Search results for: hydrocarbon solvent

Authors: Shin Woo Kim, Eui Ju Lee

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The recent development of biofuel production technology facilitates the use of bioethanol and biodiesel on automobile. Bioethanol, especially, can be used as a fuel for gasoline vehicles because the addition of ethanol has been known to increase octane number and reduce soot emissions. However, the wide application of biofuel has been still limited because of lack of detailed combustion properties such as auto-ignition temperature and pollutant emissions such as NOx and soot, which has been concerned mainly on the vehicle fire safety and environmental safety. In this study, the combustion characteristics of gasoline/ethanol fuel were investigated both numerically and experimentally. For auto-ignition temperature and NOx emission, the numerical simulation was performed on the well-stirred reactor (WSR) to simulate the homogeneous gasoline engine and to clarify the effect of ethanol addition in the gasoline fuel. Also, the response surface method (RSM) was introduced as a design of experiment (DOE), which enables the various combustion properties to be predicted and optimized systematically with respect to three independent variables, i.e., ethanol mole fraction, equivalence ratio and residence time. The results of stoichiometric gasoline surrogate show that the auto-ignition temperature increases but NOx yields decrease with increasing ethanol mole fraction. This implies that the bioethanol added gasoline is an eco-friendly fuel on engine running condition. However, unburned hydrocarbon is increased dramatically with increasing ethanol content, which results from the incomplete combustion and hence needs to adjust combustion itself rather than an after-treatment system. RSM results analyzed with three independent variables predict the auto-ignition temperature accurately. However, NOx emission had a big difference between the calculated values and the predicted values using conventional RSM because NOx emission varies very steeply and hence the obtained second order polynomial cannot follow the rates. To relax the increasing rate of dependent variable, NOx emission is taken as common logarithms and worked again with RSM. NOx emission predicted through logarithm transformation is in a fairly good agreement with the experimental results. For more tangible understanding of gasoline/ethanol fuel on pollutant emissions, experimental measurements of combustion products were performed in gasoline/ethanol pool fires, which is widely used as a fire source of laboratory scale experiments. Three measurement methods were introduced to clarify the pollutant emissions, i.e., various gas concentrations including NOx, gravimetric soot filter sampling for elements analysis and pyrolysis, thermophoretic soot sampling with transmission electron microscopy (TEM). Soot yield by gravimetric sampling was decreased dramatically as ethanol was added, but NOx emission was almost comparable regardless of ethanol mole fraction. The morphology of the soot particle was investigated to address the degree of soot maturing. The incipient soot such as a liquid like PAHs was observed clearly on the soot of higher ethanol containing gasoline, and the soot might be matured under the undiluted gasoline fuel.

Keywords: gasoline/ethanol fuel, NOx, pool fire, soot, well-stirred reactor (WSR)

Procedia PDF Downloads 212

Authors: Danilo A. F. Fontes, Magaly A. M.Lyra, Maria L. C. Moura, Leslie R. M. Ferraz, Salvana P. M. Costa, Amanda C. Q. M. Vieira, Larissa A. Rolim, Giovanna C. R. M. Schver, Ping I. Lee, Severino Alves-Júnior, José L. Soares-Sobrinho, Pedro J. Rolim-Neto

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Efavirenz (EFV) is a first-choice drug in antiretroviral therapy with high efficacy in the treatment of infection by Human Immunodeficiency Virus, which causes Acquired Immune Deficiency Syndrome (AIDS). EFV has low solubility in water resulting in a decrease in the dissolution rate and, consequently, in its bioavailability. Among the technological alternatives to increase solubility, the Lamellar Double Hydroxides (LDH) have been applied in the development of systems with poorly water-soluble drugs. The use of analytical techniques such as X-Ray Diffraction (XRD), Infrared Spectroscopy (IR) and Differential Scanning Calorimetry (DSC) allowed the elucidation of drug interaction with the lamellar compounds. The objective of this work was to characterize and develop the binary systems with EFV and LDH in order to increase the solubility of the drug. The LDH-CaAl was synthesized by the method of co-precipitation from salt solutions of calcium nitrate and aluminum nitrate in basic medium. The systems EFV-LDH and their physical mixtures (PM) were obtained at different concentrations (5-60% of EFV) using the solvent technique described by Takahashi & Yamaguchi (1991). The characterization of the systems and the PM’s was performed by XRD techniques, IR, DSC and dissolution test under non-sink conditions. The results showed improvements in the solubility of EFV when associated with LDH, due to a possible change in its crystal structure and formation of an amorphous material. From the DSC results, one could see that the endothermic peak at 173°C, temperature that correspond to the melting process of EFZ in the crystal form, was present in the PM results. For the EFZ-LDH systems (with 5, 10 and 30% of drug loading), this peak was not observed. XRD profiles of the PM showed well-defined peaks for EFV. Analyzing the XRD patterns of the systems, it was found that the XRD profiles of all the systems showed complete attenuation of the characteristic peaks of the crystalline form of EFZ. The IR technique showed that, in the results of the PM, there was the appearance of one band and overlap of other bands, while the IR results of the systems with 5, 10 and 30% drug loading showed the disappearance of bands and a few others with reduced intensity. The dissolution test under non-sink conditions showed that systems with 5, 10 and 30% drug loading promoted a great increase in the solubility of EFV, but the system with 10% of drug loading was the only one that could keep substantial amount of drug in solution at different pHs.

Keywords: Efavirenz, Lamellar Double Hydroxides, Pharmaceutical Techonology, Solubility

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Authors: L. Abukova, O. Abramova, A. Goreva, Y. Yakovlev

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Important executive decisions on oil and gas production stimulation in Eastern Siberia have been recently taken. There are unique and large fields of oil, gas, and gas-condensate in Eastern Siberia. The Talakan, Koyumbinskoye, Yurubcheno-Tahomskoye, Kovykta, Chayadinskoye fields are supposed to be developed first. It will result in an abrupt increase in environmental load on the nature of Eastern Siberia. In Eastern Siberia, the introduction of ecological imperatives in hydrocarbon production is still realistic. Underground water movement is the one of the most important factors of the ecosystems condition management. Oil and gas production is associated with the forced displacement of huge water masses, mixing waters of different composition, and origin that determines the extent of anthropogenic impact on water drive systems and their protective reaction. An extensive hydrogeological system of the depression type is identified in the pre-salt deposits here. Pressure relieve here is steady up to the basement. The decrease of the hydrodynamic potential towards the basement with such a gradient resulted in reformation of the fields in process of historical (geological) development of the Nepsko-Botuobinskaya anteclise. The depression hydrodynamic systems are characterized by extremely high isolation and can only exist under such closed conditions. A steady nature of water movement due to a strictly negative gradient of reservoir pressure makes it quite possible to use environmentally-harmful liquid substances instead of water. Disposal of the most hazardous wastes is the most expedient in the deposits of the crystalline basement in certain structures distant from oil and gas fields. The time period for storage of environmentally-harmful liquid substances may be calculated by means of the geological time scales ensuring their complete prevention from releasing into environment or air even during strong earthquakes. Disposal of wastes of chemical and nuclear industries is a matter of special consideration. The existing methods of storage and disposal of wastes are very expensive. The methods applied at the moment for storage of nuclear wastes at the depth of several meters, even in the most durable containers, constitute a potential danger. The enormous size of the depression system of the Nepsko-Botuobinskaya anteclise makes it possible to easily identify such objects at the depth below 1500 m where nuclear wastes will be stored indefinitely without any environmental impact. Thus, the water drive system of the Nepsko-Botuobinskaya anteclise is the ideal object for large-volume injection of environmentally harmful liquid substances even if there are large oil and gas accumulations in the subsurface. Specific geological and hydrodynamic conditions of the system allow the production of hydrocarbons from the subsurface simultaneously with the disposal of industrial wastes of oil and gas, mining, chemical, and nuclear industries without any environmental impact.

Keywords: Eastern Siberia, formation pressure, underground water, waste burial

Procedia PDF Downloads 259

Authors: Afifa Hafidh, Fathi Touati, Ahmed Hichem Hamzaoui, Sayda Somrani

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The objective of the present study has been to synthesize and to characterize silica hybrid materials using sol-gel technic and to investigate their properties. Silica materials were successfully fabricated using various bi-functional 1,3,4-thiadiazoles and tetraethoxysilane (TEOS) as co-precursors via a facile one-pot sol-gel pathway. TEOS was introduced at room temperature with 1,3,4-thiadiazole 2,5-difunctiunal adducts, in ethanol as solvent and using HCl acid as catalyst. The sol-gel process lead to the formation of monolithic, coloured and transparent gels. TEOS was used as a principal network forming agent. The incorporation of 1,3,4-thiadiazole molecules was realized by attachment of these later onto a silica matrix. This allowed covalent linkage between organic and inorganic phases and lead to the formation of Si-N and Si-S bonds. The prepared hybrid materials were characterized by Fourier transform infrared, NMR ²⁹Si and ¹³C, scanning electron microscopy and nitrogen absorption-desorption measurements. The optic and magnetic properties of hybrids are studied respectively by ultra violet-visible spectroscopy and electron paramagnetic resonance. It was shown in this work, that heterocyclic moieties were successfully attached in the hybrid skeleton. The formation of the Si-network composed of cyclic units (Q3 structures) connected by oxygen bridges (Q4 structures) was proved by ²⁹Si NMR spectroscopy. The Brunauer-Elmet-Teller nitrogen adsorption-desorption method shows that all the prepared xerogels have isotherms type IV and are mesoporous solids. The specific surface area and pore volume of these materials are important. The obtained results show that all materials are paramagnetic semiconductors. The data obtained by Nuclear magnetic resonance ²⁹Si and Fourier transform infrared spectroscopy, show that Si-OH and Si-NH groups existing in silica hybrids can participate in adsorption interactions. The obtained materials containing reactive centers could exhibit adsorption properties of metal ions due to the presence of OH and NH functionality in the mesoporous frame work. Our design of a simple method to prepare hybrid materials may give interest of the development of mesoporous hybrid systems and their use within the domain of environment in the future.

Keywords: hybrid materials, sol-gel process, 1, 3, 4-thiadaizole, TEOS

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Authors: Saheli Mitra, Ramesh Karri, Praveen K. Mylapalli, Arka. B. Dey, Gourav Bhattacharya, Gouriprasanna Roy, Syed M. Kamil, Surajit Dhara, Sunil K. Sinha, Sajal K. Ghosh

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The most well-known structures of lyotropic liquid crystalline systems are the two dimensional hexagonal phase of cylindrical micelles with a positive interfacial curvature and the lamellar phase of flat bilayers with zero interfacial curvature. In aqueous solution of surfactants, the concentration dependent phase transitions have been investigated extensively. However, instead of changing the surfactant concentrations, the local curvature of an aggregate can be altered by tuning the electrostatic interactions among the constituent molecules. Intermediate phases with non-uniform interfacial curvature are still unexplored steps to understand the route of phase transition from hexagonal to lamellar. Understanding such structural evolution in lyotropic liquid crystalline systems is important as it decides the complex rheological behavior of the system, which is one of the main interests of the soft matter industry. Sodium dodecyl sulfate (SDS) is an anionic surfactant and can be considered as a unique system to tune the electrostatics by cationic additives. In present study, imidazolium-based ionic liquids (ILs) with different number of carbon atoms in their single hydrocarbon chain were used as the additive in the aqueous solution of SDS. At a fixed concentration of total non-aqueous components (SDS and IL), the molar ratio of these components was changed, which effectively altered the electrostatic interactions between the SDS molecules. As a result, the local curvature is observed to modify, and correspondingly, the structure of the hexagonal liquid crystalline phases are transformed into other phases. Polarizing optical microscopy of SDS and imidazole-based-IL systems have exhibited different textures of the liquid crystalline phases as a function of increasing concentration of the ILs. The small angle synchrotron x-ray diffraction (SAXD) study has indicated the hexagonal phase of direct cylindrical micelles to transform to a rectangular phase at the presence of short (two hydrocarbons) chain IL. However, the hexagonal phase is transformed to a lamellar phase at the presence of long (ten hydrocarbons) chain IL. Interestingly, at the presence of a medium (four hydrocarbons) chain IL, the hexagonal phase is transformed to another hexagonal phase of direct cylindrical micelles through the lamellar phase. To the best of our knowledge, such a phase sequence has not been reported earlier. Even though the small angle x-ray diffraction study has revealed the lattice parameters of these phases to be similar to each other, their rheological behavior has been distinctly different. These rheological studies have shed lights on how these phases differ in their viscoelastic behavior. Finally, the packing parameters, calculated for these phases based on the geometry of the aggregates, have explained the formation of the self-assembled aggregates.

Keywords: lyotropic liquid crystals, polarizing optical microscopy, rheology, surfactants, small angle x-ray diffraction

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Authors: Mehrosadat Mirmohammadi, Sara Taghdisi, Ali Padash, Mohammad Hossein Pazandeh

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Gossypol, a yellowish anti-nutritional compound found in cotton plants, exists in various plant parts, including seeds, husks, leaves, and stems. Chemically, gossypol is a potent polyphenolic aldehyde with antioxidant and therapeutic properties. However, its free form can be toxic, posing risks to both humans and animals. Initially, we extracted gossypol from cotton seeds using n-hexane as a solvent (yield: 84.0 ± 4.0%). We also obtained cotton seed and cotton boll extracts via Soxhlet extraction (25:75 hydroalcoholic ratio). These extracts, combined with cornstarch, formed four herbal medicinal formulations. Ethical approval allowed us to investigate their effects on Leishmania-caused skin wounds, comparing them to glucantime (local ampoule). Herbal formulas outperformed the control group (ethanol only) in wound treatment (p-value 0.05). The average wound diameter after two months did not significantly differ between plant extract ointments and topical glucantime. Notably, cotton boll extract with 1% extra gossypol crystal showed the best therapeutic effect. We extracted gossypol from cotton seeds using n-hexane via Soxhlet extraction. Saponification, acidification, and recrystallization steps followed. FTIR, UV-Vis, and HPLC analyses confirmed the product’s identity. Herbal medicines from cotton seeds effectively treated chronic wounds compared to the ethanol-only control group. Wound diameter differed significantly between extract ointments and glucantime injections. It seems that due to the presence of large amounts of fat in the oil, the extraction of gossypol from it faces many obstacles. The extraction of this compound with our technique showed that extraction from oil has a higher efficiency, perhaps because of the preparation of oil by cold pressing method, the possibility of losing this compound is much less than when extraction is done with Soxhlet. On the other hand, the gossypol in the oil is mostly bound to the protein, which somehow protects the gossypol until the last stage of the extraction process. Since this compound is very sensitive to light and heat, it was extracted as a derivative with acetic acid. Also, in the treatment section, it was found that the ointment prepared with the extract is more effective and Gossypol is one of the effective ingredients in the treatment. Therefore, gossypol can be extracted from the oil and added to the extract from which gossypol has been extracted to make an effective medicine with a certain dose.

Keywords: cottonseed, glucantime, gossypol, leishmaniasis

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Authors: Ahmed. Abdel Bary, Omneya. Khowessah, Mojahed. al-jamrah

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Introduction: The major challenge with the design of oral dosage forms lies with their poor bioavailability. The most frequent causes of low oral bioavailability are attributed to poor solubility and low permeability. The aim of this study was to develop solid nanodispersed tablet formulation of Glimepiride for the enhancement of the solubility and bioavailability. Methodology: Solid nanodispersions of Glimepiride (GMP) were prepared using two different ratios of 2 different carriers, namely; PEG6000, pluronic F127, and by adopting two different techniques, namely; solvent evaporation technique and fusion technique. A full factorial design of 2 3 was adopted to investigate the influence of formulation variables on the prepared nanodispersion properties. The best chosen formula of nanodispersed powder was formulated into tablets by direct compression. The Differential Scanning Calorimetry (DSC) analysis and Fourier Transform Infra-Red (FTIR) analysis were conducted for the thermal behavior and surface structure characterization, respectively. The zeta potential and particle size analysis of the prepared glimepiride nanodispersions was determined. The prepared solid nanodispersions and solid nanodispersed tablets of GMP were evaluated in terms of pre-compression and post-compression parameters, respectively. Results: The DSC and FTIR studies revealed that there was no interaction between GMP and all the excipients used. Based on the resulted values of different pre-compression parameters, the prepared solid nanodispersions powder blends showed poor to excellent flow properties. The resulted values of the other evaluated pre-compression parameters of the prepared solid nanodispersion were within the limits of pharmacopoeia. The drug content of the prepared nanodispersions ranged from 89.6 ± 0.3 % to 99.9± 0.5% with particle size ranged from 111.5 nm to 492.3 nm and the resulted zeta potential (ζ ) values of the prepared GMP-solid nanodispersion formulae (F1-F8) ranged from -8.28±3.62 mV to -78±11.4 mV. The in-vitro dissolution studies of the prepared solid nanodispersed tablets of GMP concluded that GMP- pluronic F127 combinations (F8), exhibited the best extent of drug release, compared to other formulations, and to the marketed product. One way ANOVA for the percent of drug released from the prepared GMP-nanodispersion formulae (F1- F8) after 20 and 60 minutes showed significant differences between the percent of drug released from different GMP-nanodispersed tablet formulae (F1- F8), (P<0.05). Conclusion: Preparation of glimepiride as nanodispersed particles proven to be a promising tool for enhancing the poor solubility of glimepiride.

Keywords: glimepiride, solid Nanodispersion, nanodispersed tablets, poorly water soluble drugs

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Authors: Bagnoud-Velásquez Mariluz, Damergi Eya, Grandjean Dominique, Frédéric Vogel, Ludwig Christian

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The sustainability of algae to biofuel processes is seriously affected by the energy intensive production of fertilizers. Large amounts of nitrogen and phosphorus are required for a large-scale production resulting in many cases in a negative impact of the limited mineral resources. In order to meet the algal bioenergy opportunity it appears crucial the promotion of processes applying a nutrient recovery and/or making use of renewable sources including waste. Hydrothermal (HT) conversion is a promising and suitable technology for microalgae to generate biofuels. Besides the fact that water is used as a “green” reactant and solvent and that no biomass drying is required, the technology offers a great potential for nutrient recycling. This study evaluated the possibility to treat the water HT effluent by the growth of microalgae while producing renewable algal biomass. As already demonstrated in previous works by the authors, the HT aqueous product besides having N, P and other important nutrients, presents a small fraction of organic compounds rarely studied. Therefore, extracted heteroaromatic compounds in the HT effluent were the target of the present research; they were profiled using GC-MS and LC-MS-MS. The results indicate the presence of cyclic amides, piperazinediones, amines and their derivatives. The most prominent nitrogenous organic compounds (NOC’s) in the extracts were carefully examined by their effect on microalgae, namely 2-pyrrolidinone and β-phenylethylamine (β-PEA). These two substances were prepared at three different concentrations (10, 50 and 150 ppm). This toxicity bioassay used three different microalgae strains: Phaeodactylum tricornutum, Chlorella sorokiniana and Scenedesmus vacuolatus. The confirmed IC50 was for all cases ca. 75ppm. Experimental conditions were set up for the growth of microalgae in the aqueous phase by adjusting the nitrogen concentration (the key nutrient for algae) to fit that one established for a known commercial medium. The values of specific NOC’s were lowered at concentrations of 8.5 mg/L 2-pyrrolidinone; 1mg/L δ-valerolactam and 0.5 mg/L β-PEA. The growth with the diluted HT solution was kept constant with no inhibition evidence. An additional ongoing test is addressing the possibility to apply an integrated water cleanup step making use of the existent hydrothermal catalytic facility.

Keywords: hydrothermal process, microalgae, nitrogenous organic compounds, nutrient recovery, renewable biomass

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Authors: Lynda K. Eneh, Okal N. Mike, Anna-Karin Borg-Karlson, Ulrike Fillinger, Jenny M. Lindh

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The responses of individual gravid Anopheles gambiae sensu stricto (s.s.) to hay infusion volatiles were evaluated under laboratory conditions. Such infusions have long been known to be effective baits for monitoring mosquitoes that vector arboviral and filarial diseases but have previously not been tested for malaria vectors. Hay infusions were prepared by adding sun-dried Bermuda grass to lake water and leaving the mixture in a covered bucket for three days. The proportions of eggs laid by gravid An. gambiae s.s. in diluted (10%) and concentrated infusions ( ≥ 25%) was compared to that laid in lake water in two-choice egg-count bioassays. Furthermore, with the aim to develop a method that can be used to collect volatiles that influence the egg-laying behavior of malaria mosquitoes, different volatile trapping methods were investigated. Two different polymer-traps eluted using two different desorption methods and three parameters were investigated. Porapak®-Q traps and solvent desorption was compared to Tenax®-TA traps and thermal desorption. The parameters investigated were: collection time (1h vs. 20h), addition of salt (0.15 g/ml sodium chloride (NaCl) vs. no NaCl), and stirring the infusion (0 vs. 300 rpm). Sample analysis was with gas chromatography-mass spectrometry (GC-MS). An. gambiae s.s was ten times less likely to lay eggs in concentrated hay infusion than in lake water. The volatiles were best characterized by thermally desorbed Tenax traps, collected for 20 hours from infusion aliquots with sodium chloride added. Ten volatiles identified from headspace and previously indicated as putative oviposition semiochemicals for An. gambiae s.s. or confirmed semiochemicals for other mosquito species were tested in egg-count bioassays. Six of these (3-methylbutanol, phenol, 4-methylphenol, nonanal, indole and 3-methylindole), when added to lake water, were avoided for egg-laying when lake water was offered as the alternative in dual-choice egg count bioassays. These compounds likely contribute to the unfavorable oviposition responses towards hay infusions. This difference in oviposition response of different mosquito species should be considered when designing control measures.

Keywords: Anopheles gambiae, oviposition behaviour, egg-count cage bioassays, hay infusions, volatile detection, semiochemicals

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Authors: Hamed Movahedi, Nicolas Bovet, Henning Friis Poulsen

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Following the advent of the Industrial Revolution, there has been a significant increase in the extraction and utilization of hydrocarbon and fossil fuel resources. However, a new era has emerged, characterized by a shift towards sustainable practices, namely the reduction of carbon emissions and the promotion of renewable energy generation. Given the substantial number of mature oil and gas wells that have been developed inside the petroleum reservoir domain, it is imperative to establish an environmental strategy and adopt appropriate measures to effectively seal and decommission these wells. In general, the cement plug serves as a material for plugging purposes. Nevertheless, there exist some scenarios in which the durability of such a plug is compromised, leading to the potential escape of hydrocarbons via fissures and fractures within cement plugs. Furthermore, cement is often not considered a practical solution for temporary plugging, particularly in the case of well sites that have the potential for future gas storage or CO2 injection. The Danish oil and gas industry has promising potential as a prospective candidate for future carbon dioxide (CO2) injection, hence contributing to the implementation of carbon capture strategies within Europe. The primary reservoir component consists of chalk, a rock characterized by limited permeability. This work focuses on the development and characterization of a novel hydrogel variant. The hydrogel is designed to be injected via a low-permeability reservoir and afterward undergoes a transformation into a high-viscosity gel. The primary objective of this research is to explore the potential of this hydrogel as a new solution for effectively plugging well flow. Initially, the synthesis of polyacrylamide was carried out using radical polymerization inside the confines of the reaction flask. Subsequently, with the application of the Hoffman rearrangement, the polymer chain undergoes partial amination, facilitating its subsequent reaction with the crosslinker and enabling the formation of a hydrogel in the subsequent stage. The organic crosslinker, glutaraldehyde, was employed in the experiment to facilitate the formation of a gel. This gel formation occurred when the polymeric solution was subjected to heat within a specified range of reservoir temperatures. Additionally, a rheological survey and gel time measurements were conducted on several polymeric solutions to determine the optimal concentration. The findings indicate that the gel duration is contingent upon the starting concentration and exhibits a range of 4 to 20 hours, hence allowing for manipulation to accommodate diverse injection strategies. Moreover, the findings indicate that the gel may be generated in environments characterized by acidity and high salinity. This property ensures the suitability of this substance for application in challenging reservoir conditions. The rheological investigation indicates that the polymeric solution exhibits the characteristics of a Herschel-Bulkley fluid with somewhat elevated yield stress prior to solidification.

Keywords: polyacrylamide, hofmann rearrangement, rheology, gel time

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Authors: Arezoo Rahmani, Rinez Thapa, Juha-Matti Aalto, Petri Turhanen, Jouko Vepsalainen, Vesa-PekkaLehto, Joakim Riikonen

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Production of Scandium (Sc) is a complicated process because Sc is found only in low concentrations in ores and the concentration of Sc is very low compared with other metals. Therefore, utilization of typical extraction processes such as solvent extraction is problematic in scandium extraction. The Adsorption/desorption method can be used, but it is challenging to prepare materials, which have good selectivity, high adsorption capacity, and high stability. Therefore, efficient and environmentally friendly methods for Sc extraction are needed. In this study, the nanoporous composite material was developed for extracting Sc from an Sc ore. The nanoporous composite material offers several advantageous properties such as large surface area, high chemical and mechanical stability, fast diffusion of the metals in the material and possibility to construct a filter out of the material with good flow-through properties. The nanoporous silicon material was produced by first stabilizing the surfaces with a silicon carbide layer and then functionalizing the surface with bisphosphonates that act as metal chelators. The surface area and porosity of the material were characterized by N₂ adsorption and the morphology was studied by scanning electron microscopy (SEM). The bisphosphonate content of the material was studied by thermogravimetric analysis (TGA). The concentration of metal ions in the adsorption/desorption experiments was measured with inductively coupled plasma mass spectrometry (ICP-MS). The maximum capacity of the material was 25 µmol/g Sc at pH=1 and 45 µmol/g Sc at pH=3, obtained from adsorption isotherm. The selectivity of the material towards Sc in artificial solutions containing several metal ions was studied at pH one and pH 3. The result shows good selectivity of the nanoporous composite towards adsorption of Sc. Scandium was less efficiently adsorbed from solution leached from the ore of Sc because of excessive amounts of iron (Fe), aluminum (Al) and titanium (Ti) which disturbed the adsorption process. For example, the concentration of Fe was more than 4500 ppm, while the concentration of Sc was only three ppm, approximately 1500 times lower. Precipitation methods were developed to lower the concentration of the metals other than Sc. Optimal pH for precipitation was found to be pH 4. The concentration of Fe, Al and Ti were decreased by 99, 70, 99.6%, respectively, while the concentration of Sc decreased only 22%. Despite the large reduction in the concentration of other metals, more work is needed to further increase the relative concentration of Sc compared with other metals to efficiently extract it using the developed nanoporous composite material. Nevertheless, the developed material may provide an affordable, efficient and environmentally friendly method to extract Sc on a large scale.

Keywords: adsorption, nanoporous silicon, ore solution, scandium

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Authors: Adam Fheed

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Carbonate porosity can be deceptive in the aspect of hydrocarbon exploration due to pore geometry variations, which are to some extent controlled by fossils. Therefore, the main aim of this paper was to assess the dependence of pore geometry and reservoir quality on fossils. The Permian Zechstein Limestone (Ca1) carbonates from the Brońsko Reef, located on the Wolsztyn Ridge in West Poland, were examined. Seventy meters of drill cores were described along with well log examination and transmitted-light microscope research. The archival porosity-permeability data was utilized to calibrate the well logs and look for the potential petrophysical trends. Several organism assemblages were recognized in the reef. Its bottom was colonized by the branched bryozoans which were fragmented and dissolved leaving poorly connected molds. Subsequently, numerous bivalves and gastropods appeared and their shells were heavily dissolved to form huge, albeit poorly communicated caverns. Such pores were also typical for local brachiopod occurrences. Although the caverns were widespread, and probably linked to the meteoric dissolution or freshwater flushing, severe anhydrite cementation has destroyed the majority of pores. Close to the top of Ca1, near the center of the reef, the fossil-rich zone comprising fenestrate bryozoans, extremely abundant encrusting foraminifers, bivalves, brachiopods, gastropods and ostracods, was identified. The zone contained extremely frequent dissolution channels formed within former shells of foraminifers, which had previously encrusted the bryozoans. The deposition of Ca1 strata has ultimately terminated with a poorly porous and generally impermeable stromatolitic layer containing scarce fossils. In general, the permeability of the reef rocks studied turned out to be the highest under the presence of foraminifer-related channels. In such cases, it frequently approached 100 mD. The presence of channels and other pores gave the average effective porosity derived from shallow resistivity and helium porosimetry of around 16 and 18 %, respectively. The highest porosity (over 18 %), often co-occurring with relatively low permeability (chiefly below 20 mD) was noted for the bottommost zone of the reef, represented by branched bryozoans. This is probably owing to a large amount of unconnected bryozoan-related molds. It was concluded that fossils played a major role in porosity formation and controlled the pore geometry significantly. While the dissolution of bivalves and brachiopods resulted in cavernous porosity formation, numerous molds were typically related with the alteration of branched bryozoans, gastropods and ostracods. Importantly, the bendy dissolution channels after the encrusting foraminifers appeared to be decisive in improving reservoir quality – specifically when permeability is considered. Acknowledgment: The research was financed by the Polish National Science Centre’s project No. UMO-2016/23/N/ST10/00350.

Keywords: dissolution channels, fossils, Permian, porosity

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Authors: Mihail Simion Beldean-Galea, Virginia Coman, Florina Copaciu, Mihaela Vlassa, Radu Mihaiescu, Adina Croitoru, Viorel Arghius, Modest Gertsiuk, Mikola Gertsiuk

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Taking into consideration the huge number of chemicals released into environment compartments a proper environmental risk assessment is difficult to predict due to the gap of legislation and improper toxicological assessment of chemicals compounds. In Romania as well as in many other countries from Europe, the chemical status of the water body is characterized taking into consideration the Water Framework Directive (WFD) and the substances listed in Annex X. This Annex includes 45 substances from different classes of organic compounds and heavy metals for which AA-EQS and MAC-EQS have been established. For other compounds which are not included in Annex X, different methodologies to prioritize chemicals for risk assessment and monitoring has been proposed. These methodologies take into account Predicted No-Effect Concentrations (PNECs) of different classes of chemicals compounds available from existing risk assessments or from read-across models for acute toxicity to the standard test organisms such as Daphnia magna and Selenastrum capricornutum. Our work presents the monitoring results of 30 priority substances including polyaromatic hydrocarbons, pesticides, halogenated compounds, plasticizers and heavy metals and other 34 substances from different classes of pesticides and pharmaceuticals which are not included on the list of priority substances, performed in the Upper Tisza River Watershed from Romania and Ukraine. The obtained monitoring data were used for the establishment of the list of more relevant pollutants in the studied area and to establish the potential river basin specific pollutants. For this purpose, two indicators such as the Frequency of exceedance and Extent of exceedance of Predicted no-Effect Concentration (PNEC) were evaluated. These two indicators are based on maximum environmental concentrations (MECs) of priority substances and for other pollutants is use statistically based averages of obtained measured concentration compared to the lowest PNEC thresholds. From the obtained results it can be concluded that polyaromatic hydrocarbon such as Fluoranthene, Benzo[a]pyrene, Benzo[b]fluorathene, benzo[k]fluoranthene, Benzo(g.h.i)perylene, Indeno(1.2.3-cd)-pyrene, heavy metals such as Cadmium, Lead and Nickel can be considered as river basin specific pollutants, their concentration exceeding the Annual Average EQS concentration. Other compounds such as estrone, estriol, 174-β estradiol, naproxen or some antibiotics (Penicillin G, Tetracycline or Ceftazidime) should be taken into account for a long monitoring, in some cases their concentration exceeding PNEC. Acknowledgements: This work is performed in the frame of NATO SfP Programme, Project no. 984440.

Keywords: prioritization, river basin specific pollutants, Tisza River, water framework directive

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Authors: Iwona Misztalewska-Turkowicz, Agnieszka Z. Wilczewska, Karolina H. Markiewicz

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Carbenes - species which possess neutral carbon atom with two shared and two unshared valence electrons, are known for their high reactivity and instability. Nevertheless, it is also known, that some carbenes i.e. N-heterocyclic carbenes (NHCs), can form stable crystals. The usability of NHCs in organic synthesis was studied. Due to their exceptional properties (high nucleophilicity) NHCs are commonly used as organocatalysts and also as ligands in transition metal complexes. NHC ligands possess better electron-donating properties than phosphines. Moreover, they exhibit lower toxicity. Due to these features, phosphines are frequently replaced by NHC ligands. In this research is discussed the synthesis of five-membered NHCs which are mainly obtained by deprotonation of azolium salts, e.g., imidazolium or imidazolinium salts. Some of them are immobilized on a solid support what leads to formation of heterogeneous, recyclable catalysts. Magnetic nanoparticles (MNPs) are often used as a solid support for catalysts. MNPs can be easily separated from the reaction mixture using an external magnetic field. Due to their low size and high surface to volume ratio, they are a good choice for immobilization of catalysts. Herein is presented synthesis of N-heterocyclic carbene copper complexes directly on the surface of magnetic nanoparticles. Formation of four different catalysts is discussed. They vary in copper oxidation state (Cu(I) and Cu(II)) and structure of NHC ligand. Catalysts were tested in Huisgen reaction, a type of copper catalyzed azide-alkyne cycloaddition (CuAAC) reaction. Huisgen reaction represents one of the few universal and highly efficient reactions in which 1,2,3-triazoles can be obtained. The catalytic activity of all synthesized catalysts was compared with activity of commercially available ones. Different reaction conditions (solvent, temperature, the addition of reductant) and reusability of the obtained catalysts were investigated and are discussed. The project was financially supported by National Science Centre, Poland, grant no. 2016/21/N/ST5/01316. Analyses were performed in Centre of Synthesis and Analyses BioNanoTechno of University of Bialystok. The equipment in the Centre of Synthesis and Analysis BioNanoTechno of University of Bialystok was funded by EU, as a part of the Operational Program Development of Eastern Poland 2007-2013, project: POPW.01.03.00-20-034/09-00 and POPW.01.03.00-20-004/11.

Keywords: N-heterocyclic carbenes, click reaction, magnetic nanoparticles, copper catalysts

Procedia PDF Downloads 157

Authors: Sai Snehitha Yadavalli, K. Sruthi, Swati Ghosh Acharyya

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Heavy metal ions are toxic to humans and all living species when exposed in large quantities or for long durations. Though Fe acts as a nutrient, when intake is in large quantities, it becomes toxic. These toxic heavy metal ions, when consumed through water, will cause many disorders and are harmful to all flora and fauna through biomagnification. Specifically, humans are prone to innumerable diseases ranging from skin to gastrointestinal, neurological, etc. In higher quantities, they even cause cancer in humans. Detection of these toxic heavy metal ions in water is thus important. Traditionally, the detection of heavy metal ions in water has been done by techniques like Inductively Coupled Plasma Mass Spectroscopy (ICPMS) and Atomic Absorption Spectroscopy (AAS). Though these methods offer accurate quantitative analysis, they require expensive equipment and cannot be used for on-site measurements. Anodic Stripping Voltammetry is a good alternative as the equipment is affordable, and measurements can be made at the river basins or lakes. In the current study, Square Wave Anodic Stripping Voltammetry (SWASV) was used to detect the heavy metal ions in water. Literature reports various electrodes on which deposition of heavy metal ions was carried out like Bismuth, Polymers, etc. The working electrode used in this study is a polyvinyl chloride (PVC) modified glassy carbon electrode (GCE). Ag/AgCl reference electrode and Platinum counter electrode were used. Biologic Potentiostat SP 300 was used for conducting the experiments. Through this work of simultaneous detection, four heavy metal ions were successfully detected at a time. The influence of modifying GCE with PVC was studied in comparison with unmodified GCE. The simultaneous detection of Cd⁺², Fe⁺², Co⁺², Pb⁺² heavy metal ions was done using PVC modified GCE by drop casting 1 wt.% of PVC dissolved in Tetra Hydro Furan (THF) solvent onto GCE. The concentration of all heavy metal ions was 0.2 mg/L, as shown in the figure. The scan rate was 0.1 V/s. Detection parameters like pH, scan rate, temperature, time of deposition, etc., were optimized. It was clearly understood that PVC helped in increasing the sensitivity and selectivity of detection as the current values are higher for PVC-modified GCE compared to unmodified GCE. The peaks were well defined when PVC-modified GCE was used.

Keywords: cadmium, cobalt, electrochemical sensing, glassy carbon electrodes, heavy metal Ions, Iron, lead, polyvinyl chloride, potentiostat, square wave anodic stripping voltammetry

Procedia PDF Downloads 104

Authors: Carlos Y. Soto, Camila A. Lota, G. Astrid Garzón

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Bacterial biofilms cause an ongoing problem for food safety. They are formed when microorganisms aggregate to form a community that attaches to solid surfaces. Biofilms increase the resistance of pathogens to cleaning, disinfection and antibacterial products. This resistance gives rise to problems for human health, industry, and agriculture. At present, plant extracts rich in polyphenolics are being investigated as natural alternatives to degrade bacterial biofilms. The pomace of the tropical Berry Vaccinium meridionale S. contains high amounts of phenolic compounds. Therefore, in the current study, the antimicrobial and antibiofilm effects of extracts from the pomace of Vaccinium meridionale S. were tested on three foodborne pathogens: Enterohaemorrhagic Escherichia coli O157:H7 (ATCC®700728TM), Staphylococcus aureus subsp. aureus (ATCC® 6538TM), and Salmonella enterica serovar Enteritidis (ATCC® 13076TM). Microwave-assisted extraction was used to extract polyphenols with aqueous methanol (80% v/v) at a solid to solvent ratio of 1:10 (w/v) for 20 min. The magnetic stirring was set at 400 rpm, and the microwave power was adjusted to 400 W. The antimicrobial effect of the extract was assessed by determining the half maximal inhibitory concentration (IC50) against the three food poisoning pathogens at concentrations ranging from 50 to 2,850 μg gallic acid equivalents (GAE)/mL of the extract. Biofilm inhibition was assessed using a crystal violet assay applying the same range of concentration. Three replications of the experiments were carried out, and all analyses were run in triplicate. IC50 values were determined using the GraphPad Prism8® program. Significant differences (P<0.05) among means were identified using one-factor analysis of variance (ANOVA) and the post-hoc least significant difference (LSD) test using the Statgraphics plus program, version 2.1.There was significant difference among the mean IC50 values for the tested bacteria. The IC50 for S. aureus was 48 ± 9 μg GAE/mL, followed by 123 ± 49 μg GAE/mL for Salmonella and 376 ± 32 μg GAE/mL for E. coli. The percent inhibition of the extract on biofilm formation was significantly higher for S. aureus (85.8  0.3), followed by E. coli (74.5  1.0) and Salmonella (53.6  9.7). These findings suggest that polyphenolic extracts obtained from the pomace of V. meridionale S. might be used as natural antimicrobial and anti-biofilm natural agents, effective against S. aureus, E. coli and Salmonella enterica.

Keywords: antibiofilm, antimicrobial, E. coli, S. aureus, salmonella, IC50, pomace, V. meridionale

Procedia PDF Downloads 63

Authors: Bharti Verma, Chandrajit Balomajumder

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Water pollution is escalated owing to industrialization and random ejection of one or more toxic heavy metal ions from the semiconductor industry, electroplating, metallurgical, mining, chemical manufacturing, tannery industries, etc., In semiconductor industry various kinds of chemicals in wafers preparation are used . Fluoride, toxic solvent, heavy metals, dyes and salts, suspended solids and chelating agents may be found in wastewater effluent of semiconductor manufacturing industry. Also in the chrome plating, in the electroplating industry, the effluent contains heavy amounts of Chromium. Since Cr(VI) is highly toxic, its exposure poses an acute risk of health. Also, its chronic exposure can even lead to mutagenesis and carcinogenesis. On the contrary, Cr (III) which is naturally occurring, is much less toxic than Cr(VI). Discharge limit of hexavalent chromium and trivalent chromium are 0.05 mg/L and 5 mg/L, respectively. There are numerous methods such as adsorption, chemical precipitation, membrane filtration, ion exchange, and electrochemical methods for the heavy metal removal. The present study focuses on the removal of Chromium ions by using flat sheet UF5kDa membrane. The Ultra filtration membrane process is operated above micro filtration membrane process. Thus separation achieved may be influenced due to the effect of Sieving and Donnan effect. Ultrafiltration is a promising method for the rejection of heavy metals like chromium, fluoride, cadmium, nickel, arsenic, etc. from effluent water. Benefits behind ultrafiltration process are that the operation is quite simple, the removal efficiency is high as compared to some other methods of removal and it is reliable. Polyamide membranes have been selected for the present study on rejection of Cr(VI) from feed solution. The objective of the current work is to examine the rejection of Cr(VI) from aqueous feed solutions by flat sheet UF5kDa membranes with different parameters such as pressure, feed concentration and pH of the feed. The experiments revealed that with increasing pressure, the removal efficiency of Cr(VI) is increased. Also, the effect of pH of feed solution, the initial dosage of chromium in the feed solution has been studied. The membrane has been characterized by FTIR, SEM and AFM before and after the run. The mass transfer coefficients have been estimated. Membrane transport parameters have been calculated and have been found to be in a good correlation with the applied model.

Keywords: heavy metal removal, membrane process, waste water treatment, ultrafiltration

Procedia PDF Downloads 141

Authors: Marcin Debowski, Marcin Zielinski, Miroslaw Krzemieniewski, Agata Glowacka-Gil, Paulina Rusanowska, Magdalena Zielinska, Agnieszka Cydzik-Kwiatkowska

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Technologies of biogas upgrading are now perceived as competitive solution combustion and production of electricity and heat. Biomethane production will ensure broader application as energy carrier than biogas. Biomethane can be used as fuel in internal combustion engines or introduced into the natural gas transmission network. Therefore, there is a need to search for innovative, economically and technically justified methods for biogas enrichment. The aim of this paper is to present a technology solution for biogas upgrading with immobilized algae biomass. Reactor for biogas upgrading with immobilized algae biomass can be used for removing CO₂ from the biogas, flue gases and the waste gases especially coming from different industry sectors, e.g. from the food industry from yeast production process, biogas production systems, liquid and gaseous fuels combustion systems, hydrocarbon processing technology. The basis for the technological assumptions of presented technology were laboratory works and analyses that tested technological variants of biogas upgrading. The enrichment of biogas with a methane content of 90-97% pointed to technological assumptions for installation on a technical scale. Reactor for biogas upgrading with algae biomass is characterized by a significantly lower cubature in relation to the currently used solutions which use CO₂ removal processes. The invention, by its structure, assumes achieving a very high concentration of biomass of algae through its immobilization in capsules. This eliminates the phenomenon of lowering the pH value, i.e. acidification of the environment in which algae grow, resulting from the introduction of waste gases at a high CO₂ concentration. The system for introducing light into algae capsules is characterized by a higher degree of its use, due to lower losses resulting from the phenomenon of absorption of light energy by water. The light from the light source is continuously supplied to the formed biomass of algae or cyanobacteria in capsules by the light tubes. The light source may be sunlight or a light generator of a different wavelength of light from 300 nm to 800 nm. A portion of gas containing CO₂, accumulated in the tank and conveyed by the pump is periodically introduced into the housing of the photobioreactor tank. When conveying the gas that contains CO₂, it penetrates the algal biomass in capsules through the outer envelope, displacing, from the algal biomass, gaseous metabolic products which are discharged by the outlet duct for gases. It contributes to eliminating the negative impact of this factor on CO₂ binding processes. As a result of the cyclic dosing of gases containing carbon dioxide, gaseous metabolic products of algae are displaced and removed outside the technological system. Technology for biogas upgrading with immobilized algae biomass is suitable for the small biogas plant. The advantages of this technology are high efficiency as well as useful algae biomass which can be used mainly as animal feed, fertilizers and in the power industry. The construction of the device allows effective removal of carbon dioxide from gases at a high CO₂ concentration.

Keywords: biogas, carbon dioxide, immobilised biomass, microalgae, upgrading

Procedia PDF Downloads 157

Authors: Raka Rahmatulloh, Mohammad Ilham Nugraha, Muhammad Ifan Fathurrahman

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The agricultural sector covers a wide area, one of them is livestock subsector that supply needs of the food source of animal protein. Animal protein is produced by the main livestock production such as meat, milk, eggs, etc. Besides the main production, livestock would produce metabolic residue, so called livestock wastes. Characteristics of livestock wastes can be either solid (feces), liquid (urine), and gas (methane) which turned out to be useful and has economical value when well-processed and well-controlled. Nowadays, this livestock wastes is considered as a source of pollutants, especially water pollution. If the source of pollutants used in an integrated way, it will have a positive impact on organic farming and a healthy environment. Management of livestock wastes can be integrated with the farming sector to the planting and caring that rely on fertilizers. Most Indonesian farmers still use chemical fertilizers, where the use of it in the long term will disturb the ecological balance of the environment. One of the main efforts is to use organic fertilizers instead of chemical fertilizer that conducted by the Faculty of Animal Husbandry, Padjadjaran University. The method is to use the solid waste of livestock and agricultural wastes into liquid organic fertilizer, feed additive, biogas and vermicompost through decomposition. The decomposition takes as long as 14 days including aeration and extraction process using water as a nutrients solvent media which contained in decomposes and disinfection media to release pathogenic microorganisms in decomposes. Liquid organic fertilizer has highly efficient for the farmers to have a ratio of carbon/nitrogen (C/N) 25/1 to 30/1 and neutral pH (6.5-7.5) which is good for plant growth. Feed additive may be given to improve the digestibility of feed so that substances can be easily absorbed by the body for production. Biogas contains methane (CH4), which has a high enough heat to produce electricity. Vermicompost is an overhaul of waste organic material that has excellent structure, porosity, aeration, drainage, and moisture holding capacity. Based on the case study above, an integrated livestock wastes management program strongly supports the Indonesian government in the achievement of sustainable livestock development.

Keywords: integrated, livestock wastes, organic fertilizer, sustainable livestock development

Procedia PDF Downloads 435

Authors: Attila Kiss, Erzsébet Némedi, Zoltán Naár

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As natural prebiotic (non-digestible) carbohydrates stimulate the growth of colon microflora and contribute to maintain the health of the host, analytical studies aiming at revealing the chemical behavior of these beneficial food components came to the forefront of interest. Food processing (especially baking) may lead to a significant conversion of the parent compounds, hence it is of utmost importance to characterize the transformation patterns and the plausible decomposition products formed by thermal degradation. The relevance of this work is confirmed by the wide-spread use of these carbohydrates (fructo-oligosaccharides, cyclodextrins, raffinose and resistant starch) in the food industry. More and more functional foodstuffs are being developed based on prebiotics as bioactive components. 12 different types of oligosaccharides have been investigated in order to reveal their thermal degradation characteristics. Different carbohydrate derivatives (D-fructose and D-glucose oligomers and polymers) have been exposed to elevated temperatures (150 °C 170 °C, 190 °C, 210 °C, and 220 °C) for 10 min. An advanced HPLC method was developed and used to identify the decomposition products of carbohydrates formed as a consequence of thermal treatment. Gradient elution was applied with binary solvent elution (acetonitrile, water) through amine based carbohydrate column. Evaporative light scattering (ELS) proved to be suitable for the reliable detection of the UV/VIS inactive carbohydrate degradation products. These experimental conditions and applied advanced techniques made it possible to survey all the formed intermediers. Change in oligomer distribution was established in cases of all studied prebiotics throughout the thermal treatments. The obtained results indicate increased extent of chain degradation of the carbohydrate moiety at elevated temperatures. Prevalence of oligomers with shorter chain length and even the formation of monomer sugars (D-glucose and D-fructose) might be observed at higher temperatures. Unique oligomer distributions, which have not been described previously are revealed in the case of each studied, specific carbohydrate, which might result in various prebiotic activities. Resistant starches exhibited high stability when being thermal treated. The degradation process has been modeled by a plausible reaction mechanism, in which proton catalyzed degradation and chain cleavage take place.

Keywords: prebiotics, thermal degradation, fructo-oligosaccharide, HPLC, ELS detection

Procedia PDF Downloads 306

Authors: Lucero Gonzalez, Salvador Alfaro

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Carbon dioxide (CO2) and methane (CH4) are considered as the compounds with higher abundance among the greenhouse gases (CO2, NOx, SOx, CxHx, etc.), due to its higher concentration, this two gases have a greater impact in the environment pollution and provokes global warming. So, recovery, disposal and subsequent reuse, are of great interest, especially from the ecological and health perspective. By one hand, porous inorganic materials are good candidates to capture gases, because these type of materials are higher stability from the point view of thermal, chemical and mechanical under adsorption gas processes. By another hand, during the design and the synthetic preparation of the porous materials is possible add other intrinsic properties (physicochemical and structural) by adding chemical compounds as dopants or using structured directed agents or surfactants to improve the porous structure, the above features allow to have alternative materials for separation, capture and storage of greenhouse gases. In this work, ordered mesoporous materials base silica were prepared using Surfynol as surfactant. The surfactant micelles are commonly used as self-assembly templates for the development of new structure porous silica’s, adding a variety of textures and structures. By another hand, the Surfynol is a commercial surfactant, is non-ionic, for that is necessary determine its critical micelles concentration (cmc) by the pyrene I1/I3 ratio method, before to prepare silica particles. One time known the CMC, a precursor gel was prepared via sol-gel process at room temperature using TEOS as silica precursor, NH4OH as catalyst, Surfynol as template and H2O as solvent. Then, the gel precursor was treatment hydrothermally in a Teflon-lined stainless steel autoclave with a volume of 100 mL and kept at 100 ºC for 24 h under static conditions in a convection oven. After that, the porous silica particles obtained were impregnated with lithium to improve the CO2 adsorption capacity. Then the silica particles were characterized physicochemical, morphology and structurally, by XRD, FTIR, BET and SEM techniques. The thermal stability and the CO2 adsorption capacity was evaluated by thermogravimetric analysis (TGA). According the results, we found that the Surfynol is a good candidate to prepare silica particles with an ordered structure. Also the TGA analysis shown that the particles has a good thermal stability in the range of 250 °C and 800 °C. The best materials had, the capacity to adsorbing 70 and 90 mg per gram of silica particles and its CO2 adsorption capacity depends on the way to thermal pretreatment of the porous silica before of the adsorption experiments and of the concentration of surfactant used during the synthesis of silica particles. Acknowledgments: This work was supported by SIP-IPN through project SIP-20161862.

Keywords: CO2 adsorption, lithium as dopant, porous silica, surfynol as surfactant, thermogravimetric analysis

Procedia PDF Downloads 269

Authors: Riddhiman Sherlekar, Umang Paladia, Rachit Desai, Yash Patel

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A number of surfactants which exhibit ultra-low interfacial tension and an excellent microemulsion phase behavior with crude oils of low to medium gravity are not sufficiently soluble at optimum salinity to produce stable aqueous solutions. Such solutions often show phase separation after a few days at reservoir temperature, which does not suffice the purpose and the time is short when compared to the residence time in a reservoir for a surfactant flood. The addition of polymer often exacerbates the problem although the poor stability of the surfactant at high salinity remains a pivotal issue. Surfactants such as SDS, Ctab with large hydrophobes produce lowest IFT, but are often not sufficiently water soluble at desired salinity. Hydrophilic co-solvents and/or co-surfactants are needed to make the surfactant-polymer solution stable at the desired salinity. This study focuses on contrasting the effect of addition of a co-solvent in stability of a surfactant –oil emulsion. The idea is to use a co-surfactant to increase stability of an emulsion. Stability of the emulsion is enhanced because of creation of micro-emulsion which is verified both visually and with the help of particle size analyzer at varying concentration of salinity, surfactant and co-surfactant. A lab-experimental method description is provided and the method is described in detail to permit readers to emulate all results. The stability of the oil-water emulsion is visualized with respect to time, temperature, salinity of the brine and concentration of the surfactant. Nonionic surfactant TX-100 when used as a co-surfactant increases the stability of the oil-water emulsion. The stability of the prepared emulsion is checked by observing the particle size distribution. For stable emulsion in volume% vs particle size curve, the peak should be obtained for particle size of 5-50 nm while for the unstable emulsion a bigger sized particles are observed. The UV-Visible spectroscopy is also used to visualize the fraction of oil that plays important role in the formation of micelles in stable emulsion. This is important as the study will help us to decide applicability of the surfactant based EOR method for a reservoir that contains a specific type of crude. The use of nonionic surfactant as a co-surfactant would also increase the efficiency of surfactant EOR. With the decline in oil discoveries during the last decades it is believed that EOR technologies will play a key role to meet the energy demand in years to come. Taking this into consideration, the work focuses on the optimization of the secondary recovery(Water flooding) with the help of surfactant and/or co-surfactants by creating desired conditions in the reservoir.

Keywords: co-surfactant, enhanced oil recovery, micro-emulsion, surfactant flooding

Procedia PDF Downloads 252

Authors: Vivek Rangarajan, Kim G. Clarke

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Bacillus lipopeptides are biosurfactants with wide ranging applications in the medical, food, agricultural, environmental and cosmetic industries. They are produced as a mix of three families, surfactin, iturin and fengycin, each comprising a large number of homologues of varying functionalities. Consequently, the method and degree of purification of the lipopeptide cocktail becomes particularly important if the functionality of the lipopeptide end-product is to be maximized for the specific application. However, downstream processing of Bacillus lipopeptides is particularly challenging due to the subtle variations observed in the different lipopeptide homologues and isoforms. To date, the most frequently used lipopeptide purification operations have been acid precipitation, solvent extraction, membrane ultrafiltration, adsorption and size exclusion. RP-HPLC (reverse phase high pressure liquid chromatography) also has potential for fractionation of the lipopeptide homologues. In the studies presented here, membrane ultrafiltration and RP-HPLC were evaluated for lipopeptide purification to different degrees of purities for maximum functionality. Batch membrane ultrafiltration using 50 kDa polyether sulphone (PES) membranes resulted in lipopeptide recovery of about 68% for surfactin and 82 % for fengycin. The recovery was further improved to 95% by using size-conditioned lipopeptide micelles. The conditioning of lipopeptides with Ca2+ ions resulted in uniformly sized micelles with average size of 96.4 nm and a polydispersity index of 0.18. The size conditioning also facilitated removal of impurities (molecular weight ranging between 2335-3500 Da) through operation of the system under dia-filtration mode, in a way similar to salt removal from protein by dialysis. The resultant purified lipopeptide was devoid of macromolecular impurities and could ideally suit applications in the cosmetic and food industries. Enhanced purification using RP-HPLC was carried out in an analytical C18 column, with the aim to fractionate lipopeptides into their constituent homologues. The column was eluted with mobile phase comprising acetonitrile and water over an acetonitrile gradient, 35% - 80%, over 70 minutes. The gradient elution program resulted in as many as 41 fractions of individual lipopeptide homologues. The efficacy test of these fractions against fungal phytopathogens showed that first 21 fractions, identified to be homologues of iturins and fengycins, displayed maximum antifungal activities, suitable for biocontrol in the agricultural industry. Thus, in the current study, the downstream processing of lipopeptides leading to tailor-made products for selective applications was demonstrated using two major downstream unit operations.

Keywords: bacillus lipopeptides, membrane ultrafiltration, purification, RP-HPLC

Procedia PDF Downloads 205

Authors: Natarajan Ramasamy, Gurulingamurthy Haralur, Ramesh Nivarthu, Nikhil Kumar Singha

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Elastomers are polymeric materials with varied backbone architectures ranging from linear to dendrimeric structures and wide varieties of monomeric repeat units. These elastomers show strongly viscous and weakly elastic when it is not cross-linked. But when crosslinked, based on the extent the properties of these elastomers can range from highly flexible to highly stiff nature. Lightly cross-linked systems are well studied and reported. Understanding the nature of highly cross-linked rubber based upon chemical structure and architecture is critical for varieties of applications. One of the critical parameters is cross-link density. In the current work, we have studied the highly cross-linked state of linear, lightly branched to star-shaped branched elastomers and determined the cross-linked density by using different models. Change in hardness, shift in Tg, change in modulus and swelling behavior were measured experimentally as a function of the extent of curing. These properties were analyzed using varied models to determine cross-link density. We used hardness measurements to examine cure time. Hardness to the extent of curing relationship is determined. It is well known that micromechanical transitions like Tg and storage modulus are related to the extent of crosslinking. The Tg of the elastomer in different crosslinked state was determined by DMA, and based on plateau modulus the crosslink density is estimated by using Nielsen’s model. Usually for lightly crosslinked systems, based on equilibrium swelling ratio in solvent the cross link density is estimated by using Flory–Rhener model. When it comes to highly crosslinked system, Flory-Rhener model is not valid because of smaller chain length. So models based on the assumption of polymer as a Non-Gaussian chain like 1) Helmis–Heinrich–Straube (HHS) model, 2) Gloria M.gusler and Yoram Cohen Model, 3) Barbara D. Barr-Howell and Nikolaos A. Peppas model is used for estimating crosslink density. In this work, correction factors are determined to the existing models and based upon it structure-property relationship of highly crosslinked elastomers was studied.

Keywords: dynamic mechanical analysis, glass transition temperature, parts per hundred grams of rubber, crosslink density, number of networks per unit volume of elastomer

Procedia PDF Downloads 166

Authors: Ana Carolina Kogawa, Selma Gutierrez Antonio, Hérida Regina Nunes Salgado

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Rifaximin is an oral antimicrobial, gut - selective and not systemic with adverse effects compared to placebo. It is used for the treatment of hepatic encephalopathy, travelers diarrhea, irritable bowel syndrome, Clostridium difficile, ulcerative colitis and acute diarrhea. The crystalline form present in the rifaximin with minimal systemic absorption is α, being the amorphous form significantly different. Regulators are increasingly attention to polymorphisms. Polymorphs can change the form by altering the drug characteristics compromising the effectiveness and safety of the finished product. International Conference on Harmonization issued the ICH Guidance Q6A, which aim to improve the control of polymorphism in new and existing pharmaceuticals. The objective of this study was to obtain polymorphic forms of rifaximin employing recrystallization processes and characterize them by thermal analysis (thermogravimetry - TG and differential scanning calorimetry - DSC), X-ray diffraction, scanning electron microscopy and solubility test. Six polymorphic forms of rifaximin, designated I to VI were obtained by the crystallization process by evaporation of the solvent. The profiles of the TG curves obtained from polymorphic forms of rifaximin are similar to rifaximin and each other, however, the DTG are different, indicating different thermal behaviors. Melting temperature values of all the polymorphic forms were greater to that shown by the rifaximin, indicating the higher thermal stability of the obtained forms. The comparison of the diffractograms of the polymorphic forms of rifaximin with rifaximin α, β and γ constant in patent indicate that forms III, V and VI are formed by mixing polymorph β and α and form III is formed by polymorph β. The polymorphic form I is formed by polymorph β, but with a significant amount of amorphous material. Already, the polymorphic form II consists of polymorph γ, amorphous. In scanning electron microscope is possible to observe the heterogeneity of morphological characteristics of crystals of polymorphic forms among themselves and with rifaximin. The solubility of forms I and II was greater than the solubility of rifaximin, already, forms III, IV and V presented lower solubility than of rifaximin. Similarly, the bioavailability of the amorphous form of rifaximin is considered significantly higher than the form α, the polymorphic forms obtained in this work can not guarantee the excellent tolerability of the reference medicine. Therefore, studies like these are extremely important and they point to the need for greater requirements by the regulatory agencies competent about polymorphs analysis of the raw materials used in the manufacture of medicines marketed globally. These analyzes are not required in the majority of official compendia. Partnerships between industries, research centers and universities would be a viable way to consolidate researches in this area and contribute to improving the quality of solid drugs.

Keywords: electronic microscopy, polymorphism, rifaximin, solubility, X-ray diffraction

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Authors: E Tolufase

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The demand, high costs and health implications of using energy derived from hydrocarbon compound have necessitated the continuous search for alternative source of energy. The World energy market is facing some challenges viz: depletion of fossil fuel reserves, population explosion, lack of energy security, economic and urbanization growth and also, in Nigeria some rural areas still depend largely on wood, charcoal, kerosene, petrol among others, as the sources of their energy. To overcome these short falls in energy supply and demand, as well as taking into consideration the risks from global climate change due to effect of greenhouse gas emissions and other pollutants from fossil fuels’ combustion, brought a lot of attention on efficiently harnessing the renewable energy sources. A very promising among the renewable energy resources for a clean energy technology for power production, vehicle and domestic usage is biogas. Therefore, optimization of biogas yield and quality is imperative. Hence, this study investigated yield and quality of biogas using low cost bio-digester and combination of various feed stocks referred to as co-digestion. Batch/Discontinuous Bio-digester type was used because it was cheap, easy, plausible and appropriate for different substrates used to get the desired results. Three substrates were used; cow dung, chicken droppings and lemon grass digested in five separate 21 litre digesters, A, B, C, D, and E and the gas collection system was designed using locally available materials. For single digestion we had; cow dung, chicken droppings, lemon grass, in Bio-digesters A, B, and C respectively, the co-digested three substrates in different mixed ratio 7:1:2 in digester D and E in ratio 5:3:2. The respective feed-stocks materials were collected locally, digested and analyzed in accordance with standard procedures. They were pre-fermented for a period of 10 days before being introduced into the digesters. They were digested for a retention period of 28 days, the physiochemical parameters namely; pressure, temperature, pH, volume of the gas collector system and volume of biogas produced were all closely monitored and recorded daily. The values of pH and temperature ranged 6.0 - 8.0, and 220C- 350C respectively. For the single substrate, bio-digester A(Cow dung only) produced biogas of total volume 0.1607m3(average volume of 0.0054m3 daily),while B (Chicken droppings ) produced 0.1722m3 (average of 0.0057m3 daily) and C (lemon grass) produced 0.1035m3 (average of 0.0035m3 daily). For the co-digested substrates in bio-digester D the total biogas produced was 0.2007m³ (average volume of 0.0067m³ daily) and bio-digester E produced 0.1991m³ (average volume of 0.0066m³ daily) It’s obvious from the results, that combining different substrates gave higher yields than when a singular feed stock was used and also mixing ratio played some roles in the yield improvement. Bio-digesters D and E contained the same substrates but mixed with different ratios, but higher yield was noticed in D with mixing ratio of 7:1:2 than in E with ratio 5:3:2.Therefore, co-digestion of substrates and mixing proportions are important factors for biogas production optimization.

Keywords: anaerobic, batch, biogas, biodigester, digestion, fermentation, optimization

Procedia PDF Downloads 30

Authors: Wei Wang, Yuan Hu

Abstract:

Epoxy resins (EP), one of the most important thermosetting polymers, is widely applied in various fields due to its desirable properties, such as excellent electrical insulation, low shrinkage, outstanding mechanical stiffness, satisfactory adhesion and solvent resistance. However, like most of the polymeric materials, EP has the fatal drawbacks including inherent flammability and high yield of toxic smoke, which restricts its application in the fields requiring fire safety. So, it is still a challenge and an interesting subject to develop new flame retardants which can not only remarkably improve the flame retardancy, but also render modified resins low toxic gases generation. In recent work, polymer nanocomposites based on nanohybrids that contain two or more kinds of nanofillers have drawn intensive interest, which can realize performance enhancements. The realization of previous hybrids of carbon nanotubes (CNTs) and molybdenum disulfide provides us a novel route to decorate layered double hydroxide (LDH) nanosheets on the surface of β-FeOOH nanorods; the deposited LDH nanosheets can fill the network and promote the work efficiency of β-FeOOH nanorods. Moreover, the synergistic effects between LDH and β-FeOOH can be anticipated to have potential applications in reducing fire hazards of EP composites for the combination of condense-phase and gas-phase mechanism. As reported, β-FeOOH nanorods can act as a core to prepare hybrid nanostructures combining with other nanoparticles through electrostatic attraction through layer-by-layer assembly technique. In this work, LDH nanosheets wrapped β-FeOOH nanorods (LDH-β-FeOOH) hybrids was synthesized by a facile method, with the purpose of combining the characteristics of one dimension (1D) and two dimension (2D), to improve the fire resistance of epoxy resin. The hybrids showed a well dispersion in EP matrix and had no obvious aggregation. Thermogravimetric analysis and cone calorimeter tests confirmed that LDH-β-FeOOH hybrids into EP matrix with a loading of 3% could obviously improve the fire safety of EP composites. The plausible flame retardancy mechanism was explored by thermogravimetric infrared (TG-IR) and X-ray photoelectron spectroscopy. The reasons were concluded: condense-phase and gas-phase. Nanofillers were transferred to the surface of matrix during combustion, which could not only shield EP matrix from external radiation and heat feedback from the fire zone, but also efficiently retard transport of oxygen and flammable pyrolysis.

Keywords: fire hazards, toxic gases, self-assembly, epoxy

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Authors: Claudio Lamilla, Misael Riquelme, Victoria Saez, Fernanda Sepulveda, Monica Pavez, Leticia Barrientos

Abstract:

Biosurfactants are compounds synthesized by microorganisms that show various chemical structures, including glycolipids, lipopeptides, polysaccharide-protein complex, phospholipids, and fatty acids. These molecules have attracted attention in recent years due to the amphipathic nature of these compounds, which allows their application in various activities related to emulsification, foaming, detergency, wetting, dispersion and solubilization of hydrophobic compounds. Microorganisms that produce biosurfactants are ubiquitous, not only present in water, soil, and sediments but in extreme conditions of pH, salinity or temperature such as those present in Antarctic ecosystems. Due to this, it is of interest to study biosurfactants producing bacterial strains isolated from Antarctic environments, with the potential to be used in various biotechnological processes. The objective of this research was to characterize biosurfactants produced by bacterial strains isolated from Antarctic environments, with potential use in biotechnological processes for the cleaning of sites contaminated with hydrocarbons. The samples were collected from soils and sediments in the South Shetland Islands and the Antarctic Peninsula, during the Antarctic Research Expedition INACH 2016, from both pristine and human occupied areas (influenced). The bacteria isolation was performed from solid R2A, M1 and LB media. The selection of strains producing biosurfactants was done by hemolysis test on blood agar plates (5%) and blue agar (CTAB). From 280 isolates, it was determined that 10 bacterial strains produced biosurfactants after stimulation with different carbon sources. 16S rDNA taxonomic markers, using the universal primers 27F-1492R, were used to identify these bacterias. Biosurfactants production was carried out in 250 ml flasks using Bushnell Hass liquid culture medium enriched with different carbon sources (olive oil, glucose, glycerol, and hexadecane) during seven days under constant stirring at 20°C. Each cell-free supernatant was characterized by physicochemical parameters including drop collapse, emulsification and oil displacement, as well as stability at different temperatures, salinity, and pH. In addition, the surface tension of each supernatant was quantified using a tensiometer. The strains with the highest activity were selected, and the production of biosurfactants was stimulated in six liters of culture medium. Biosurfactants were extracted from the supernatants with chloroform methanol (2:1). These biosurfactants were tested against crude oil and motor oil, to evaluate their displacement activity (detergency). The characterization by physicochemical properties of 10 supernatants showed that 80% of them produced the drop collapse, 60% had stability at different temperatures, and 90% had detergency activity in motor and olive oil. The biosurfactants obtained from two bacterial strains showed a high activity of dispersion of crude oil and motor oil with halos superior to 10 cm. We can conclude that bacteria isolated from Antarctic soils and sediments provide biological material of high quality for the production of biosurfactants, with potential applications in the biotechnological industry, especially in hydrocarbons -contaminated areas such as petroleum.

Keywords: antarctic, bacteria, biosurfactants, hydrocarbons

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Authors: A. Julio, R. Caparica, S. Costa Lima, S. Reis, J. G. Costa, P. Fonte, T. Santos De Almeida

Abstract:

The Mycobacterium leprae causes a chronic and infectious disease called leprosy, which the most common symptoms are peripheral neuropathy and deformation of several parts of the body. The pharmacological treatment of leprosy is a combined therapy with three different drugs, rifampicin, clofazimine, and dapsone. However, clofazimine and dapsone have poor solubility in water and also low bioavailability. Thus, it is crucial to develop strategies to overcome such drawbacks. The use of ionic liquids (ILs) may be a strategy to overcome the low solubility since they have been used as solubility promoters. ILs are salts, liquid below 100 ºC or even at room temperature, that may be placed in water, oils or hydroalcoholic solutions. Another approach may be the encapsulation of drugs into polymeric nanoparticles, which improves their bioavailability. In this study, two different classes of ILs were used, the imidazole- and the choline-based ionic liquids, as solubility enhancers of the poorly soluble antileprotic drugs. Thus, after the solubility studies, it was developed IL-PLGA nanoparticles hybrid systems to deliver such drugs. First of all, the solubility studies of clofazimine and dapsone were performed in water and in water: IL mixtures, at ILs concentrations where cell viability is maintained, at room temperature for 72 hours. For both drugs, it was observed an improvement on the drug solubility and [Cho][Phe] showed to be the best solubility enhancer, especially for clofazimine, where it was observed a 10-fold improvement. Later, it was produced nanoparticles, with a polymeric matrix of poly(lactic-co-glycolic acid) (PLGA) 75:25, by a modified solvent-evaporation W/O/W double emulsion technique in the presence of [Cho][Phe]. Thus, the inner phase was an aqueous solution of 0.2 % (v/v) of the above IL with each drug to its maximum solubility determined on the previous study. After the production, the nanosystem hybrid was physicochemically characterized. The produced nanoparticles had a diameter of around 580 nm and 640 nm, for clofazimine and dapsone, respectively. Regarding the polydispersity index, it was in agreement of the recommended value of this parameter for drug delivery systems (around 0.3). The association efficiency (AE) of the developed hybrid nanosystems demonstrated promising AE values for both drugs, given their low solubility (64.0 ± 4.0 % for clofazimine and 58.6 ± 10.0 % for dapsone), that prospects the capacity of these delivery systems to enhance the bioavailability and loading of clofazimine and dapsone. Overall, the study achievement may signify an upgrading of the patient’s quality of life, since it may mean a change in the therapeutic scheme, not requiring doses of drug so high to obtain a therapeutic effect. The authors would like to thank Fundação para a Ciência e a Tecnologia, Portugal (FCT/MCTES (PIDDAC), UID/DTP/04567/2016-CBIOS/PRUID/BI2/2018).

Keywords: ionic liquids, ionic liquids-PLGA nanoparticles hybrid systems, leprosy treatment, solubility

Procedia PDF Downloads 152

Authors: Emmanuel Ikechuckwu Onwubuya, Afees Adebayo Oladejo

Abstract:

Background: The use of medicinal plants in the treatment of chronic diseases especially myocardial infarction, is gaining wide acceptance globally. Andrographis paniculata (Acanthaceae) is a medicinal plant commonly known as the king of bitters in Nigeria and has been acclaimed for several therapeutic activities. Materials and methods: This study investigated the cardio-protective effect of the leaf extract of A. paniculata in isoproterenol-induced myocardial infarction. Fresh green leaves of A paniculata were harvested from the Faculty of Agriculture farmland, Nnamdi Azikiwe University, Awka, Nigeria. Identification and authentication of the plant were carried out at the Department of Botany, Nnamdi Azikiwe University and a voucher specimen was deposited at the herbarium. The plant material was then shredded, air-dried under shade and pulverized. The fine powders obtained were weighed and extraction was done via a solvent combination of water and ethanol (3:7) for 72 hr via maceration. The filtrate gotten was evaporated to dryness to obtain the ethanol extract, which was used for further bioassay study. The bioactive constituents of the plant extract were quantitatively analyzed by Gas chromatography-mass spectrometry (GC-MS). The animals were administered the extract of A. paniculata orally for seven days at a divided dose of 100 mg/kg, 200 mg/kg and 400 mg/kg body weights. On the eighth day, myocardial infarction was induced through subcutaneous administration of isoproterenol at a dose of 150 mg/kg/day diluted in 2 ml of saline on two consecutive days. Subsequently, the blood pressures were monitored and blood was collected for bioassay studies. Results: The results of the study showed that the leaf extract of A. paniculata was rich in Dodecanoic acid (8.261%), 4-Dibenzofuranamine (6.03%), Cyclotrisiloxane (4.679 %). The findings also showed a significant decrease (p>0.05) in the Mean arterial blood pressure, heart rate, aspartate transaminase, alanine transaminase, creatinine kinase and lactate dehydrogenase activities of the treatment group compared with the untreated control group while the antioxidant (superoxide dismutase, catalase and glutathione) activities were significantly increased in the treatment group, compared with the untreated control group. Conclusion: The findings of this work have shown that the leaf of A. paniculata was rich in bioactive compounds, which could be synthesized to produce plant-based products to fight cardiovascular diseases, especially myocardial infarction.

Keywords: cardiovascular disease, myocardial infarction, medicinal plant, andrographis paniculata, isoproterenol

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