Search results for: acid pretreatment

Authors: Ashish Bohre, Blaž Likozar, Saikat Dutta, Dionisios G. Vlachos, Basudeb Saha

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Graphene oxide, decorated with surface oxygen functionalities, has emerged as a sustainable alternative to precious metal catalysts for many reactions. Herein, we report for the first time that graphene oxide becomes super active for C-C coupling upon incorporation of multilayer crystalline features, highly oxidized surface, Brønsted acidic functionalities and defect sites on the surface and edges via modified oxidation. The resulting improved graphene oxide (IGO) demonstrates superior activity to commonly used framework zeolites for upgrading of low carbon biomass furanics to long carbon chain aviation fuel precursors. A maximum 95% yield of C15 fuel precursor with high selectivity is obtained at low temperature (60 C) and neat conditions via hydroxyalkylation/alkylation (HAA) of 2-methylfuran (2-MF) and furfural. The coupling of 2-MF with carbonyl molecules ranging from C3 to C6 produced the precursors of carbon numbers 12 to 21. The catalyst becomes inactive in the 4th cycle due to the loss of oxygen functionalities, defect sites and multilayer features; however, regains comparable activity upon regeneration. Extensive microscopic and spectroscopic characterization of the fresh and reused IGO is presented to elucidate high activity of IGO and to establish a correlation between activity and surface and structural properties. Kinetic Monte Carlo (KMC) and density functional theory (DFT) calculations are presented to further illustrate the surface features and the reaction mechanism.

Keywords: methacrylic acid, itaconic acid, biomass, monomer, solid base catalyst

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Authors: Gowri Balaji, Muthusamy Nachiyappan, Ramalingam Venugopal

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Amongst the wide spectrum of pesticides, pyrethroids are preferably used rather than organochlorine, organophosphorous and carbamates pesticides due to their high effectiveness. Synthetic pyrethroids which are the chemicals used for the pest control in agriculture are now being excessively used in India. The aim of the present study was to evaluate the adverse effect of cypermethrin on the fresh water fish Cyprinus carpio, the common carp. The effect was assessed by comparing the biochemical parameters in the blood and liver tissues of control fishes with three experimental group of fishes exposed with cypermethrin for 7 days 1/15 Lc50 (E1) 1/10 Lc50 (E2) and 1/5 Lc50 values (E3). After 7 days of exposure, blood was collected and liver and gills was dissected out. The activities of acid phosphatase, alkaline phosphatase, lactate dehydrogenase, aspartate aminotransferase and alanine aminotransferase were estimated by standard spectrophotometric techniques in the blood, liver and gills tissue homogenate. Lactate dehydrogenase was significantly decreased in E2 and E3 experimental groups. The activities of acid phosphatase, alkaline phosphatase, aspartate aminotransferase and alanine aminotransferase were significantly altered in the experimental groups. All the biochemical parameters studied were adversely affected in the liver and gills of cypermethrin exposed fish. The results obtained from the present study of cypermethrin exposed fishes indicate a marked toxic effect of cypermethrin and also its dose dependent impact on different organs of the fish.

Keywords: cypermethrin, Cyprinus carpio, ALT, AST, LDH, liver, gills

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Authors: Jannika Dombrowski, Sabine Ambros, Ulrich Kulozik

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Several drying techniques are used to preserve sensitive substances such as probiotic lactic acid bacteria. With the aim to better understand differences between these processes, this work gives new insights into structural variations resulting from different preservation methods and their impact on product quality and storage stability. Industrially established methods (freeze drying, spray drying) were compared to upcoming vacuum, microwave-freeze, and microwave-vacuum drying. For freeze and microwave-freeze dried samples, survival and activity maintained 100%, whereas vacuum and microwave-vacuum dried cultures achieved 30-40% survival. Spray drying yielded in lowest viability. The results are directly related to temperature and oxygen content during drying. Interestingly, most storage stable products resulted from vacuum and microwave-vacuum drying due to denser product structures as determined by helium pycnometry and SEM images. Further, lower water adsorption velocities were responsible for lower inactivation rates. Concluding, resulting product structures as well as survival rates and storage stability mainly depend on the type of water removal instead of energy input. Microwave energy compared to conductive heating did not lead to significant differences regarding the examined factors. Correlations could be proven for three investigated microbial strains. The presentation will be completed by an overview on the energy efficiency of the presented methods.

Keywords: drying techniques, energy efficiency, lactic acid bacteria, probiotics, survival rates, structure characterization

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Authors: Luz Stella Cadavid-Rodriguez, Viviana E. Castro-Lopez

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Fish waste (FW) has a high content of potentially biodegradable components, so it is amenable to be digested anaerobically. In this line, anaerobic digestion (AD) of FW has been studied for biogas production. Nevertheless, intermediate products such as volatile fatty acids (VFA), generated during the acidogenic stage, have been scarce investigated, even though they have a high potential as a renewable source of carbon. In the literature, there are few studies about the Inoculum-Substrate (I/S) ratio on acidogenesis. On the other hand, it is well known that pH is a critical factor in the production of VFA. The optimum pH for the production of VFA seems to change depending on the substrate and can vary in a range between 5.25 and 11. Nonetheless, the literature about VFA production from protein-rich waste, such as FW, is scarce. In this context, it is necessary to deepen on the determination of the optimal operating conditions of acidogenic fermentation for VFA production from protein-rich waste. Therefore, the aim of this research was to optimize the volatile fatty acid production from artisanal fishing waste, studying the effect of pH and the I/S ratio on the acidogenic process. For this research, the inoculum used was a methanogenic sludge (MS) obtained from a UASB reactor treating wastewater of a slaughterhouse plant, and the FW was collected in the port of Tumaco (Colombia) from the local artisanal fishers. The acidogenic fermentation experiments were conducted in batch mode, in 500 mL glass bottles as anaerobic reactors, equipped with rubber stoppers provided with a valve to release biogas. The effective volume used was 300 mL. The experiments were carried out for 15 days at a mesophilic temperature of 37± 2 °C and constant agitation of 200 rpm. The effect of 3 pH levels: 5, 7, 9, coupled with five I/S ratios, corresponding to 0.20, 0.15, 0.10, 0.05, 0.00 was evaluated taking as a response variable the production of VFA. A complete randomized block design was selected for the experiments in a 5x3 factorial arrangement, with two repetitions per treatment. At the beginning and during the process, pH in the experimental reactors was adjusted to the corresponding values of 5, 7, and 9 using 1M NaOH or 1M H2SO4, as was appropriated. In addition, once the optimum I/S ratio was determined, the process was evaluated at this condition without pH control. The results indicated that pH is the main factor in the production of VFA, obtaining the highest concentration with neutral pH. By reducing the I/S ratio, as low as 0.05, it was possible to maximize VFA production. Thus, the optimum conditions found were natural pH (6.6-7.7) and I/S ratio of 0.05, with which it was possible to reach a maximum total VFA concentration of 70.3 g Ac/L, whose major components were acetic acid (35%) and butyric acid (32%). The findings showed that the acidogenic fermentation of FW is an efficient way of producing VFA and that the operating conditions can be simple and economical.

Keywords: acidogenesis, artisanal fishing waste, inoculum to substrate ratio, volatile fatty acids

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Authors: Vesna Tumbas Šaponjac, Sonja Djilas, Jasna Čanadanović-Brunet, Gordana Ćetković, Jelena Vulić, Slađana Stajčić, Milica Vinčić

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Substantial interest has been expressed in fruits and berries due to their potential favourable health effects and high content of polyphenols, especially flavonoids and anthocyanins. Chokeberries (Aronia melanocarpa) are dark berries, similar to blackcurrants, that have been used by native Americans both as a food resource and in traditional medicine for treatment of cold. Epidemiological studies revealed positive effects of chokeberries on colorectal cancer, cardiovascular diseases, and various inflammatory conditions. Chokeberries are well known as good natural antioxidants, which contain phenolic compounds, flavonoids, anthocyanidins and antioxidant vitamins. The aim of this study was to provide information on polyphenolic compounds present in fresh chokeberries as well as to determine its antioxidant activity. Individual polyphenolic compounds have been identified and quantified using HPLC/UV-Vis. Results showed that the most dominant phenolic acid was protocatechuic acid (274.23 mg/100 g FW), flavonoid rutin (319.66 mg/100 g FW) and anthocyanin cyanidin-3-galactoside (1532.68 mg/100 g FW). Generally, anthocyanins were predominant compounds in fresh chokeberry (2342.82 mg/100 g FW). Four anthocyanins have been identified in fresh chokeberry and all of them were cyanidin glicosides. Antioxidant activity was determined using spectrophotometric DPPH assay and compared to standard antioxidant compound vitamin C. The resulting EC50 value (amount of fresh chokeberries that scavenge 50% of DPPH radicals) is 0.33 mg vitamin C equivalent/100 g FW. The results of this investigation provide evidence on high contents of phenolic compounds, especially anthocyanins, in chokeberries as well as high antioxidant activity of this fruit.

Keywords: chokeberry, polyphenols, antioxidant, DPPH radicals

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Authors: Moulay Driss Mellaoui, Abdallah Imjjad, Rachid Boutiddar, Haydar Mohammad-Salim, Nivedita Acharjee, Hassan Bourzi, Souad El Issami, Khalid Abbiche, Hanane Zejli

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We have investigated the underlying molecular processes involved in the [3+2] cycloaddition (32CA) reactions between N-methyl-C-(2-furyl) nitrone and three acetylene derivatives: 4b, 5b, and 6b. For this investigation, we utilized molecular electron density theory (MEDT) and density functional theory (DFT) methods at the B3LYP-D3/6 31G (d) computational level. These 32CA reactions, which exhibit a zwitterionic (zw-type) nature, proceed through a one-step mechanism with activation enthalpies ranging from 8.80 to 14.37 kcal mol−1 in acetonitrile and ethanol solvents. When the nitrone reacts with phenyl methyl propiolate (4b), two regioisomeric pathways lead to the formation of two products: P1,5-4b and P1,4-4b. On the other hand, when the nitrone reacts with dimethyl acetylene dicarboxylate (5b) and acetylene dicarboxylic acid (but-2-ynedioic acid) (6b), it results in the formation of a single product. Through topological analysis, we can categorize the nitrone as a zwitterionic three-atom component (TAC). Furthermore, the analysis of conceptual density functional theory (CDFT) indices classifies the 32CA reactions of the nitrone with 4b, 5b, and 6b as forward electron density flux (FEDF) reactions. The study of bond evolution theory (BET) reveals that the formation of new C-C and C-O covalent bonds does not initiate in the transition states, as the intermediate stages of these reactions display pseudoradical centers of the atoms already involved in bonding.

Keywords: 4-isoxazoline, DFT/B3LYP-D3, regioselectivity, cycloaddition reaction, MEDT, ELF

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Authors: S. M. Shahinul Islam, Israt Ara, Narendra Tuteja, Sreeramanan Subramaniam

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Through anther and microspore culture methods, complete homozygous plants can be produced within a year as compared to the long inbreeding method. Isolated microspore culture is one of the most important techniques for rapid development of haploid plants. The efficiency of this method is influenced by several factors such as cultural conditions, growth regulators, plant media, pretreatments, physical and growth conditions of the donor plants, pollen isolation procedure, etc. The main purpose of this study was to improve the isolated microspore culture protocol in order to increase the efficiency of embryoids, its regeneration and reducing albinisms. Under this study we have tested mainly three different microspore isolation procedures by glass rod, homozeniger and by blending and found the efficiency on gametic embryogenesis. There are three types of media viz. washing, pre-culture and induction was used. The induction medium as AMC (modified MS) supplemented by 2, 4-D (2.5 mg/l), kinetin (0.5 mg/l) and higher amount of D-Manitol (90 g/l) instead of sucrose and two types of amino acids (L-glutamine and L-serine) were used. Out of three main microspore isolation procedure by homogenizer isolation (P4) showed best performance on ELS induction (177%) and green plantlets (104%) compared with other techniques. For all cases albinisims occurred but microspore isolation from excised anthers by glass rod and homogenizer showed lesser numbers of albino plants that was also one of the important findings in this study.

Keywords: androgenesis, pretreatment, microspore culture, regeneration, albino plants, Oryza sativa

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Authors: Hasan Basri Jumin, Danil Endriand Basri

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Isolated protoplast from embryogenic callus of orange Jessamine (Murraya paniculata L. (Jack) cultured and maintained under growth chamber at the temperature +25oC. The parameter observed are the plating efficiency, the number of spherical embryos, heard-shaped embryos-like structure, shoot formation, and plantlets obtained. Treatment was arranged with 0.0, 0.001, 0.01, 0.1 or 1.0 mg 1-1 Naphthalene acetic acid (NAA), and 0, 300, 500 mg 1/l malt extract (ME) and 0.M sorbitol in the medium with 2.5 % sucrose. Interaction between 0.001 mg/l NAA and 500 mg/l was observed the higher percentage of planting efficiency. For embryo development from callus, the media was added to 0.0 mg/l, 0.001 mg/l, 0.01 ,mg/l, 0.1 mg/l, 1.0 mg/l NAA, and 1.0 %, 2.0 %, 3.0 %, 4.0 % sucrose. Media supplemented with 0.01mg/l NAA, and 1.0% sucrose was found to be a suitable medium for the development of spherical somatic embryos. A combination of 0.1 mg/ indole acetic acid (IAA) and 0.1 mg/l zeatin constituted the spherical somatic embryo became heart-shaped embryos-like structure. A combination between GA3 0.1 mg 1/l GA3 and 0.1 mg 1-1 zeatin is looking high, growing the heart-shaped embryos-like structure to form a shoot. Cells were developed into spherical embryos and grew into heart-shaped embryos, and then spherical somatic embryos developed into shoot formation. Sequence from single protoplast to plantlets was obtained by using a low concentration of plant growth regulator and sucrose; This recovery of single protoplast to be completed plantlets is a new technology in plant cell culture, and this could be used in genetic engineering in citrus.

Keywords: heart-shaped-embryos-like-structure, Muraya-paniculata, plant-growth-regulator, spherical- somatic-embryo, single protoplast, glucose

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Authors: O. Adjroud

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The present study was conducted to investigate the interaction between selenium (Se) and chloride nickel (NiCl2) on energy profiles in Wistar albino preimplanted rats. NiCl2 was given on day 3 of pregnancy either in distilled drinking water at a dose of 20 mg/L/day for 16 consecutive days or as a single subcutaneous (s.c.) dose of 25, 50, or 100 mg/kg. Se was given as a s.c. injection (0.3 mg/kg) together with the higher dose (100 mg/kg) of NiCl2. Changes in energy profiles were evaluated in treated and control groups on days 5 and 20 of gestation. NiCl2 s.c. induced a significant increase in plasma glucose on day 20 of pregnancy. NiCl2 s.c. induced on day 5 and 20 of gestation a significant decrease in plasma triglycerides, with the higher dose. This decrease was maintained at day 20 of gestation with doses of 50 mg /kg. In addition, NiCl2 s.c. caused on day 5 of gestation a significant decrease in plasma total cholesterol with the low and medium doses. The pretreatment with Se reversed the effects of NiCl2 on plasma glucose, total cholesterol and triglycerides levels. NiCl2 administered in the drinking water augmented significantly the plasma triglycerides and total cholesterol levels and slighty the plasma glucose on day 20 of gestation, while on day 5 of gestation NiCl2 s.c. Induced a significant decrease in cholesterol. Three doses of NiCl2 (sc) induced severe alterations in liver and architecture which are markedly improved by Selenium. These results suggested that selenium has protective effects on energy profiles against the toxicity induced by NiCl2 administered subcutaneously in preimplanted rats.

Keywords: hepatotoxicity, nickel chloride, preimplanted rat, biochemical parameters

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Authors: Zakia Belhadj, Bing He, Hua Zhang, Xueqing Wang, Wenbing Dai, Qiang Zhang

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Mononuclear phagocyte system (MPS) forms an abominable obstacle hampering the tumor delivery efficiency of nanoparticles. Passively targeted nanocarriers have received clinical approval over the past 20 years. However, none of the actively targeted nanocarriers have entered clinical trials. Thus it is important to endue effective targeting ability to actively targeted approaches by overcoming biological barriers to nanoparticle drug delivery. Here, it presents that an Esomeprazole-based preconditioning strategy for regulating nanocarrier-MPS interaction to substantially prolong circulation time and enhance tumor targeting of nanoparticles. In vitro, the clinically approved proton pump inhibitor Esomeprazole “ESO” was demonstrated to reduce interactions between macrophages and subsequently injected targeted vesicles by interfering with their lysosomal trafficking. Of note, in vivo studies demonstrated that ESO pretreatment greatly decreased the liver and spleen uptake of c(RGDm7)-modified vesicles, highly enhanced their tumor accumulation, thereby provided superior therapeutic efficacy of c(RGDm7)-modified vesicles co-loaded with Doxorubicin (DOX) and Gefitinib (GE). This MPS-preconditioning strategy using ESO provides deeper insights into regulating nanoparticles interaction with the phagocytic system and enhancing their cancer cells' accessibility for anticancer therapy.

Keywords: esomeprazole (ESO), mononuclear phagocyte system (MPS), preconditioning strategy, targeted lipid vesicles

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Authors: Flackson Tshuma, James Bennett, Pieter Andreas Swanepoel, Johan Labuschagne, Stephan van der Westhuizen, Francis Rayns

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Amongst other things, tillage and synthetic agrochemicals can be effective methods of seedbed preparation and pest control. Nonetheless, frequent and intensive tillage and excessive application of synthetic agrochemicals, such as herbicides and insecticides, can reduce soil microbial enzyme activity. A decline in soil microbial enzyme activity can negatively affect nutrient cycling and crop productivity. In this study, the effects of four tillage treatments; continuous mouldboard plough; shallow tine-tillage to a depth of about 75 mm; no-tillage; and tillage rotation (involving shallow tine-tillage once every four years in rotation with three years of no-tillage), and two rates of synthetic agrochemicals (standard: with regular application of synthetic agrochemicals; and reduced: fewer synthetic agrochemicals in combination with bio-chemicals/ or bio-stimulants) on soil microbial enzyme activity were investigated between 2018 and 2020 in a typical Mediterranean climate zone in South Africa. Four different bio-stimulants applied contained: Trichoderma asperellum, fulvic acid, silicic acid, and Nereocystis luetkeana extracts, respectively. The study was laid out as a complete randomised block design with four replicated blocks. Each block had 14 plots, and each plot measured 50 m x 6 m. The study aimed to assess the combined impact of tillage practices and reduced rates of synthetic agrochemical application on soil microbial enzyme activity in a dryland cropping system. It was hypothesised that the application of bio-stimulants in combination with minimum soil disturbance will lead to a greater increase in microbial enzyme activity than the effect of applying either in isolation. Six soil cores were randomly and aseptically collected from each plot for microbial enzyme activity analysis from the 0-150 mm layer of a field trial under a dryland crop rotation system in the Swartland region. The activities of four microbial enzymes, β-glucosidase, acid phosphatase, alkaline phosphatase and urease, were assessed. The enzymes are essential for the cycling of glucose, phosphorus, and nitrogen, respectively. Microbial enzyme activity generally increased with a reduction of both tillage intensity and synthetic agrochemical application. The use of the mouldboard plough led to the least (P<0.05) microbial enzyme activity relative to the reduced tillage treatments, whereas the system with bio-stimulants (reduced synthetic agrochemicals) led to the highest (P<0.05) microbial enzyme activity relative to the standard systems. The application of bio-stimulants in combination with reduced tillage, particularly no-tillage, could be beneficial for enzyme activity in a dryland farming system.

Keywords: bio-stimulants, soil microbial enzymes, synthetic agrochemicals, tillage

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Authors: Sameh A. S. Thabit Alariqi

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Our previous studies aimed to investigate the biodegradation of γ-sterilized polyolefins in composting and microbial culture environments at different doses and γ-dose rates. It was concluded from the previous studies that the pretreatment of γ-irradiation can accelerate the biodegradation of neat polymer matrix in biotic conditions significantly. A similar work was carried out to study the stabilization of γ-sterilized polyolefins using different mixtures of stabilizers which are approved for food-contact applications. Ethylene-propylene (EP) copolymer has been melt-mixed with hindered amine stabilizers (HAS), phenolic antioxidants and hydroperoxide decomposers. Results were discussed by comparing the stabilizing efficiency, combination and consumption of stabilizers and the synergistic and antagonistic effects was explained through the interaction between the stabilizers. In this attempt, we have aimed to study the influence of the synergistic and antagonistic mixtures of oligomeric stabilizers on the biodegradation of the γ-irradiated polyolefins in composting and microbial culture. Neat and stabilized films of EP copolymer irradiated under γ-radiation and incubated in compost and fungal culture environments. The changes in functional groups, surface morphology, mechanical properties and intrinsic viscosity in polymer chains were characterized by FT-IR spectroscopy, SEM, instron, and viscometric measurements respectively. Results were discussed by comparing the effect of different stabilizers, stabilizers mixtures on the biodegradation of the γ-irradiated polyolefins. It was found that the biodegradation significantly depends on the components of stabilization system, mobility, interaction, and consumption of stabilizers.

Keywords: biodegradation, γ-irradiation, polyolefins, stabilization

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Authors: Harald Lindorfer, Bettina Frauz, Dietmar Ramhold

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Next to the well-known inhibitors in anaerobic digestion like ammonia, antibiotics or disinfectants, the number of process failures connected with mould growth in the feedstock increased significantly in the last years. It was assumed that mycotoxins are the cause of the negative effects. The financial damage to plants associated with these process failures is considerable. The aim of this study was to find a way of predicting the failures and furthermore strategies for a fast process recovery. In a first step, mould-contaminated feedstocks causing process failures in full-scale digesters were sampled and analysed on mycotoxin content. A selection of these samples was applied to biological inhibition tests. In this test, crystalline cellulose is applied in addition to the feedstock sample as standard substrate. Affected digesters were also sampled and analytical process data as well as operational data of the plants were recorded. Additionally, different mycotoxin substances, Deoxynivalenol, Zearalenon, Aflatoxin B1, Mycophenolic acid and Citrinin, were applied as pure substances to lab-scale digesters, individually and in various combinations, and effects were monitored. As expected, various mycotoxins were detected in all of the mould-contaminated samples. Nevertheless, inhibition effects were observed with only one of the collected samples, after applying it to an inhibition test. With this sample, the biogas yield of the standard substrate was reduced by approx. 20%. This result corresponds with observations made on full-scale plants. However, none of the tested mycotoxins applied as pure substance caused a negative effect on biogas production in lab scale digesters, neither after application as individual substance nor in combination. The recording of the process data in full-scale plants affected by process failures in most cases showed a severe accumulation of fatty acids alongside a decrease in biogas production and methane concentration. In the analytical data of the digester samples, a typical distribution of fatty acids with exceptionally high acetic acid concentrations could be identified. This typical fatty acid pattern can be used as a rapid identification parameter pointing to the cause of the process troubles and enable a fast implication of countermeasures. The results of the study show that more attention needs to be paid to feedstock storage and feedstock conservation before their application to anaerobic digesters. This is all the more important since first studies indicate that the occurrence of mycotoxins will likely increase in Europe due to the ongoing climate change.

Keywords: Anaerobic digestion, Biogas, Feedstock conservation, Fungal mycotoxins, Inhibition, process failure

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Authors: Benchouala Amira, Bojic Clement, Poupin Pascal, Cossu Leguille-carole

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The objective of this study is to evaluate in vitro the cytotoxic and androgenic potential of several antifungal molecules (amphotericin B, econazole, ketoconazole and miconazole) on MDA-Kb2 cell lines. This biological model is an effective tool for the detection of endocrine disruptors because it responds well to the main agonist of the androgen receptor (testosterone) and also to an antagonist: flutamide. The cytotoxicity of each chemical compound tested was measured using an MTT assay (tetrazolium salt, 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide) which measures the activity of the reductase function of mitochondrial succinate dehydrogenase enzymes of cultured cells. This complementary cytotoxicity test is essential to ensure that the effects of reduction in luminescence intensity observed during androgenic tests are only attributable to the anti-androgenic action of the compounds tested and not to their possible cytotoxic properties. Tests of the androgenic activity of antifungals show that these compounds do not have the capacity to induce transcription of the luciferase gene. These compounds do not exert an androgenic effect on MDA-Kb2 cells in culture for the environmental concentrations tested. The addition of flutamide for the same tested concentrations of antifungal molecules reduces the luminescence induced by amphotericin B, econazole and miconazole, which is explained by a strong interaction of these molecules with flutamide which may have a greater toxic effect than when tested alone. The cytotoxicity test shows that econazole and ketoconazole can cause cell death at certain concentrations tested. This cell mortality is perhaps induced by a direct or indirect action on deoxyribonucleic acid (DNA), ribonucleic acid (RNA) or proteins necessary for cell division.

Keywords: cytotoxicity, androgenic potential, antifungals, MDA-Kb2

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Authors: Fangyan Li, Lin Min Lee, Hui Zhu Peh, Shoet Harn Chan

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Advantame, a derivative of aspartame, is the latest addition to a family of low caloric and high potent dipeptide sweeteners which include aspartame, neotame and alitame. The use of advantame as a high-intensity sweetener in food was first accepted by Food Standards Australia New Zealand in 2011 and subsequently by US and EU food authorities in 2014, with the results from toxicity and exposure studies showing advantame poses no safety concern to the public at regulated levels. To our knowledge, currently there is barely any detailed information on the analytical method of advantame in food matrix, except for one report published in Japanese, stating a high performance liquid chromatography (HPLC) and liquid chromatography/ mass spectrometry (LC-MS) method with a detection limit at ppm level. However, the use of acid in sample preparation and instrumental analysis in the report raised doubt over the reliability of the method, as there is indication that stability of advantame is compromised under acidic conditions. Besides, the method may not be suitable for analyzing food matrices containing advantame at low ppm or sub-ppm level. In this presentation, a simple, specific and sensitive method for the determination of advantame in food is described. The method involved extraction with water and clean-up via solid phase extraction (SPE) followed by detection using liquid chromatography tandem mass spectrometry (LC-MS/MS) in negative electrospray ionization mode. No acid was used in the entire procedure. Single laboratory validation of the method was performed in terms of linearity, precision and accuracy. A low detection limit at ppb level was achieved. Satisfactory recoveries were obtained using spiked samples at three different concentration levels. This validated method could be used in the routine inspection of the advantame level in food.

Keywords: advantame, food, LC-MS/MS, sweetener

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Authors: Kazem Shakouri, Alireza Pishgahi, Homayoun Sadeghi-bBazargani, Shahla Dareshiri

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Introduction: Carpal Tunnel Syndrome has numerous nonsurgical treatments including splint, physical therapy and corticosteroid injections. Aim: The purpose of this study was to evaluate the effectiveness of an ultrasound guided treatment procedure, for individuals with severe carpal tunnel syndrome. Materials and Method: 20 patients with an electrodiagnostic evidence of severe carpal tunnel syndrome were treated by an office-based ultrasound guided procedure (combination of percutaneous needle release of carpal tunnel and corticosteroid injection). Electrodiagnostic (nerve conduction study), clinical (Boston Carpal Tunnel Questionnaire, grip strength) and ultrasonic (median nerve and carpal tunnel cross-sectional area) measurements were recorded at baseline and one month after intervention. Results: Our preliminary data analysis showed that in one month follow up, patients had a significantly smaller cross-sectional area of the median nerve compared to pretreatment values (mean difference 0.06; 95%CI: 0.02-0.1; p < 0.001). In addition, patients had significantly less functional impairment (mean difference 35; 95% CI:28.7-43.4 ; p < 0.001), and an improved hand grip strength in one month follow up (mean difference 5.4; 95%CI: 3.1-7.8; p < 0.001;). There were no significant complications. Conclusion: Patients with severe carpal tunnel syndrome, who are candidates for surgical intervention, can consider office-based ultrasound guided needle release of carpal tunnel as an alternative safe treatment.

Keywords: Carpal Tunnel Syndrome, needle release, pain, ultrasound

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Authors: Ajay Agrawal, Pritha Basnet, Achala Thakur, Pappu Rizal, Rubina Rai

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Context: Rapid expulsion of fetus in intrauterine fetal death (IUFD) is usually requested without any medical grounds for it. So; an efficient, safe method for induction of labor (IOL) is required. Objective: To determine if pre-treatment with mifepristone followed by IOL with misoprostol in late IUFD is more efficacious. Methods: We conducted a randomized controlled trial in 100 patients. Group-A women received single oral dose of 200 mg mifepristone, followed by induction with vaginal misoprostol after 24-hour. Group-B women were induced only with vaginal misoprostol. In each group 5 dose of misoprostol was used 4 hourly. If first cycle was unsuccessful, after break of 12 hour, second course of misoprostol was started. The primary outcome was a measure of induction to delivery time and vaginal delivery within 24 hours. Secondary outcome was to measure need of oxytocin and complications. Results: Maternal age, parity and period of gestation were comparable between groups. Number of misoprostol dose needed in group A was significantly less than group B. Mann Whitney U test showed, women in group A had significantly earlier onset of labor, however total induction to delivery interval was not significant. In group-A, 85.7% delivered within 24 hours of first dose of misoprostol while in group-B 70% delivered within 24 hour (p=0.07). More women in Group B required oxytocin. Conclusion: Pretreatment with mifepristone before IOL following late IUFD is an effective and safe regimen. It appears to shorten the duration of induction to onset of labor.

Keywords: induction of labor, intrauterine fetal death, mifepristone, misoprostol

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Authors: Rasha Hosny, Ahmed Zahran, Mahmoud Ramzi, Fatma Mahmoud Abdelhafiz, Ammona S. Mohamed, Mahmoud Fathy Mubarak

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Ionic liquids' ability to be tuned and stability under challenging environmental conditions are their significant features in enhanced oil recovery. In this study, two amino acid ionic liquids (AAILs) were prepared from quaternized hyperbranched polyamidoamine PAMAM (G0.5 C12) and amino acids (Cysteine and Lysine). The chemical structures of the prepared AAILs were verified by using FTIR and 1H-NMR spectra. These AAILs were tested for solubility, thermal stability, and surface activity in the presence of Egyptian medium crude oils under different PVT parameters after being diluted in several brine solutions of various salt compositions at 10% (w/w) salinity. The measurements reveal that the produced AAILs have good solubility and thermal stability. The effect of different concentrations of AAILs (0.1-5%) and salinity (20000-70000 ppm) on Interfacial tension (IFT) were studied. To test the efficacy of (AAILs) for a CEOR, numerous flooding experiments were carried out in samples of sandstone rock. Rock wettability is important for sandstone rocks, so conduct wettability alteration by contact angle (CA) of (30-55) and IFT of (7-13). The additional oil recovery was largely influenced by ionic liquid concentration, which may be changed by dilution with the formation and injected brines. This research has demonstrated that EOR techniques led to a recovery wt. (22-45%).

Keywords: amino acid ionic liquids, surface activity, critical micelle concentration, interfacial tension, contact angle, chemical enhanced oil recovery, wettability

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Authors: Salima Tabti, Chaima Maouche, Tinhinene Louaileche, Amel Djedouani, Ismail Warad

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Novel Schiff base ligand HL has been synthesized by condensation of aromatic amine and DHA. It was characterized by UV-Vis, FT-IR, SM, NMR (1H, 13C) and also by single-crystal X-ray diffraction. The crystal structure shows that compound crystallized in a triclinic system in P-1 space group and with a two unit per cell (Z = 2).The asymmetric unit, contains one independent molecules, the conformation is determined by an intermolecular N-H…O hydrogen bond with an S(6) ring motif. The molecule have an (E) conformation about the C=N bond. The dihedral angles between the phenyl and pyran ring planes is 89.37 (1), the two plans are approximately perpendicular. The catecholase activity of is situ copper complexes of this ligand has been investigated against catechol. The progress of the oxidation reactions was closely monitored over time following the strong peak of catechol using UV-Vis. Oxidation rates were determined from the initial slope of absorbance. time plots, then analyzed by Michaelis-Menten equations. Catechol oxidation reactions were realized using different concentrations of copper acetate and ligand (L/Cu: 1/1, 1/2, 2/1). The results show that all complexes were able to catalyze the oxidation of catechol. Acetate complexes have the highest activity. Catalysis is a branch of chemical kinetics that, more generally, studies the influence of all physical or chemical factors determining reaction rates. It solves a lot of problems in the chemistry reaction process, especially for a green, economic and less polluting chemistry. For this reason, the search for new catalysts for known organic reactions, occupies a very advanced place in the themes proposed by the chemists.

Keywords: dehydroacetic acid, catechol, copper, catecholase activity, x-ray

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Authors: B. S. Boyanov, A. B. Peltekov, K. I. Ivanov

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The ferrites of Zn, Cd, Cu, and mixed ferrites with NiO, MnO, MgO, CoO, ZnO, BaO combine the properties of dielectrics, semiconductors, ferro-magnets, catalysts, etc. The ferrites are used in an impressive range of applications due to their remarkable properties. A specific disadvantage of ferrites is that they are undesirably obtained in a lot of processes connected with metal production. They are very stable and poorly soluble compounds. The obtained ZnFe2O4 in zinc production connecting about 15% of the total zinc remains practically insoluble in dilute solutions of sulfuric acid. This decreases the degree of recovery of zinc and necessitates to further process the zinc-containing cake. In this context, the ferrites; ZnFe2O4, CdFe2O4, and CuFe2O4 are synthesized in laboratory conditions using ceramic technology. Their homogeneity and structure are proven by X-Ray diffraction analysis and Mössbauer spectroscopy. The synthesized ferrites are subjected to strong acid and high temperature leaching with solutions of H2SO4, HCl, and HNO3 (7, 10 and 15 %). The results indicate that the highest degree of leaching of Zn, Cd, and Cu from the ferrites is achieved by use of HCl. The resulting values for the degree of leaching of metals using H2SO4 are lower, but still remain significantly higher for all of the experimental conditions compared to the values obtained using HNO3. Five zinc sulfide concentrates are characterized for iron content by chemical analysis, Web-based Information System, and iron phases by Mössbauer spectroscopy. The charging was optimized using the criterion of minimal amount of zinc ferrite produced when roasting the concentrates in a fluidized bed. The results obtained are interpreted in terms of the hydrometallurgical zinc production and maximum recovery of zinc, copper and cadmium from initial zinc sulfide concentrates after their roasting.

Keywords: hydrometallurgy, inorganic acids, solubility, zinc ferrite

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Authors: Jin Choi, Zahra Aminikhoei, Yi-Oh Kim, Sang-Min Lee

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A 4 × 2 factorial experiment was conducted to determine the optimum dietary protein and lipid levels for juvenile fancy carp, Cyprinus carpio var. koi. Eight experimental diets were formulated to contain four protein levels (200, 300, 400, and 500 g kg-1) with two lipid levels (70 and 140 g kg-1). Triplicate groups of fish (initial weight, 12.1±0.2 g fish-1) were hand-fed the diets to apparent satiation for 8 weeks. Weight gain, daily feed intake, feed efficiency ratio and protein efficiency ratio were significantly (P < 0.0001) affected by dietary protein level, but not by dietary lipid level (P > 0.05). Weight gain and feed efficiency ratio tended to increase as dietary protein level increased up to 400 and 500 g kg-1, respectively. Daily feed intake of fish decreased with increasing dietary protein level and that of fish fed diet contained 500 g kg-1 protein was significantly lower than other fish groups. The protein efficiency ratio of fish fed 400 and 500 g kg-1 protein was lower than that of fish fed 200 and 300 g kg-1 protein. Moisture, crude protein and crude lipid contents of muscle and liver were significantly affected by dietary protein, but not by dietary lipid level (P > 0.05). The increase in dietary lipid level resulted in an increase in linoleic acid in liver and muscle paralleled with a decrease in n-3 highly unsaturated fatty acids content in muscle of fish. In considering these results, it was concluded that the diet containing 400 g kg-1 protein with 70 g kg-1 lipid level is optimal for growth and efficient feed utilization of juvenile fancy carp.

Keywords: fancy carp, dietary protein, dietary lipid, Cyprinus carpio, fatty acid

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Authors: Bashistha Kumar Kanth, Seung Pil Pack

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Carbonic anhydrase is ubiquitously distributed in organisms, and is fundamental to many eukaryotic biological processes such as photosynthesis, respiration, CO2 and ion transport, calcification and acid–base balance. However, CA occurs across the spectrum of prokaryotic metabolism in both the archaea and bacteria domains and many individual species contain more than one class. In this review, various roles of CA involved in cellular mechanism are presented to find out the CA functions applicable for industrial use.

Keywords: carbonic anhydrase, mechanism, CO2 sequestration, respiration

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Authors: Thidarat Duangyod, Chanida Palanuvej, Nijsiri Ruangrungsi

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Pentace burmanica Kurz., belonging to the Malvaceae family, is commonly used for anti-diarrhea in Thai traditional medicine. A method for quantification of (+)-catechin and (-)-epicatechin in P. burmanica stem bark from 12 different Thailand markets by reverse-phase high performance liquid chromatography (HPLC) was investigated and validated. The analysis was performed by a Shimadzu DGU-20A3 HPLC equipped with a Shimadzu SPD-M20A photo diode array detector. The separation was accomplished with an Inersil ODS-3 column (5 µm x 4.6 x 250 mm) using 0.1% formic acid in water (A) and 0.1% formic acid in acetonitrile (B) as mobile phase at the flow rate of 1 ml/min. The isocratic was set at 20% B for 15 min and the column temperature was maintained at 40 ºC. The detection was at the wavelength of 280 nm. Both (+)-catechin and (-)-epicatechin existed in the ethanolic extract of P. burmanica stem bark. The content of (-)-epicatechin was found as 59.74 ± 1.69 µg/mg of crude extract. In contrast, the quantitation of (+)-catechin content was omitted because of its small amount. The method was linear over a range of 5-200 µg/ml with good coefficients (r2 > 0.99) for (+)-catechin and (-)-epicatechin. Limit of detection values were found to be 4.80 µg/ml for (+)-catechin and 5.14 µg/ml for (-)-epicatechin. Limit of quantitation of (+)-catechin and (-)-epicatechin were of 14.54 µg/ml and 15.57 µg/ml respectively. Good repeatability and intermediate precision (%RSD < 3) were found in this study. The average recoveries of both (+)-catechin and (-)-epicatechin were obtained with good recovery in the range of 91.11 – 97.02% and 88.53 – 93.78%, respectively, with the %RSD less than 2. The peak purity indices of catechins were more than 0.99. The results suggested that HPLC method proved to be precise and accurate and the method can be conveniently used for (+)-catechin and (-)-epicatechin determination in ethanolic extract of P. burmanica stem bark. Moreover, the stem bark of P. burmanica was found to be a rich source of (-)-epicatechin.

Keywords: pentace burmanica, (+)-catechin, (-)-epicatechin, high performance liquid chromatography

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Authors: Silindile Gumede, Amir Hossein Mohammadi, Mbuyu Germain Ntunka

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Goal 12 of the 17 Sustainable Development Goals (SDGs) encourages sustainable consumption and production patterns. This necessitates achieving the environmentally safe management of chemicals and all wastes throughout their life cycle and the proper disposal of pollutants and toxic waste. Fluid catalytic cracking (FCC) catalysts are widely used in the refinery to convert heavy feedstocks to lighter ones. During the refining processes, the catalysts are deactivated and discarded as hazardous toxic solid waste. Spent catalysts (SC) contain high-cost metal, and the recovery of metals from SCs is a tactical plan for supplying part of the demand for these substances and minimizing the environmental impacts. Leaching followed by solvent extraction, has been found to be the most efficient method to recover valuable metals with high purity from spent catalysts. However, the use of inorganic acids during the leaching process causes a secondary environmental issue. Therefore, it is necessary to explore other alternative efficient leaching agents that are economical and environmentally friendly. In this study, the waste catalyst was collected from a domestic refinery and was characterised using XRD, ICP, XRF, and SEM. Response surface methodology (RSM) and Box Behnken design were used to model and optimize the influence of some parameters affecting the acidic leaching process. The parameters selected in this investigation were the acid concentration, temperature, and leaching time. From the characterisation results, it was found that the spent catalyst consists of high concentrations of Vanadium (V) and Nickel (Ni); hence this study focuses on the leaching of Ni and V using a biodegradable acid to eliminate the formation of the secondary pollution.

Keywords: eco-friendly leaching, optimization, metal recovery, leaching

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Authors: Kelli G. Thorup, Kristopher A. Blee

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Climate change enhances the occurrence of extreme weather: wildfires, drought, rising summer temperatures, all of which dramatically decline forest growth and increase tree mortality in the mixed-conifer forests of Sierra Nevada, California. However, microbiota living in mutualistic relations with plant rhizospheres have been found to mitigate the effects of suboptimal environmental conditions. The goal of this research is to isolate native beneficial bacteria, plant-growth promoting rhizobacteria (PGPR), that can alleviate heat stress in Pinus ponderosa seedlings. Bacteria were isolated from the rhizosphere of Pinus ponderosa juveniles located in mixed-conifer stand and further characterized for PGP potential based on their ability to produce key growth regulatory phytohormones including auxin, cytokinin, and gibberellic acid. Out of ten soil samples taken, sixteen colonies were isolated and qualitatively confirmed to produce indole-3-acetic acid (auxin) using Salkowski’s reagent. Future testing will be conducted to quantitatively assess phytohormone production in bacterial isolates. Furthermore, bioassays will be performed to determine isolates abilities to increase tolerance in heat-stressed Pinus ponderosa seedlings. Upon completion of this research, a PGPR could be utilized to support the growth and transplantation of conifer seedlings as summer temperatures continue to rise due to the effects of climate change.

Keywords: conifer, heat-stressed, phytohormones, Pinus ponderosa, plant-growth promoting rhizobacteria

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Authors: Zong Yan Cai, Wen-Chyuan Chen, Chih-Min Wu

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The purpose of this study was to investigate the acute effects of local vibration on muscle activation, metabolic and hormone responses. Totally 12 healthy, physically inactive, male adults participated in this study and completed LV exercise session. During LV exercise session, four custom-made vibrations (diameter: 20 mm; thickness: 8 mm; weight: 0.022 g) were locally placed over the belly of the thigh of each subject’s non-dominant leg in supine lying position, and subjects received 10 sets for 1 min at the frequency of 35-40Hz, with 1–2 min of rest between sets. The surface electromyography (EMG) were obtained from the vastus medialis and rectus femoris, and the subjects’ rating of perceived exertion (RPE) and heart rate (HR) were measured. EMG data, RPE values as well as HR were obtained by averaging the results of 10 sets of each exercise session. Blood samples were drawn before exercise, immediately after exercise, and 15min and 30min after exercise in each session for analysis of lactic acid (LA), growth hormone (GH), testosterone (T) and cortisol (C). The results indicated that the HR did not increase after LV (63.18±3.5 to 63.25±2.58 beat/min, p > 0.05). The average RPE values during the LV exposure were at 2.86±0.39. The root mean square % EMG values from the vastus medialis and rectus femoris were 19.02±2.19 and 8.25±2.20 respectively. There were no significant differences after acute LV exercise among LA, GH and T values as compared with baseline values (LA: 0.68±0.11 to 0.7±0.1 mmol/L; GH: 0.06±0.05 to 0.57±0.27 ng/mL; T: 551.33±46.62 to 520.42±43.78 ng/dL, p>0.05). However, the LV treatment caused a significant decrease in C values after exercise (16.56±1.05 to 11.64±1.85 nmol/L, p<0.05). In conclusion, acute LV exercise only slightly increase muscle activation which may not cause effective exercise response. However, acute LV exercise reduces C level, which may reduce the catabolic response. The probable reason might partly due to the vibration rhythmically which massage on muscles.

Keywords: cortisol, growth hormone, lactic acid, testosterone

Procedia PDF Downloads 268

Authors: Rangrong Yoksan, Amporn Sane, Nattaporn Khanoonkon, Chanakorn Yokesahachart, Narumol Noivoil, Khanh Minh Dang

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Polylactic acid (PLA) is the most commercially available bio-based and biodegradable plastic at present. PLA has been used in plastic related industries including single-used containers, disposable and environmentally friendly packaging owing to its renewability, compostability, biodegradability, and safety. Although PLA demonstrates reasonably good optical, physical, mechanical, and barrier properties comparable to the existing petroleum-based plastics, its brittleness and mold shrinkage as well as its price are the points to be concerned for the production of rigid and semi-rigid packaging. Blending PLA with other bio-based polymers including thermoplastic starch (TPS) is an alternative not only to achieve a complete bio-based plastic, but also to reduce the brittleness, shrinkage during molding and production cost of the PLA-based products. TPS is a material produced mainly from starch which is cheap, renewable, biodegradable, compostable, and non-toxic. It is commonly prepared by a plasticization of starch under applying heat and shear force. Although glycerol has been reported as one of the most plasticizers used for preparing TPS, its migration caused the surface stickiness of the TPS products. In some cases, mixed plasticizers or natural fibers have been applied to impede the retrogradation of starch or reduce the migration of glycerol. The introduction of fibers into TPS-based materials could reinforce the polymer matrix as well. Therefore, the objective of the present research is to study the effect of starch type (i.e. native starch and phosphate starch), plasticizer type (i.e. glycerol and xylitol with a weight ratio of glycerol to xylitol of 100:0, 75:25, 50:50, 25:75, and 0:100), and fiber content (i.e. in the range of 1-25 % wt) on properties of PLA/TPS blend and composite. PLA/TPS blends and composites were prepared using a twin-screw extruder and then converted into dumbbell-shaped specimens using an injection molding machine. The PLA/TPS blends prepared by using phosphate starch showed higher tensile strength and stiffness than the blends prepared by using the native one. In contrast, the blends from native starch exhibited higher extensibility and heat distortion temperature (HDT) than those from the modified starch. Increasing xylitol content resulted in enhanced tensile strength, stiffness, and water resistance, but decreased extensibility and HDT of the PLA/TPS blend. Tensile properties and hydrophobicity of the blend could be improved by incorporating silane treated-jute fibers.

Keywords: polylactic acid, thermoplastic starch, Jute fiber, composite, blend

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Authors: Muga Moses

Abstract:

Plant growth regulators are actively involved in the growth and yield of plants. However, limited information is available on the combined effect of gibberellic acid (GA3) on growth attributes and yield of African nightshade. This experiment will be designed to fill this gap by studying the performance of African nightshade under the application of hormones. Gibberellic acid is a plant growth hormone that promotes cell expansion and division. A greenhouse and laboratory experiment will be conducted at the University of Sussex biotechnology greenhouse and Agriculture laboratory using a growth chamber to study the effect of GA3 on the growth and development attributes of African nightshade. The experiment consists of three replications and 5 treatments and is laid out in a randomized complete block design consisting of various concentrations of GA3. 0ppm, 50ppm, 100ppm, 150ppm and 200ppm. local farmer seed was grown in plastic pots, 6 seeds then hardening off to remain with four plants per pot at the greenhouse to attain purity of germplasm, proper management until maturity of berries then harvesting and squeezing to get seeds, paper dry on the sun for 7 days. In a laboratory, place 5 Whatman filter paper on glass petri-dish subject to different concentrations of stock solution, count 50 certified and clean, healthy seeds, then arrange on the moist filter paper and mark respectively. Spray with the stock solution twice a day and protrusion of radicle termed as germination count and discard to increase the accuracy of precision. Data will be collected on the application of GA3 to compare synergistic effects on the growth, yield, and nutrient contents on African nightshade.

Keywords: African nightshade, growth, yield, shoot, gibberellins

Procedia PDF Downloads 86

Authors: Jaqueline G. L. Cosme, Paulo H. S. Picciani, Regina C. R. Nunes

Abstract:

Electrospinning is a technique for the fabrication of nanoscale fibers. The general electrospinning system consists of a syringe filled with polymer solution, a syringe pump, a high voltage source and a grounded counter electrode. During electrospinning a volumetric flow is set by the syringe pump and an electric voltage is applied. This forms an electric potential between the needle and the counter electrode (collector plate), which results in the formation of a Taylor cone and the jet. The jet is moved towards the lower potential, the counter electrode, wherein the solvent of the polymer solution is evaporated and the polymer fiber is formed. On the way to the counter electrode, the fiber is accelerated by the electric field. The bending instabilities that occur form a helical loop movements of the jet, which result from the coulomb repulsion of the surface charge. Trough bending instabilities the jet is stretched, so that the fiber diameter decreases. In this study, a thermoplastic/elastomeric binary blend of non-vulcanized epoxidized natural rubber (ENR) and poly(latic acid) (PLA) was electrospun using polymer solutions consisting of varying proportions of PCL and NR. Specifically, 15% (w/v) PLA/ENR solutions were prepared in /chloroform at proportions of 5, 10, 25, and 50% (w/w). The morphological and thermal properties of the electrospun mats were investigated by scanning electron microscopy (SEM) and differential scanning calorimetry analysis. The SEM images demonstrated the production of micrometer- and sub-micrometer-sized fibers with no bead formation. The blend miscibility was evaluated by thermal analysis, which showed that blending did not improve the thermal stability of the systems.

Keywords: epoxidized natural rubber, poly(latic acid), electrospinning, chemistry

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Authors: P. Mirahmadpour, M. H. Banitaba, D. Nematollahi

Abstract:

The chemistry of coordination polymers in recent years has grown exponentially not only because of their interesting architectures but also due to their various technical applications in many fields including ion exchange, chemical catalysis, small molecule separations, and drug release. The use of bridging ligands for the controlled self-assembly of one, two or three dimensional metallo-supramolecular species is the subject of serious study in last decade. Numerous different synthetic methods have been offered for the preparation of coordination polymers such as (a) diffusion from the gas phase, (b) slow diffusion of the reactants into a polymeric matrix, (c) evaporation of the solvent at ambient or reduced temperatures, (d) temperature controlled cooling, (e) precipitation or recrystallisation from a mixture of solvents and (f) hydrothermal synthesis. The electrosynthetic process suggested several advantages over conventional approaches. A general advantage of electrochemical synthesis is that it allows synthesis under milder conditions than typical solvothermal or microwave synthesis. In this work we have introduced a simple electrochemical method for growing metal coordination polymers based on copper with a flexible 2,2’-thiodiacetic acid (TDA) and rigid 1,2,4,5-benzenetetracarboxylate (BTC) ligands. The structure of coordination polymers were characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), elemental analysis, thermal gravimetric (TG) and differential thermal analyses (DTA). The single-crystal X-ray diffraction analysis revealed that different conformations of the ligands and different coordination modes of the carboxylate group as well as different coordination geometries of the copper atoms. Electrochemical synthesis of coordination polymers has different advantages such as faster synthesis at lower temperature in compare with conventional chemical methods and crystallization of desired materials in a single synthetic step.

Keywords: 1, 2, 4, 5-benzenetetracarboxylate, coordination polymer, copper, 2, 2’-thiodiacetic acid

Procedia PDF Downloads 204