific differences in response sensitivity to metal-based water pollution, indicating behavioural insensitivity of P. pungitiuscompared to G. aculeatus. While many studies highlight the usefulness and suitability of nine-spined sticklebacks for evolutionary and ecological research, attested by their increasing popularity in these fields, great caution must be exercised when using them as model species in ecotoxicological research to probe metal contamination. Meanwhile, G. aculeatus showed to be a promising bioindicator species in the environmental ecotoxicology field.

Keywords: acute toxicity, comparative behaviour, metal mixture, swimming activity

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Authors: Isam A. H. Al Zubaidy

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A quick process may be needed to get the benefit the big generated quantity of waste oil sludge (WOS). The process includes the mixing process of WOS with commercial diesel fuel. Different ratios of WOS to diesel fuel were prepared ranging 1:1 to 20:1 by mass. The mixture was continuously mixing for 10 minutes using bench type overhead stirrer and followed by filtration process to separate the soil waste from filtrate oil product. The quantity and the physical properties of the oil filtrate were measured. It was found that the addition of up to 15% WOS to diesel fuel was accepted without dramatic changes to the properties of diesel fuel. The amount of waste oil sludge was decreased by about 60% by mass. This means that about 60 % of the mass of sludge was recovered as light fuel oil. The physical properties of the resulting fuel from 10% sludge mixing ratio showed that the specific gravity, ash content, carbon residue, asphaltene content, viscosity, diesel index, cetane number, and calorific value were affected slightly. The color was changed to light black color. The sulfur content was increased also. This requires other processes to reduce the sulfur content of the resulting light fuel. A new desulfurization process was achieved using adsorption techniques with activated biomaterial to reduce the sulfur content to acceptable limits. Adsorption process by ZnCl₂ activated date palm kernel powder was effective for improvement of the physical properties of diesel like fuel. The final sulfur content was increased to 0.185 wt%. This diesel like fuel can be used in all tractors, buses, tracks inside and outside the refineries. The solid remaining seems to be smooth and can be mixed with asphalt mixture for asphalting the roads or can be used with other materials as an asphalt coating material for constructed buildings. Through this process, valuable fuel has been recovered, and the amount of waste material had decreased.

Keywords: oil sludge, diesel fuel, blending process, filtration process

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Authors: Muhammad Naeem Mushtaq, Muhammad Arshad, Shahid Majeed

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Maize is known as queen of cereals because of its highest genetic yield potential and multipurpose characteristics in human being and animal diet. Maize crop visited by many major, minor, visitors and sporadic insect pests. This study was conducted during 2014 to evaluate the richness and evenness of these insect pests and their interaction with metrological conditions at University of Agriculture, Faisalabad. In this experiment, two localities were selected; one was treated with pesticide and second was untreated. Maize field visited by many insect pests. Those insect pests were collected by using three collection method: sweep net, pitfall trap and plant inspection. The data was collected weekly interval from August to October and statistically analyzed by using Shannon Index which showed the results of insect pest richness and evenness. The value of Shannon Index was higher with the increase in number of species and abundance of insects. Camponotus nearcticus was most abundant in sweep net and pitfall trap method while Rhopalosiphum maidis was abundant in plant inspection method. Temperature was negatively co-relate with the insect population in all three collection methods while the relative humidity and rainfall had varying results.

Keywords: abundance, evenness, maize, richness

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Authors: Zineddine Bouyahiaoui, Rabah Haoui

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The aim of this work is to analyze a flow around the axisymmetric blunt body taken into account the chemical and vibrational nonequilibrium flow. This work concerns the entry of spacecraft in the atmosphere of the planet Mars. Since the equations involved are non-linear partial derivatives, the volume method is the only way to solve this problem. The choice of the mesh and the CFL is a condition for the convergence to have the stationary solution.

Keywords: blunt body, finite volume, hypersonic flow, viscous flow

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Authors: Mozhgan Bahadory, Gholam-Hossein Rostami

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Over the next quarter of a century, the US government and the private sector will spend billions of dollars annually to clean the contaminated sites from pollution such as petroleum products, heavy metals, and solvents organic compounds. During the past three decades, almost 750,000 sites that require remediation have been reported to the United States federal and state agencies. Out of these contamination sites, approximately 300,000 are still in need of remediation. In these sites, the most widespread forms of contamination are petroleum products and heavy metals. At least half of US Department of Defense, US Department of Energy, Superfund sites, and Resource Conservation and Recovery Act (RCRA) sites have been reported to contain heavy metals. Heavy metals most often found in the contaminated water are lead, mercury, chromium, cadmium, arsenic, and zinc. This investigation emphasizes the elimination of arsenic and cadmium from aqueous solution. During the past several years, we developed a novel material called Alkali-Activated fly ash Material Permeable Reactive Barrier (AAM-PRB), which includes fly ash, fine aggregates, coarse aggregates, activating chemicals, and water. AAM can be produced with high permeability, 10-1 cm/s, then crushed into pelletized form. Laboratory experiments showed that water containing 10 ppm, 100 ppm, and 1000 ppm of arsenic and cadmium ion passing through AAM-PRB reduced to less than 0.1 ppm. However, water containing 10,000 ppm arsenic ion passing through AAM- PRB shows that the breakthrough was achieved. The removal of the mixture of arsenic and cadmium from aqueous solutions was also tested by using AAM-PRB. The results indicate that the efficiency of AAM-PRB for simultaneous removal of arsenic and cadmium from 10 ppm, 100 ppm, and 1,000 ppm were marginally below that of arsenic alone. Still, it was significantly lower for cadmium from the aqueous solution. The basic science behind removing heavy metal and microstructural investigation AAM-PRB will be the focus of our future work.

Keywords: arsenic, cadmium, contaminated water, fly ash, permeability, reactive barrier

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Authors: Sarah Ekuwo Okende, Armand Lokolo

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Gradually, the recognition of wild bees in processes affecting ecosystems and as major components of biodiversity has led to their protection as well as their areas in Kinshasa. And despite their decisive role in the well-being of men, the general public and decision-makers know nothing of the consequences of the loss of these, which are nevertheless of considerable magnitude. On this, they provide the pollination of sexual plants, and they also provide us with a number of goods that have a direct economic value, such as food, medicines, etc. And yet today, more than half of these wild bee species are threatened in Kinshasa. The causes of this phenomenon are largely unknown to the general public in the Kinshasa region. The objective of this study is to find the causes leading to the disappearance of wild bee species in Kinshasa. Also, this research contributes to current knowledge of the biodiversity of wild bees in the Kinshasa region and helps the authorities to develop a good policy for the conservation or safeguarding of this biodiversity, which plays a key role in maintaining the integrity of our ecosystems. We carried out field surveys using interview sheets in the forest areas of Kinshasa where wild bees populated them. To achieve this, an interview sheet was made, and it included questions on the causes of the disappearance of wild bees and the destruction of forest areas. The interviews were carried out with the natives of these forest areas. The results of this study show us that the destruction of habitats or natural areas and the use of pesticides are the causes of the disappearance of these wild bees.

Keywords: wild bees, pollinisation, forest, biodiversity, habitats, ecosystem, destruction, pesticide

Procedia PDF Downloads 91

Authors: Gerald Amatre, Julius Bunny Lejju, Morgan Andama

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Despite several interventions, jigger flea infestations continue to be reported in the Busoga sub-region in Eastern Uganda. The purpose of this study was to identify factors that expose the indigenous people to jigger flea infestations and evaluate the effectiveness of any indigenous materials used in flea control by the affected communities. Flea compositions in residences were described, factors associated with flea infestation and indigenous materials used in flea control were evaluated. Field surveys were conducted in the affected communities after obtaining preliminary information on jigger infestation from the offices of the District Health Inspectors to identify the affected villages and households. Informed consent was then sought from the local authorities and household heads to conduct the study. Focus group discussions were conducted with key district informants, namely, the District Health Inspectors, District Entomologists and representatives from the District Health Office. A GPS coordinate was taken at central point at every household enrolled. Fleas were trapped inside residences using Kilonzo traps. A Kilonzo Trap comprised a shallow pan, about three centimetres deep, filled to the brim with water. The edges of the pan were smeared with Vaseline to prevent fleas from crawling out. Traps were placed in the evening and checked every morning the following day. The trapped fleas were collected in labelled vials filled with 70% aqueous ethanol and taken to the laboratory for identification. Socio-economic and environmental data were collected. The results indicate that the commonest flea trapped in the residences was the cat flea (Ctenocephalides felis) (50%), followed by Jigger flea (Tunga penetrans) (46%) and rat flea (Xenopsylla Cheopis) (4%), respectively. The average size of residences was seven squire metres with a mean of six occupants. The residences were generally untidy; with loose dusty floors and the brick walls were not plastered. The majority of the jigger affected households were headed by peasants (86.7%) and artisans (13.3%). The household heads mainly stopped at primary school level (80%) and few at secondary school level (20%). The jigger affected households were mainly headed by peasants of low socioeconomic status. The affected community members use soil-cow dung-ash mixture to smear floors of residences as the only measure to control fleas. This method was found to be ineffective in controlling the insects. The study recommends that home improvement campaigns be continued in the affected communities to improve sanitation and hygiene in residences as one of the interventions to combat flea infestations. Other cheap, available and effective means should be identified to curb jigger flea infestations.

Keywords: cow dung-soil-ash mixture, infestations, jigger flea, Tunga penetrans

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Authors: Vilma Sasyte, Vilma Viliene, Asta Raceviciute-Stupeliene, Agila Dauksiene, Romas Gruzauskas, Virginijus Slausgalvis, Jamal Al-Saifi

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The aim of the present study was to investigate the effect of butyrate, acids, medium-chain fatty acids and plant extract mixture on performance, blood and gastrointestinal tract characteristics of laying hens’. For the period of 8 weeks, 24 Hisex Brown laying hens were randomly assigned to 2 dietary treatments: 1) control wheat-corn-soybean meal based diet (Control group), 2) control diet supplemented with the mixture of butyrate, acids, medium chain fatty acids and plant extract (Lumance®) at the level of 1.5 g/kg of feed (Experimental group). Hens were fed with a crumbled diet at 125 g per day. Housing and feeding conditions were the same for all groups and met the requirements of growth for laying hens of Hisex Brown strain. In the blood serum total protein, bilirubin, cholesterol, DTL- and MTL- cholesterol, triglycerides, glucose, GGT, GOT, GPT, alkaline phosphatase, alpha amylase, contents of c-reactive protein, uric acid, and lipase were analyzed. Development of intestines and internal organs (intestinal length, intestinal weight, the weight of glandular and muscular stomach, pancreas, heart, and liver) were determined. The concentration of short chain fatty acids in caecal content was measured using the method of HPLC. The results of the present study showed that 1.5 g/kg supplementation of feed additive affected egg production and feed conversion ratio for the production of 1 kg of egg mass. Dietary supplementation of analyzed additive in the diets increased the concentration of triglycerides, GOT, alkaline phosphatase and decreased uric acid content compared with the control group (P<0.05). No significant difference for others blood indices in comparison to the control was observed. The addition of feed additives in laying hens’ diets increased intestinal weight by 11% and liver weight by 14% compared with the control group (P<0.05). The short chain fatty acids (propionic, acetic and butyric acids) in the caecum of laying hens in experimental groups decreased compared with the control group. The supplementation of the mixture of butyrate, acids, medium-chain fatty acids and plant extract at the level of 1.5 g/kg in the laying hens’ diets had the effect on the performance, some gastrointestinal tract function and blood parameters of laying hens.

Keywords: acids, butyrate, laying hens, MCFA, performance, plant extract, psysiological state

Procedia PDF Downloads 296

Authors: Jean Yves Uwamungu, Fiston Bizimana, Chunsheng Hu

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Although pesticides are used in crop productivity, their use is highly harming the soil environment, and measures must be taken in the future to eradicate soil and groundwater pollution. The primary aim was to determine the effect of biochar addition on the imidacloprid adsorption on soil prior to no-tillage (NT) and rotational tillage (RT) conditions. In the laboratory, batch tests were conducted to determine the imidacloprid adsorption on soil using equilibrium and kinetic modelling with the addition of biochar. The clay level of the soil was found to be more significant when no-tillage was applied (22.42) than when rotational tillage was applied (14.27). The imidacloprid adsorption equilibrium was significantly shortened to 25 min after biochar addition. The isotherms and kinetic findings confirmed that the adsorption occurred according to Freundlich and pseudo-second-order kinetic models, respectively. The adsorption capacity of imidacloprid (40<35<25 °C) increased with decreasing temperature, indicating an exothermic adsorption behaviour, whereas negative Gibbs free energy (G) values of -6980.5 and 5983.93 Jmol-1, respectively, for soil prior to NT and RT at 25 °C, asserted spontaneous adsorption. The negative values of entropy (ΔS); -22.83 and -38.15 Jmol-1K-1, prior to NT and RT applications, respectively, described a lowered randomness process. The enthalpy was greater when RT was applied (-17533 J mol-1) than when NT was applied (-450 J mol-1). Lastly, it was shown that NTtreatment enhanced imidacloprid adsorption capacity more than RT treatment and that biochar addition enhanced pesticide adsorption in both treatments.

Keywords: adsorption, biochar, imidacloprid, soil, tillage

Procedia PDF Downloads 148

Authors: Esther Acha, Jose Cambra, De Chen

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Hydrogen is considered an important energy vector for the 21st century. Nowadays there are some difficulties for hydrogen economy implantation, and one of them is the high purity required for hydrogen. This energy vector is still being mainly produced from fuels, from wich hydrogen is produced as a component of a mixture containing other gases, such as CO, CO2 and H2O. A forthcoming sustainable pathway for hydrogen is steam-reforming of bio-oils derived from biomass, e.g. via fast pyrolysis. Bio-oils are a mixture of acids, alcohols, aldehydes, esters, ketones, sugars phenols, guaiacols, syringols, furans, multi-functional compounds and also up to a 30 wt% of water. The sorption enhanced steam reforming (SESR) process is attracting a great deal of attention due to the fact that it combines both hydrogen production and CO2 separation. In the SESR process, carbon dioxide is captured by an in situ sorbent, which shifts the reversible reforming and water gas shift reactions to the product side, beyond their conventional thermodynamic limits, giving rise to a higher hydrogen production and lower cost. The hydrogen containing mixture has been obtained from the SESR of bio-oil type compounds. Different types of catalysts have been tested. All of them contain Ni at around a 30 wt %. Two samples have been prepared with the wet impregnation technique over conventional (gamma alumina) and non-conventional (olivine) supports. And a third catalysts has been prepared over a hydrotalcite-like material (HT). The employed sorbent is a commercial dolomite. The activity tests were performed in a bench-scale plant (PID Eng&Tech), using a stainless steel fixed bed reactor. The catalysts were reduced in situ in the reactor, before the activity tests. The effluent stream was cooled down, thus condensed liquid was collected and weighed, and the gas phase was analysed online by a microGC. The hydrogen yield, and process behavior was analysed without the sorbent (the traditional SR where a second purification step will be needed but that operates in steady state) and the SESR (where the purification step could be avoided but that operates in batch state). The influence of the support type and preparation method will be observed in the produced hydrogen yield. Additionally, the stability of the catalysts is critical, due to the fact that in SESR process sorption-desorption steps are required. The produced hydrogen yield and hydrogen purity has to be high and also stable, even after several sorption-desorption cycles. The prepared catalysts were characterized employing different techniques to determine the physicochemical properties of the fresh-reduced and used (after the activity tests) materials. The characterization results, together with the activity results show the influence of the catalysts preparation method, calcination temperature, or can even explain the observed yield and conversion.

Keywords: CO2 sorbent, enhanced steam reforming, hydrogen

Procedia PDF Downloads 579

Authors: Sameh A. S. Thabit Alariqi

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Food is widely packaged with plastic materials to prevent microbial contamination and spoilage. Ionizing radiation is widely used to sterilize the food-packaging materials. Sterilization by γ-radiation causes degradation for the plastic packaging materials such as embrittlement, stiffening, softening, discoloration, odour generation, and decrease in molecular weight. Many antioxidants can prevent γ-degradation but most of them are toxic. The migration of antioxidants to its environment gives rise to major concerns in case of food packaging plastics. In this attempt, we have aimed to utilize synergistic mixtures of stabilizers which are approved for food-contact applications. Ethylene-propylene-diene terpolymer (EPDM) have been melt-mixed with hindered amine stabilizers (HAS), phenolic antioxidants and organo-phosphites (hydroperoxide decomposer). Results were discussed by comparing the stabilizing efficiency of mixtures with and without phenol system. Among phenol containing systems where we mostly observed discoloration due to the oxidation of hindered phenol, the combination of secondary HAS, tertiary HAS, organo-phosphite and hindered phenol exhibited improved stabilization efficiency than single or binary additive systems. The mixture of secondary HAS and tertiary HAS, has shown antagonistic effect of stabilization. However, the combination of organo-phosphite with secondary HAS, tertiary HAS and phenol antioxidants have been found to give synergistic even at higher doses of -sterilization. The effects have been explained through the interaction between the stabilizers. After γ-irradiation, the consumption of oligomeric stabilizer significantly depends on the components of stabilization mixture. The effect of the organo-phosphite antioxidant on the overall stability has been discussed.

Keywords: ethylene-propylene-diene terpolymer, synergistic mixtures, gamma sterilization, gamma stabilization

Procedia PDF Downloads 440

Authors: Esa Abiso Godana, Qiya Yang, Kaili Wang, Zhang Hongyin, Xiaoyun Zhang, Lina Zhao

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Blue mold decay caused by Penicillium expansum is among the recent identified diseases of grapes (Vitis vinifera). The increasing concern about use of chemical substance and pesticide in postharvest fruit push the trends of research toward biocontrol strategies which are more sustainable and ecofriendly. In this study, we determined the biocontrol efficacy of Pichia anomala alone and supplemented with 1% chitosan in the grapefruit against blue mold disease caused by P. expansum. The result showed that 1% chitosan better enhances the biocontrol efficacy P. anomala. Chitosan (1% w/v) also improved the number of population of P. anomala in grape wounds, surface and on nutrient yeast dextrose broth (NYDB). P. anomala supplemented with 1% w/v chitosan significantly reduced the disease incidence, lesion diameter and natural decay of grapefruits without affecting the fruit quality as compared to the control. The scanned electron microscope (SEM) concisely illustrates how the high number of yeast cells on the wounds reduced the growth of P. expansum. P. anomala alone or P. anomala supplemented with 1% w/v chitosan are presented as a potential biocontrol alternative against the postharvest blue mold of grapefruit.

Keywords: biocontrol, Pichia anomala, chitosan, Penicillium expansum, grape

Procedia PDF Downloads 114

Authors: Awadhesh Kishore

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The goal of the study was to determine how different non-metallic nutrients are partitioned from feed in various physiological contexts and how buffer addition in ruminant nutrition affects these processes. Six lactating crossbred dairy cows were selected and divided into three groups on the basis of their phenotypic and productive features (374±14 kg LW). Two treatments, T1 and T2, were randomly assigned to one animal from each group. Animals under T1 and T2 were moved to T2 and T1, respectively, after 30 days. T2 was the only group to receive buffers containing magnesium oxide and sodium bicarbonate at 0.0 and 0.01% of LW (the real amounts are equivalent to 75.3±4.0 and 30 7.7±2.0 g/d, respectively). T1 was used as the control. Wheat straw and berseem were part of the base diet, whereas wheat grain and mustard cake were part of the concentrate mixture. Following a 21-day feeding period, metabolic and milk production trials were carried out for seven consecutive days. The Kearl equation used the urine's calorific value to determine its volume. Chemical analyses were performed to determine the levels of nitrogen, carbohydrates, calories, and phosphorus in samples of feed, waste, buffer, mineral mixture, water, feces, urine, and milk that were collected. The information was analyzed statistically. Notable results included decreased nitrogen and carbohydrate partitioning to feces from feed, while increased calorie partitioning to milk and body storage, and increased carbohydrate partitioning to body storage. Phosphorus balance was significantly better in T2. The application of buffers in ruminant diets was found to increase the output of calories in milk, as well as the number of calories and carbohydrates stored in the body, while decreasing the amount of nitrogen in faeces. As a result, it may be advised to introduce buffers to feed crossbred dairy cattle.

Keywords: cattle, Magnesium oxide, non-metallic nutrients, partitioning, Sodium bicarbonate

Procedia PDF Downloads 58

Authors: Hyuk-Hoon Kim, Young Gi Min

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Background: Acute poisoning is the common cause of morbidity and mortality. Characteristics of acute poisoning differ between countries. While other countries operate the database system for poisoning, Korea has not collected the database for acute poisoning. Distribution of incidence of acute poisoning depending on the types of materials have also not studied in Korea. Our aims are to evaluate the etiologic and demographic characteristics of acute poisoning cases and to obtain up-to-date information on acute poisonings. Method: We retrospectively recorded cases of acute poisoning from eight emergency departments of second level or university hospitals from different cities in Gyeonggi province in Korea from April 2006 and March 2015. The distributions of incidence of acute poisoning depending on the types of materials are mapped by geographic information system. Result: A total of 3,449 poisoned cases were analyzed. Mean estimated age of patients was 39.56 ± 22.40 years. Mean male to female ratio of patients was 1:1.4. Mean proportion of intentional poisoning was 57.9%. Common materials are benzodiazepine (16.6%), carbon monoxide (10.5%), pesticide (8.1%) and zolpidem (7.1%) Common route of exposure is ingestion (79.5%) and followed by inhalation (16.5%). Common treatment methods are gastric lavage (20%) and activated charcoal (30%). Most cases had uneventful recovery; 61.4% were treated as outpatients and 0.1% of the poisoning resulted in death in ER. Conclusion: Even though the cases enrolled in our study is not the overall cases of acute poisoning in Korea, our study could be the basis of countermeasures for analysis and prevention of acute poisoning in Korea.

Keywords: acute poisoning, emergency department, epidemiology, Korea

Procedia PDF Downloads 403

Authors: Pedro J. Rolim-Neto, Leslie R. M. Ferraz, Fabiana L. A. Santos, Pablo A. Ferreira, Ricardo T. L. Maia-Jr., Magaly A. M. Lyra, Danilo A F. Fonte, Salvana P. M. Costa, Amanda C. Q. M. Vieira, Larissa A. Rolim

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Initially developed as an antimalarial agent, hydroxychloroquine (HCQ) sulfate is often used as a slow-acting antirheumatic drug in the treatment of disorders of connective tissue. The United States Pharmacopeia (USP) 37 provides a reversed-phase HPLC method for quantification of HCQ. However, this method was not reproducible, producing asymmetric peaks in a long analysis time. The asymmetry of the peak may cause an incorrect calculation of the concentration of the sample. Furthermore, the analysis time is unacceptable, especially regarding the routine of a pharmaceutical industry. The aiming of this study was to develop a fast, easy and efficient method for quantification of HCQ sulfate by High Performance Liquid Chromatography (HPLC) based on the Quality by Design (QbD) methodology. This method was optimized in terms of peak symmetry using the surface area graphic as the Design of Experiments (DoE) and the tailing factor (TF) as an indicator to the Design Space (DS). The reference method used was that described at USP 37 to the quantification of the drug. For the optimized method, was proposed a 33 factorial design, based on the QbD concepts. The DS was created with the TF (in a range between 0.98 and 1.2) in order to demonstrate the ideal analytical conditions. Changes were made in the composition of the USP mobile-phase (USP-MP): USP-MP: Methanol (90:10 v/v, 80:20 v/v and 70:30 v/v), in the flow (0.8, 1.0 and 1.2 mL) and in the oven temperature (30, 35, and 40ºC). The USP method allowed the quantification of drug in a long time (40-50 minutes). In addition, the method uses a high flow rate (1,5 mL.min-1) which increases the consumption of expensive solvents HPLC grade. The main problem observed was the TF value (1,8) that would be accepted if the drug was not a racemic mixture, since the co-elution of the isomers can become an unreliable peak integration. Therefore, the optimization was suggested in order to reduce the analysis time, aiming a better peak resolution and TF. For the optimization method, by the analysis of the surface-response plot it was possible to confirm the ideal setting analytical condition: 45 °C, 0,8 mL.min-1 and 80:20 USP-MP: Methanol. The optimized HPLC method enabled the quantification of HCQ sulfate, with a peak of high resolution, showing a TF value of 1,17. This promotes good co-elution of isomers of the HCQ, ensuring an accurate quantification of the raw material as racemic mixture. This method also proved to be 18 times faster, approximately, compared to the reference method, using a lower flow rate, reducing even more the consumption of the solvents and, consequently, the analysis cost. Thus, an analytical method for the quantification of HCQ sulfate was optimized using QbD methodology. This method proved to be faster and more efficient than the USP method, regarding the retention time and, especially, the peak resolution. The higher resolution in the chromatogram peaks supports the implementation of the method for quantification of the drug as racemic mixture, not requiring the separation of isomers.

Keywords: analytical method, hydroxychloroquine sulfate, quality by design, surface area graphic

Procedia PDF Downloads 639