Search results for: non aqueous solvent

Authors: Diwan Singh

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The ability of non-living Spirogyra sp. biomass for biosorption of copper(II) ions from aqueous solutions was explored. The effect of contact time, pH, initial copper ion concentration, biosorbent dosage and temperature were investigated in batch experiments. Both the Freundlich and Langmuir Isotherms were found applicable on the experimental data (R2>0.98). Qmax obtained from the Langmuir Isotherms was found to be 28.7 mg/g of biomass. The values of Gibbs free energy (ΔGº) and enthalpy change (ΔHº) suggest that the sorption is spontaneous and endothermic at 20ºC-40ºC.

Keywords: biosorption, Spirogyra sp., contact time, pH, dose

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Authors: F. Mutelet, L. Cesari

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Development of safer and environmentally friendly processes and products is needed to achieve sustainable production and consumption patterns. Ionic liquids, which are of great interest to the chemical and related industries because of their attractive properties as solvents, should be considered. Ionic liquids are comprised of an asymmetric, bulky organic cation and a weakly coordinating organic or inorganic anion. A large number of possible combinations allows for the ability to ‘fine tune’ the solvent properties for a specific purpose. Physical and chemical properties of ionic liquids are not only influenced by the nature of the cation and the nature of cation substituents but also by the polarity and the size of the anion. These features infer to ionic liquids numerous applications, in organic synthesis, separation processes, and electrochemistry. Separation processes required a good knowledge of the behavior of organic compounds with ionic liquids. Gas chromatography is a useful tool to estimate the interactions between organic compounds and ionic liquids. Indeed, retention data may be used to determine infinite dilution thermodynamic properties of volatile organic compounds in ionic liquids. Among others, the activity coefficient at infinite dilution is a direct measure of solute-ionic liquid interaction. In this work, infinite dilution thermodynamic properties of volatile organic compounds in specific bis(trifluoromethylsulfonyl)imide based ionic liquids measured by gas chromatography is presented. It was found that apolar compounds are not miscible in this family of ionic liquids. As expected, the solubility of organic compounds is related to their polarity and hydrogen-bond. Through activity coefficients data, the performance of these ionic liquids was evaluated for different separation processes (benzene/heptane, thiophene/heptane and pyridine/heptane). Results indicate that ionic liquids may be used for the extraction of polar compounds (aromatics, alcohols, pyridine, thiophene, tetrahydrofuran) from aliphatic media. For example, 1-benzylpyridinium bis(trifluoromethylsulfonyl) imide and 1-cyclohexylmethyl-1-methylpyrrolidinium bis(trifluoromethylsulfonyl)imide are more efficient for the extraction of aromatics or pyridine from aliphatics than classical solvents. Ionic liquids with long alkyl chain length present important capacity values but their selectivity values are low. In conclusion, we have demonstrated that specific bis(trifluoromethylsulfonyl)imide based ILs containing polar chain grafted on the cation (for example benzyl or cyclohexyl) increases considerably their performance in separation processes.

Keywords: interaction organic solvent-ionic liquid, gas chromatography, solvation model, COSMO-RS

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Authors: Gabriela Rivadeneyra-Romero, Claudia del C. Gutierrez Torres, Sergio A. Martinez-Delgadillo, Victor X. Mendoza-Escamilla, Alejandro Alonzo-Garcia

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Ultrasonic degradation is currently being used in sonochemical reactors to degrade pollutant compounds from aqueous media, as emerging contaminants (e.g. pharmaceuticals, drugs and personal care products.) because they can produce possible ecological impacts on the environment. For this reason, it is important to develop appropriate water and wastewater treatments able to reduce pollution and increase reuse. Pollutants such as textile dyes, aromatic and phenolic compounds, cholorobenzene, bisphenol-A and carboxylic acid and other organic pollutants, can be removed from wastewaters by sonochemical oxidation. The effect on the removal of pollutants depends on the type of the ultrasonic frequency used; however, not much studies have been done related to the behavior of the fluid into the sonoreactors operated at different ultrasonic frequencies. Based on the above, it is necessary to study the hydrodynamic behavior of the liquid generated by the ultrasonic irradiation to design efficient sonoreactors to reduce treatment times and costs. In this work, it was studied the hydrodynamic behavior of the fluid in sonochemical reactors at different frequencies (250 kHz, 500 kHz and 1000 kHz). The performances of the sonoreactors at those frequencies were simulated using computational fluid dynamics (CFD). Due to there is great sound speed gradient between piezoelectric and fluid, k-e models were used. Piezoelectric was defined as a vibration surface, to evaluate the different frequencies effect on the fluid into sonochemical reactor. Structured hexahedral cells were used to mesh the computational liquid domain, and fine triangular cells were used to mesh the piezoelectric transducers. Unsteady state conditions were used in the solver. Estimation of the dissipation rate, flow field velocities, Reynolds stress and turbulent quantities were evaluated by CFD and 2D-PIV measurements. Test results show that there is no necessary correlation between an increase of the ultrasonic frequency and the pollutant degradation, moreover, the reactor geometry and power density are important factors that should be considered in the sonochemical reactor design.

Keywords: CFD, reactor, ultrasound, wastewater

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Authors: A. W. Fareezal, R. Rosazley, M. A. Izzati, M. Z. Shazana, I. Rushdan

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Kenaf cellulose CNT paper production was for lightweight, high strength and excellent flexibility electrical purposes. Aqueous dispersions of kenaf cellulose and varied weight percentage of CNT were combined with the assistance of PEI solution by using ultrasonic probe. The solution was dried using vacuum filter continued with air drying in condition room for 2 days. Circle shape conductive paper was characterized with Fourier transformed infrared (FTIR) spectra, scanning electron microscopy (SEM) and therma gravimetric analysis (TGA).

Keywords: cellulose, CNT paper, PEI solution, electrical conductive paper

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Authors: Neveen AlQasas, Daniel Johnson

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Membranes for water treatment are an established technology that attracts great attention due to its simplicity and cost effectiveness. However, membranes in operation suffer from the adverse effect of membrane fouling. Bio-fouling is a phenomenon that occurs at the water-membrane interface, and is a dynamic process that is initiated by the adsorption of dissolved organic material, including biomacromolecules, on the membrane surface. After initiation, attachment of microorganisms occurs, followed by biofilm growth. The biofilm blocks the pores of the membrane and consequently results in reducing the water flux. Moreover, the presence of a fouling layer can have a substantial impact on the membrane separation properties. Understanding the mechanism of the initiation phase of biofouling is a key point in eliminating the biofouling on membrane surfaces. The adhesion and attachment of different fouling materials is affected by the surface properties of the membrane materials. Therefore, surface properties of different polymeric materials had been studied in terms of their surface energies and Hansen solubility parameters (HSP). The difference between the combined HSP parameters (HSP distance) allows prediction of the affinity of two materials to each other. The possibilities of measuring the HSP of different polymer films via surface measurements, such as contact angle has been thoroughly investigated. Knowing the HSP of a membrane material and the HSP of a specific foulant, facilitate the estimation of the HSP distance between the two, and therefore the strength of attachment to the surface. Contact angle measurements using fourteen different solvents on five different polymeric films were carried out using the sessile drop method. Solvents were ranked as good or bad solvents using different ranking method and ranking was used to calculate the HSP of each polymeric film. Results clearly indicate the absence of a direct relation between contact angle values of each film and the HSP distance between each polymer film and the solvents used. Therefore, estimating HSP via contact angle alone is not sufficient. However, it was found if the surface tensions and viscosities of the used solvents are taken in to the account in the analysis of the contact angle values, a prediction of the HSP from contact angle measurements is possible. This was carried out via training of a neural network model. The trained neural network model has three inputs, contact angle value, surface tension and viscosity of solvent used. The model is able to predict the HSP distance between the used solvent and the tested polymer (material). The HSP distance prediction is further used to estimate the total and individual HSP parameters of each tested material. The results showed an accuracy of about 90% for all the five studied films

Keywords: surface characterization, hansen solubility parameter estimation, contact angle measurements, artificial neural network model, surface measurements

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Authors: Vadim V. Zefirov, Victor E. Sizov, Marina A. Pigaleva, Igor V. Elmanovich, Mikhail S. Kondratenko, Marat O. Gallyamov

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This work presents a novel method for treating porous hydrophobic polyolefin membranes using supercritical carbon dioxide that allows usage of the modified membrane in redox flow batteries with an aqueous electrolyte. Polyolefin membranes are well known and widely used, however, they cannot be used as separators in redox flow batteries with an aqueous electrolyte since they have insufficient wettability, and therefore do not provide sufficient proton conductivity. The main aim of the presented work was the development of hydrophilic composites based on cheap membranes and precursors. Supercritical fluid was used as a medium for the deposition of the hydrophilic phase on the hydrophobic surface of the membrane. Due to the absence of negative capillary effects in a supercritical medium, a homogeneous composite is obtained as a result of synthesis. The in-situ synthesized silicon oxide nanoparticles and the chitosan polymer layer act as the hydrophilic phase and not only increase the affinity of the membrane towards the electrolyte, but also reduce the pore size of the polymer matrix, which positively affects the ion selectivity of the membrane. The composite material obtained as a result of synthesis has enhanced hydrophilic properties and is capable of providing proton conductivity in redox flow batteries. The morphology of the obtained composites was characterized by electron microscopy. To analyze the phase composition, infrared spectroscopy was used. The hydrophilic properties were studied by water contact angle measurements. In addition, the proton conductivity and ion selectivity of the obtained samples were studied, and tests in real redox flow batteries were performed. As a result, modified membrane was characterised in detail and moreover it was shown that modified cheap polyolefin membranes have pronounced proton conductivity and high ion selectivity, so their performance in a real redox flow battery approaches expensive commercial analogues, reaching 70% of energy efficiency.

Keywords: carbon dioxide, chitosan, polymer membrane, redox flow batteries, silica nanoparticles, supercritical fluid

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Authors: Mahmoud H. Aboul-Ela, Riham R. Mohamed, Magdy W. Sabaa

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Synthesis of cross-linked hydrogels composed of trimethyl chitosan (TMC) and poly(vinyl alcohol) (PVA) in different weight ratios in presence of glutaraldehyde as cross-linking agent. Characterization of the prepared hydrogels was done using FTIR, XRD, SEM and TGA. The prepared hydrogels were investigated as adsorbent materials for some transition metal ions from their aqueous solutions. Moreover, the swell ability of the prepared hydrogels was also investigated in both acidic and alkaline pHs, as well as in simulated body fluid (SBF).

Keywords: trimethyl chitosan, hydrogels, metal uptake, superabsorbent materials

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Authors: Imen Salhi, Salah Bouhlel, Bernrd Lehmann

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The Kebbouch South Pb-Zn deposit is located 20 km to the east of El Kef (NW) in the southeastern part of the Triassic diapir belt in the Tunisian Atlas. The deposit is composed of sulfide and non-sulfide zinc-lead ore bodies. The aim of this study is to provide petrographic results, mineralogy, as well as fluid inclusion data of the carbonate-hosted Pb-Zn Kebbouch South deposit. Mineralization forms two major ore types: (1) lenticular dolostones and clay breccias in the contact zone between Triassic and Upper Cretaceous strata;, it consists of small-scale lenticular, strata-or fault-controlled mineralization mainly composed of marcasite, galena, sphalerite, pyrite, and (2) stratiform mineralization in the Bahloul Formation (Upper Cenomanian-Lower Turonian) consisting of framboidal and cubic pyrite, disseminated sphalerite and galena. Non-metalliferous and/or gangue minerals are represented by dolomite, calcite, celestite and quartz. Fluid inclusion petrography study has been carried out on calcite and celestite. Fluid inclusions hosted in celestite are less than 20 µm large and show two types of aqueous inclusions: monophase liquid aqueous inclusions (L), abundant and very small, generally less than 15 µm and liquid-rich two phase inclusions (L+V). The gas phase forms a mobile vapor bubble. Microthermometric analyses of (L+V) fluid inclusions for celestite indicate that the homogenization temperature ranges from 121 to 156°C, and final ice melting temperatures are in the range of – 19 to -9°C corresponding to salinities of 12 to 21 wt% NaCl eq. (L+V) fluid inclusions from calcite are frequently localized along the growth zones; their homogenization temperature ranges from 96 to 164°C with final ice melting temperatures between -16 and -7°C corresponding to salinities of 9 to 19 wt% NaCl eq. According to mineralogical and fluid inclusion studies, mineralization in the Pb – Zn Kebbouch South deposit formed between 96 to 164°C with salinities ranging from 9 to 21 wt% NaCl eq. A contribution of basinal brines in the ore formation of the kebbouch South Pb–Zn deposit is likely. The deposit is part of the family of MVT deposits associated with the salt diapir environment.

Keywords: fluid inclusion, Kebbouch South, mineralogy, MVT deposits, Pb-Zn

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Authors: Lawrence Koech, Ray Everson, Hein Neomagus, Hilary Rutto

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Wet Flue gas desulphurization (FGD) systems are commonly used to remove sulphur dioxide from flue gas by contacting it with limestone in aqueous phase which is obtained by dissolution. Dissolution is important as it affects the overall performance of a wet FGD system. In the present study, effects of pH, stirring speed, solid to liquid ratio and acid concentration on the dissolution of limestone using an organic acid (adipic acid) were investigated. This was investigated using the pH stat apparatus. Calcium ions were analyzed at the end of each experiment using Atomic Absorption (AAS) machine.

Keywords: desulphurization, limestone, dissolution, pH stat apparatus

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Authors: Ahmed A. Abdel-Khalek, Reham A. Mohamed

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The kinetics of oxidation of binary complex [CrIII(DMG)2(H2O)4 ]+ to Cr(VI) by periodate has been investigated spectrophotometrically where, [DMG= Dimethylglyoxime] at 370nm under pseudo first order reaction conditions in aqueous medium over 20- 40ºC range, PH 2-3, and I=0.07 mol dm-3. The reaction is first order with respect to both [IO4-] and Cr(III), and the reaction increased with PH increased. Thermodymanic activation parameters have been calculated. It is suggested that electron transfer proceeds through an inner sphere mechanism via coordination of IO4- to Cr (III). The reaction obeys the following rate law Rate= {k1 K5+ k2 K6 K2 } [Cr III (DMG)2(H2O)4 ]+ [H5IO6].

Keywords: chromium, dimethylglyoxime, kinetics, oxidation, periodate

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Authors: Abubakar Bello Usman, Alhassan Muhammad Gani, Kolo Ibrahim

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The use of botanical raw materials to produce pharmaceuticals, herbal remedies, teas, spirits, cosmetics, sweets, dietary supplements, special industrial compounds and crude materials constitute an important global resource in terms of healthcare and economy. In Nigeria and other developing countries, the indigenous knowledge on the uses of plants lies with the older generation and the traditional healers. However, these custodians are decreasing in number due to death and other unforeseen occurrences. An Ethno-botanical survey was carried out to obtain information on the ethno medical values of wide range of plants used by the people of Gombe State, North-Eastern Nigeria, in the practice of healing and cure of typhoid (enteric) fever. Oral interviews were conducted so as to consider those with low literacy level who are involved in the practice of traditional medicine and thirty four (34) informants availed themselves for the interview and were consulted. All relevant information obtained from the respondents was recorded. A recent and valid nomenclature, along with local names, family names, part of the plant(s) used, methods of preparation and administration and fifty four (54) plant species belonging to 27 families as well as 7 unidentified species that are commonly used by the people of the state in ethnomedical treatment of the ailment were tabulated. Those interviewed included traditional practitioners, local herb sellers, traditional rulers, hunters, farmers and patients. Specific questions were asked and information supplied by informants was promptly documented. Results showed that the people of Gombe State are knowledgeable on herbal medicine in the treatment of diseases and ailments. Furthermore, the aqueous leaf extracts of Senna siamea, the plant species with the highest PPK (percentage of people who have knowledge about the use of a species for treating typhoid fever) in this ethnobotanical survey, was tested for its activity against clinical isolates of Salmonella typhi using the agar well diffusion method. The aqueous extracts showed some activity (zones of inhibition 11, 9, 7.5, 3.5, 1.3 mm) at 2000, 1800, 1600, 1400, 1200 µg/ml concentrations respectively. Preliminary phytochemical studies of the aqueous leaf extracts of the plant revealed the presence of secondary metabolites such as alkaloids, saponins, tannins, flavonoids and cardiac glycosides. Though a large number of traditionally used plants for the treatment of enteric fever were identified, further scientific validation of the traditional claims of anti-typhoid properties is imperative. This would establish their candidature for any possible future research for active principles and the possible development of new cheaper and more effective anti-typhoid drugs, as well as in the conservation of this rich diversity of medicinal plants.

Keywords: antimicrobial activities, ethnobotany, gombe state, north-eastern Nigeria, phytochemical screening, senna siamea, typhoid fever

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Authors: G. Magalhães-Mota, C. Magro, S. Sério, E. Mateus, P. A. Ribeiro, A. B. Ribeiro, M. Raposo

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Triclosan [5-chloro-2-(2,4-dichlorophenoxy) phenol], belonging to the class of Pharmaceuticals and Personal Care Products (PPCPs), is a broad-spectrum antimicrobial agent and bactericide. Because of its antimicrobial efficacy, it is widely used in personal health and skin care products, such as soaps, detergents, hand cleansers, cosmetics, toothpastes, etc. However, it has been considered to disrupt the endocrine system, for instance, thyroid hormone homeostasis and possibly the reproductive system. Considering the widespread use of triclosan, it is expected that environmental and food safety problems regarding triclosan will increase dramatically. Triclosan has been found in river water samples in both North America and Europe and is likely widely distributed wherever triclosan-containing products are used. Although significant amounts are removed in sewage plants, considerable quantities remain in the sewage effluent, initiating widespread environmental contamination. Triclosan undergoes bioconversion to methyl-triclosan, which has been demonstrated to bio accumulate in fish. In addition, triclosan has been found in human urine samples from persons with no known industrial exposure and in significant amounts in samples of mother's milk, demonstrating its presence in humans. The action of sunlight in river water is known to turn triclosan into dioxin derivatives and raises the possibility of pharmacological dangers not envisioned when the compound was originally utilized. The aim of this work is to detect low concentrations of triclosan in an aqueous complex matrix through the use of a sensor array system, following the electronic tongue concept based on impedance spectroscopy. To achieve this goal, we selected the appropriate molecules to the sensor so that there is a high affinity for triclosan and whose sensitivity ensures the detection of concentrations of at least nano-molar. Thin films of organic molecules and oxides have been produced by the layer-by-layer (LbL) technique and sputtered onto glass solid supports already covered by gold interdigitated electrodes. By submerging the films in complex aqueous solutions with different concentrations of triclosan, resistance and capacitance values were obtained at different frequencies. The preliminary results showed that an array of interdigitated electrodes sensor coated or uncoated with different LbL and films, can be used to detect TCS traces in aqueous solutions in a wide range concentration, from 10⁻¹² to 10⁻⁶ M. The PCA method was applied to the measured data, in order to differentiate the solutions with different concentrations of TCS. Moreover, was also possible to trace a curve, the plot of the logarithm of resistance versus the logarithm of concentration, which allowed us to fit the plotted data points with a decreasing straight line with a slope of 0.022 ± 0.006 which corresponds to the best sensitivity of our sensor. To find the sensor resolution near of the smallest concentration (Cs) used, 1pM, the minimum measured value which can be measured with resolution is 0.006, so the ∆logC =0.006/0.022=0.273, and, therefore, C-Cs~0.9 pM. This leads to a sensor resolution of 0.9 pM for the smallest concentration used, 1pM. This attained detection limit is lower than the values obtained in the literature.

Keywords: triclosan, layer-by-layer, impedance spectroscopy, electronic tongue

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Authors: Samir Karimov, Elshad Abdullayev, Muslum Gurbanov

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As one of the γ-radiolysis products of hexachlorocyclohexane and hexachlorobenzene, the study of 1.4 g/L concentrated 1,2,4-trichlorobenzene (TCB) in methanol solution has been irradiated at 0-209.3 kGy dose of γ-radiation and the results have been studied via GC-MS. At maximum radiation dose of 209.3 kGy 91.38% of TCB has converted into different organic compounds, such as 1,4-, 1,3- and 1,2- dichlorobenzenes (DCB), chlorobenzene, toluene, benzene and other chlorinated and non-chlorinated compounds. The variation of compounds formed by γ-radiolysis depends on the nature of solvent and radiation dose. One of the frequently identified radiolysis products of TCB in different organic solvents - 1,4-DCB studied quantitatively with external standard. The concentration of DCB increases by increasing absorbed radiation dose to approximately 131.8 kGy, then at higher doses with its conversion into chlorobenzene, it decreases.

Keywords: γ-radiolysis, chlorinated pesticides, radiation dose, dechlorination

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Authors: Hang Zhou, Limin Zhu

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This paper investigates the fabrication of microstructures on Si surfaces by using electrochemical anodic oxidation with agarose stamps. The fabricating process is based on a selective anodic oxidation reaction that occurs in the contact area between a stamp and a Si substrate. The stamp which is soaked in electrolyte previously acts as a current flow channel. After forming the oxide patterns as an etching mask, a KOH aqueous is used for the wet etching of Si. A complicated microstructure array of 1 cm2 was fabricated by the method with high accuracy.

Keywords: microstructures, anodic oxidation, silicon, agarose stamps

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Authors: Askar Sabet, Abdolrasoul Fakhraee, Motahahre Ramezanpour, Noorallah Alipour

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An efficient and green method for oxidation of thiols to the corresponding disulfides is reported using ionic liquid [HSO3N(C2H4OSO3H)3] in the presence of free nano-Fe2O3 at 60°C. Ionic liquid is selective oxidant for S-S Coupling variety aliphatic and aromatic of thiols to corresponding disulfide in the presence of free nano-Fe2O3 as recoverable catalyst. Reaction has been performed in methanol as an inexpensive solvent. This reaction is clean and easy work-up with no side reaction.

Keywords: thiol, disulfide, ionic liquid, free nano-Fe2O3, oxidation, coupling

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Authors: Deepak Kakde, Steve Howdle, Derek Irvine, Cameron Alexander

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The poor aqueous solubility is one of the major obstacles in the formulation development of many drugs. Around 70% of drugs are poorly soluble in aqueous media. In the last few decades, micelles have emerged as one of the major tools for solubilization of hydrophobic drugs. Micelles are nanosized structures (10-100nm) obtained by self-assembly of amphiphilic molecules into the water. The hydrophobic part of the micelle forms core which is surrounded by a hydrophilic outer shell called corona. These core-shell structures have been used as a drug delivery vehicle for many years. Although, the utility of micelles have been reduced due to the lack of sustainable materials. In the present study, a novel methoxy poly(ethylene glycol)-b-poly(ε-decalactone) (mPEG-b-PεDL) copolymer was synthesized by ring opening polymerization (ROP) of renewable ε-decalactone (ε-DL) monomers on methoxy poly(ethylene glycol) (mPEG) initiator using 1,5,7-triazabicyclo[4.4.0]dec-5-ene (TBD) as a organocatalyst. All the reactions were conducted in bulk to avoid the use of toxic organic solvents. The copolymer was characterized by nuclear magnetic resonance spectroscopy (NMR), gel permeation chromatography (GPC) and differential scanning calorimetry (DSC).The mPEG-b-PεDL block copolymeric micelles containing indomethacin (IND) were prepared by nanoprecipitation method and evaluated as drug delivery vehicle. The size of the micelles was less than 40nm with narrow polydispersity pattern. TEM image showed uniform distribution of spherical micelles defined by clear surface boundary. The indomethacin loading was 7.4% for copolymer with molecular weight of 13000 and drug/polymer weight ratio of 4/50. The higher drug/polymer ratio decreased the drug loading. The drug release study in PBS (pH7.4) showed a sustained release of drug over a period of 24hr. In conclusion, we have developed a new sustainable polymeric material for IND delivery by combining the green synthetic approach with the use of renewable monomer for sustainable development of polymeric nanomedicine.

Keywords: dopolymer, ε-decalactone, indomethacin, micelles

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Authors: Marta Paszkiewicz, Justyna Łuczak, Martyna Marchelek, Adriana Zaleska-Medynska

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In recent years, photocatalytical processes have been intensively investigated for destruction of pollutants, hydrogen evolution, disinfection of water, air and surfaces, for the construction of self-cleaning materials (tiles, glass, fibres, etc.). Titanium dioxide (TiO2) is the most popular material used in heterogeneous photocatalysis due to its excellent properties, such as high stability, chemical inertness, non-toxicity and low cost. It is well known that morphology and microstructure of TiO2 significantly influence the photocatalytic activity. This characteristics as well as other physical and structural properties of photocatalysts, i.e., specific surface area or density of crystalline defects, could be controlled by preparation route. In this regard, TiO2 particles can be obtained by sol-gel, hydrothermal, sonochemical methods, chemical vapour deposition and alternatively, by ionothermal synthesis using ionic liquids (ILs). In the TiO2 particles synthesis ILs may play a role of a solvent, soft template, reagent, agent promoting reduction of the precursor or particles stabilizer during synthesis of inorganic materials. In this work, the effect of the ILs anion type on morphology and photoactivity of TiO2 is presented. The preparation of TiO2 microparticles with spherical structure was successfully achieved by solvothermal method, using tetra-tert-butyl orthotitatane (TBOT) as the precursor. The reaction process was assisted by an ionic liquids 1-butyl-3-methylimidazolium bromide [BMIM][Br], 1-butyl-3-methylimidazolium tetrafluoroborate [BMIM][BF4] and 1-butyl-3-methylimidazolium haxafluorophosphate [BMIM][PF6]. Various molar ratios of all ILs to TBOT (IL:TBOT) were chosen. For comparison, reference TiO2 was prepared using the same method without IL addition. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Brenauer-Emmett-Teller surface area (BET), NCHS analysis, and FTIR spectroscopy were used to characterize the surface properties of the samples. The photocatalytic activity was investigated by means of phenol photodegradation in the aqueous phase as a model pollutant, as well as formation of hydroxyl radicals based on detection of fluorescent product of coumarine hydroxylation. The analysis results showed that the TiO2 microspheres had spherical structure with the diameters ranging from 1 to 6 µm. The TEM micrographs gave a bright observation of the samples in which the particles were comprised of inter-aggregated crystals. It could be also observed that the IL-assisted TiO2 microspheres are not hollow, which provides additional information about possible formation mechanism. Application of the ILs results in rise of the photocatalytic activity as well as BET surface area of TiO2 as compared to pure TiO2. The results of the formation of 7-hydroxycoumarin indicated that the increased amount of ·OH produced at the surface of excited TiO2 for samples TiO2_ILs well correlated with more efficient degradation of phenol. NCHS analysis showed that ionic liquids remained on the TiO2 surface confirming structure directing role of that compounds.

Keywords: heterogeneous photocatalysis, IL-assisted synthesis, ionic liquids, TiO2

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Authors: Shagufta Tabassum, V. P. Pawar, jr., G. N. Shinde

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The study of dielectric relaxation properties of polar liquids in the binary mixture has been carried out at 10, 15, 20 and 25 ºC temperatures for 11 different concentrations using time domain reflectometry technique. The dielectric properties of a solute-solvent mixture of polar liquids in the frequency range of 10 MHz to 30 GHz gives the information regarding formation of monomers and multimers and also an interaction between the molecules of the liquid mixture under study. The dielectric parameters have been obtained by the least squares fit method using the Debye equation characterized by a single relaxation time without relaxation time distribution.

Keywords: excess properties, relaxation time, static dielectric constant, and time domain reflectometry technique

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Authors: Julia R. Beulig, Stefan Ohla, Detlev Belder

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In contrast to off-line analytical methods, lab-on-a-chip technology delivers direct information about the observed reaction. Therefore, microfluidic devices make an important scientific contribution, e.g. in the field of synthetic chemistry. Herein, the rapid generation of analytical data can be applied for the optimization of chemical reactions. These microfluidic devices enable a fast change of reaction conditions as well as a resource saving method of operation. In the presented work, we focus on the investigation of multiphase regimes, more specifically on a biphasic microfluidic droplet systems. Here, every single droplet is a reaction container with customized conditions. The biggest challenge is the rapid qualitative and quantitative readout of information as most detection techniques for droplet systems are non-specific, time-consuming or too slow. An exception is the electrospray mass spectrometry (ESI-MS). The combination of a reaction screening platform with a rapid and specific detection method is an important step in droplet-based microfluidics. In this work, we present a novel approach for synthesis optimization on the nanoliter scale with direct ESI-MS detection. The development of a droplet-based microfluidic device, which enables the modification of different parameters while simultaneously monitoring the effect on the reaction within a single run, is shown. By common soft- and photolithographic techniques a polydimethylsiloxane (PDMS) microfluidic chip with different functionalities is developed. As an interface for the MS detection, we use a steel capillary for ESI and improve the spray stability with a Teflon siphon tubing, which is inserted underneath the steel capillary. By optimizing the flow rates, it is possible to screen parameters of various reactions, this is exemplarity shown by a Domino Knoevenagel Hetero-Diels-Alder reaction. Different starting materials, catalyst concentrations and solvent compositions are investigated. Due to the high repetition rate of the droplet production, each set of reaction condition is examined hundreds of times. As a result, of the investigation, we receive possible reagents, the ideal water-methanol ratio of the solvent and the most effective catalyst concentration. The developed system can help to determine important information about the optimal parameters of a reaction within a short time. With this novel tool, we make an important step on the field of combining droplet-based microfluidics with organic reaction screening.

Keywords: droplet, mass spectrometry, microfluidics, organic reaction, screening

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Authors: Ebere Christian Ugochukwu, Okafor Josephine, Oyawoye Tomisin

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The occurrence of multidrug resistance patterns that have been developed by bacteria has made it difficult to properly treat infections using standard clinical medications. Hence, the use of herbs as an alternative source of therapy is considered cheap and easily accessible to locals. This research explored the antimicrobial effects of aqueous and ethanolic extracts obtained from Chrysophyllum albidum (commonly called ‘Agbalumo’ in southwest Nigeria and ‘Udara’ in the eastern and southern parts of Nigeria) plant parts (leaves, roots and seeds) against bacteria isolated from urinary catheter tips. The following isolates were obtained; Pseudomonas aeruginosa, Staphylococcus aureus, Escherichia coli, Proteus mirabilis, and Klebsiella aerogenes. The agar well diffusion method was used. The average percentages of antimicrobial resistance of the isolates to gentamycin were 45.5% for P. aeruginosa, 42.1% for E. coli, 46.9% for K. aerogenes, and ˃90% for other isolates. Qualitative phytochemical screening of the plant parts extracts was done using chemical test for the screening and identification of bioactive chemical constituents. The ethanolic extract mixtures (leaf, root and seed) had the greatest effect on all the isolates, with inhibition zones (IZs) ranging from 8-26 mm and MICs ranging from <16-32 mg/ml. The Potencies of the C. albidum extracts based on the IZ and MIC values were greater in the extract mixtures, followed by those in the roots. Phytochemical screening revealed that all the extracts contained phenol except for the seeds while tannins were present in all the extracts except the leaves. The activity of the ethanolic extracts of each part at high and low concentrations was greater than that of the aqueous extracts at the same concentrations (p<0.05). The acute toxicity results showed that the LD50 of the extracts was ˃5000 mg/body weight, indicating no toxicity. The antibacterial activities of the extract mixtures and roots on the isolates confirmed the use of C. albidum in folk medicine for the treatment of CAUTIs, hence indicating its antibacterial potential for use in novel antibiotic production.

Keywords: antimicrobials, susceptibility, minimum inhibitory concentration, extracts

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Authors: A. Heshmati, M. Y Alikhani, M. T. Godarzi, M. R. Sadeghimanesh

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Herbal essential oil and extracts are a good source of natural antioxidants and antimicrobial compounds. Hypericum is one of the potential sources of these compounds. In this study, the antioxidant and antimicrobial activity of essential oil and aqueous, methanol, ethanol, ethyl acetate and acetone extract of Hypericum scabrum was assessed. Flowers of Hypericum scabrum were collected from the surrounding mountains of Hamadan province and after drying in the shade, the essential oil of the plant was extracted by Clevenger and water, methanol, ethanol, ethyl acetate and acetone extract was obtained by maceration method. Essential oil compounds were identified using the GC-Mass. The Folin-Ciocalteau and aluminum chloride (AlCl₃) colorimetric method was used to measure the amount of phenolic acid and flavonoids, respectively. Antioxidant activity was evaluated using DPPH and FRAP. The minimum inhibitory concentration (MIC) and the minimum bacterial/fungicide concentration (MBC/MFC) of essential oil and extracts were evaluated against Staphylococcus aureus, Bacillus cereus, Pseudomonas aeruginosa, Salmonella typhimurium, Aspergillus flavus and Candida albicans. The essential oil yield of was 0.35%, the lowest and highest extract yield was related to ethyl acetate and water extract. The most component of essential oil was α-Pinene (46.35%). The methanol extracts had the highest phenolic acid (95.65 ± 4.72 µg galic acid equivalent/g dry plant) and flavonoids (25.39 ± 2.73 µg quercetin equivalent/g dry plant). The percentage of DPPH radical inhibition showed positive correlation with concentrations of essential oil or extract. The methanol and ethanol extract had the highest DDPH radical inhibitory. Essential oil and extracts of Hypericum had antimicrobial activity against the microorganisms studied in this research. The MIC and MBC values for essential oils were in the range of 25-25.6 and 25-50 μg/mL, respectively. For the extracts, these values were 1.5625-100 and 3.125-100 μg/mL, respectively. Methanol extracts had the highest antimicrobial activity. Essential oil and extract of Hypericum scabrum, especially methanol extract, have proper antimicrobial and antioxidant activity, and it can be used to control the oxidation and inhibit the growth of pathogenic and spoilage microorganisms. In addition, it can be used as a substitute for synthetic antioxidant and antimicrobial compounds.

Keywords: antimicrobial, antioxidant, extract, hypericum

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Authors: Grzegorz Swiderski, Agata Jablonska-Trypuc, Natalia Popow, Renata Swislocka, Wlodzimierz Lewandowski

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Doxorubicin belongs to the group of anthracycline antitumor antibiotics. Because of the wide spectrum of actions, it is one of the most widely used anthracycline antibiotics, including the treatment of breast, ovary, bladder, lung cancers as well as neuroblastoma, lymphoma, leukemia and myeloid leukemia. Antitumor activity of doxorubicin is based on the same mechanisms as for most anthracyclines. Like the metal ions affect the nucleic acids on many biological processes, so the environment of the metal chelates of antibiotics can have a significant effect on the pharmacological properties of drugs. Complexation of anthracyclines with metal ions may contribute to the production of less toxic compounds. In the framework of this study, the composition of complexes obtained in aqueous solutions of doxorubicin with metal ions (Cu2+ and Zn2+). Complexation was analyzed by spectrophotometric titration in aqueous solution at pH 7.0. The pH was adjusted with 0.02M Tris-HCl buffer. The composition of the complexes found was Cu: doxorubicin (1: 2) and a Zn: doxorubicin (1: 1). The effect of Dox, Dox-Cu and Dox-Zn was examined in MCF-7 breast cancer cell line, which were obtained from American Type Culture Collection (ATCC). The compounds were added to the cultured cells for a final concentration in the range of 0,01µM to 0,5µM. The number of MCF-7 cells with division into living and dead, was determined by direct counts of cells with the use of trypan blue dye using LUNA Logos Biosystems cell counter. ApoTox-Glo Triplex Assay (Promega, Madison, Wisconsin, USA) was used according to the manufacturer’s instructions to measure the MCF-7 cells’ viability, cytotoxicity and apoptosis. We observed a decrease in cells proliferation in a dose-dependent manner. An increase in cytotoxicity and decrease in viability in the ApoTox Triplex assay was also showed for all tested compounds. Apoptosis, showed as caspase 3/7 activation, was observed only in Dox treatment. In Dox-Zn and Dox-Cu caspase 3/7 activation was not observed. This work was financially supported by National Science Centre, Poland, under the research project number 2014/13/B/NZ7/02 352.

Keywords: anticancer properties, anthracycline antibiotic, doxorubicine, metal complexes

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Authors: Mihaela Beregoi, Horia Iovu, Cristina Busuioc, Alexandru Evanghelidis, Elena Matei, Monica Enculescu, Ionut Enculescu

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Nanomaterials field is very attractive for all researchers who are attempting to develop new devices with the same or improved properties than the micro-sized ones, while reducing the reagents and power consumptions. In this way, a wide range of nanomaterials were fabricated and integrated in applications for electronics, optoelectronics, solar cells, tissue reconstruction and drug delivery. Obviously, the most appealing ones are those dedicated to the medical domain. Different types of nano-sized materials, such as particles, fibers, films etc., can be synthesized by using physical, chemical or electrochemical methods. One of these techniques is electrospinning, which enable the production of fibers with nanometric dimensions by pumping a polymeric solution in a high electric field; due to the electrostatic charging and solvent evaporation, the precursor mixture is converted into nonwoven meshes with different fiber densities and mechanical properties. Moreover, polyaniline is a conducting polymer with interesting optical properties, suitable for displays and electrochromic windows. Otherwise, polyaniline is an electroactive polymer that can contract/expand by applying electric stimuli, due to the oxidation/reduction reactions which take place in the polymer chains. These two main properties can be exploited in order to synthesize smart materials that change their dimensions, exhibiting in the same time good electrochromic properties. In the context aforesaid, a poly(methyl metacrylate) solution was spun to get webs composed of fibers with diameter values between 500 nm and 1 µm. Further, the polymer meshes were covered with a gold layer in order to make them conductive and also appropriate as working electrode in an electrochemical cell. The gold shell was deposited by DC sputtering. Such metalized fibers can be transformed into smart materials by covering them with a thin layer of conductive polymer. Thus, the webs were coated with a polyaniline film by the electrochemical route, starting from and aqueous solution of aniline and sulfuric acid, where sulfuric acid acts as oxidant agent. For the polymerization of aniline, a saturated calomel electrode was employed as reference, a platinum plate as counter electrode and the gold covered webs as working electrode. Chronoamperometry was selected as deposition method for polyaniline, by modifying the deposition time. Metalized meshes with different fiber densities were used, the transmission ranging between 70 and 80 %. The morphological investigation showed that polyaniline layer has a granular structure for all deposition experiments. As well, some preliminary optical tests were done by using sulfuric acid as electrolyte, which revealed the modification of polyaniline colour from green to dark blue when applying a voltage. In conclusion, new multilayered materials were obtained by a simple approach: the merge of the electrospinning method benefits with polyaniline chemistry. This synthesis method allows the fabrication of structures with reproducible characteristics, suitable for display or tissue substituents.

Keywords: electrospinning, fibers, smart materials, polyaniline

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Authors: Jovana Nikolov, Natasa Todorovic, Ivana Stojkovic

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Monitoring of 222Rn in drinking or surface waters, as well as in groundwater has been performed in connection with geological, hydrogeological and hydrological surveys and health hazard studies. Liquid scintillation counting (LSC) is often preferred analytical method for 222Rn measurements in waters because it allows multiple-sample automatic analysis. LSC method implies mixing of water samples with organic scintillation cocktail, which triggers radon diffusion from the aqueous into organic phase for which it has a much greater affinity, eliminating possibility of radon emanation in that manner. Two direct LSC methods that assume different sample composition have been presented, optimized and evaluated in this study. One-phase method assumed direct mixing of 10 ml sample with 10 ml of emulsifying cocktail (Ultima Gold AB scintillation cocktail is used). Two-phase method involved usage of water-immiscible cocktails (in this study High Efficiency Mineral Oil Scintillator, Opti-Fluor O and Ultima Gold F are used). Calibration samples were prepared with aqueous 226Ra standard in glass 20 ml vials and counted on ultra-low background spectrometer Quantulus 1220TM equipped with PSA (Pulse Shape Analysis) circuit which discriminates alpha/beta spectra. Since calibration procedure is carried out with 226Ra standard, which has both alpha and beta progenies, it is clear that PSA discriminator has vital importance in order to provide reliable and precise spectra separation. Consequentially, calibration procedure was done through investigation of PSA discriminator level influence on 222Rn efficiency detection, using 226Ra calibration standard in wide range of activity concentrations. Evaluation of presented methods was based on obtained efficiency detections and achieved Minimal Detectable Activity (MDA). Comparison of presented methods, accuracy and precision as well as different scintillation cocktail’s performance was considered from results of measurements of 226Ra spiked water samples with known activity and environmental samples.

Keywords: 222Rn in water, Quantulus1220TM, scintillation cocktail, PSA parameter

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Authors: Kai-Sheng Ji, Yi-Feng Lin

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The pervaporation process for solvent and water separation has attracted research attention due to its lower energy consumption compared with conventional distillation processes. The membranes used for the pervaporation approach should exhibit high flux and separation factors. In this study, the ZIF-7 crystal particles were successfully incorporated into chitosan (CS) membranes to form ZIF-7/CS mixed-matrix membranes. The as-prepared ZIF-7/CS mixed-matrix membranes were used to separate mixtures of water/ethanol at 25℃ in the pervaporation process. The mixed-matrix membranes with different ZIF-7 wt% incorporation showed better separation efficiency than the pristine CS membranes because of the smaller pore size of the mixed-matrix membranes. The separation factor and the flux of the ZIF-7/CS membranes clearly exceed the upper limit of the previously reported CS-based and mixed-matrix membranes.

Keywords: pervaporation, chitosan, ZIF-7, memberane separation

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Authors: F. Garousi, S. Veres, É. Bódi, S. Várallyay, B. Kovács

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Extracting and determining chlorophyll pigments (chlorophyll a and b) in green leaves are the procedures based on the solvent extraction of pigments in samples using N,N-dimethylformamide as the extractant. In this study, two species of soluble inorganic selenium forms, selenite (Se( IV)) and selenate (Se( VI)) at different concentrations were investigated on maize plants that were growing in nutrient solutions during 2 weeks and at the end of the experiment, amounts of chlorophyll a and b for first and second leaves of maize were measured. In accordance with the results we observed that our regarded Se concentrations in both forms of Se( IV) and Se( VI) were not effective on maize plants’ chlorophyll a and b significantly although high level of 3 mg.kg-1 Se( IV) had negative affect on growth of the samples that had been treated by it but about Se( VI) samples we did not observe this state and our different considered Se( VI) concentrations were not toxic for maize plants.

Keywords: maize, sodium selenate, sodium selenite, chlorophyll a and b

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Authors: Yuvraj S. Malghe, Atul B. Lavand

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In recent years, semiconductor photocatalytic degradation processes have attracted a lot of attention and are used widely for the destruction of organic pollutants present in waste water. Among various semiconductors, titanium dioxide (TiO2) is the most popular photocatalyst due to its excellent chemical stability, non-toxicity, relatively low cost and high photo-oxidation power. It has been known that zinc oxide (ZnO) with band gap energy 3.2 eV is a suitable alternative to TiO2 due to its high quantum efficiency, however it corrodes in acidic medium. Unfortunately TiO2 and ZnO both are active only in UV light due to their wide band gaps. Sunlight consist about 5-7% UV light, 46% visible light and 47% infrared radiation. In order to utilize major portion of sunlight (visible spectrum), it is necessary to modify the band gap of TiO2 as well as ZnO. This can be done by several ways such as semiconductor coupling, doping the material with metals/non metals. Doping of TiO2 using transition metals like Fe, Co and non-metals such as N, C or S extends its absorption wavelengths from UV to visible region. In the present work, we have synthesized ZnO-TiO2 nanocomposite using reverse microemulsion method. Visible light photocatalytic activity of synthesized nanocomposite was investigated for degradation of aqueous solution of malachite green (MG). To increase the photocatalytic activity of ZnO-TiO2 nanocomposite, it is decorated with C and Fe. Pure, carbon (C) doped and carbon, iron(C, Fe) co-doped nanosized ZnO-TiO2 nanocomposites were synthesized using reverse microemulsion method. These composites were characterized using, X-ray diffraction (XRD), Energy dispersive X-ray spectroscopy (EDX), Scanning electron microscopy (SEM), UV visible spectrophotometery and X-ray photoelectron spectroscopy (XPS). Visible light photocatalytic activities of synthesized nanocomposites were investigated for degradation of aqueous malachite green (MG) solution. C, Fe co-doped ZnO-TiO2 nanocomposite exhibit better photocatalytic activity and showed threefold increase in photocatalytic activity. Effect of amount of catalyst, pH and concentration of MG solution on the photodegradation rate is studied. Stability and reusability of photocatalyst is also studied. C, Fe decorated ZnO-TiO2 nanocomposite shows threefold increase in photocatalytic activity.

Keywords: malachite green, nanocomposite, photocatalysis, titanium dioxide, zinc oxide

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Authors: Bartlomiej S. Witkowski, Lukasz Wachnicki, Sylwia Gieraltowska, Rafal Pietruszka, Marek Godlewski

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Zinc oxide is extensively studied II-VI semiconductor with a direct energy gap of about 3.37 eV at room temperature and high transparency in visible light spectral region. Due to these properties, ZnO is an attractive material for applications in photovoltaic, electronic and optoelectronic devices. ZnO nanorods, due to a well-developed surface, have potential of applications in sensor technology and photovoltaics. In this work we present a new inexpensive method of the ultra-fast growth of ZnO nanorods from the aqueous solution. This environment friendly and fully reproducible method allows growth of nanorods in few minutes time on various substrates, without any catalyst or complexing agent. Growth temperature does not exceed 50ºC and growth can be performed at atmospheric pressure. The method is characterized by simplicity and allows regulation of size of the ZnO nanorods in a large extent. Moreover the method is also very safe, it requires organic, non-toxic and low-price precursors. The growth can be performed on almost any type of substrate through the homo-nucleation as well as hetero-nucleation. Moreover, received nanorods are characterized by a very high quality - they are monocrystalline as confirmed by XRD and transmission electron microscopy. Importantly oxygen vacancies are not found in the photoluminescence measurements. First results for obtained by us ZnO nanorods in sensor applications are very promising. Resistance UV sensor, based on ZnO nanorods grown on a quartz substrates shows high sensitivity of 20 mW/m2 (2 μW/cm2) for point contacts, especially that the results are obtained for the nanorods array, not for a single nanorod. UV light (below 400 nm of wavelength) generates electron-hole pairs, which results in a removal from the surfaces of the water vapor and hydroxyl groups. This reduces the depletion layer in nanorods, and thus lowers the resistance of the structure. The so-obtained sensor works at room temperature and does not need the annealing to reset to initial state. Details of the technology and the first sensors results will be presented. The obtained ZnO nanorods are also applied in simple-architecture photovoltaic cells (efficiency over 12%) in conjunction with low-price Si substrates and high-sensitive photoresistors. Details informations about technology and applications will be presented.

Keywords: hydrothermal method, photoresistor, photovoltaic cells, ZnO nanorods

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Authors: Dalila Chouder, Djaafer Benachour

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This work concerns the study of the adsorption of metal ions Ag +, Mg +, and Ni2+ in aqueous medium by polydibenzoether-ROWN based on three factors: Temperature, time and concentration. The polydibenzoether crown was synthesized by two means: Chemical and electrochemical. The behavior of the two polymers has been different, and turns out very interesting for chemical polydibenzoether crown has identified conditions. Chemical and électronique polydibenzoether crown have different extraction screw vi property of adsoption of ions fifférents, this study also shows that plyméres doped may have an advantageous electrical conductivity.

Keywords: polymerization, electrochemical, conductivity, complexing metal ions

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Authors: Daseul Lee, Jeong Jun Lee, Ok-Sang Jung

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Self-assembly of a series of ZnX2 (X- = Cl-, Br-, and I-) with 2,3-bis(4’-nicotinamidephenoxy)naphthalene (L) as a new bidentate pyridyl-donor ligand yields systematic metallacyclodimeric unit, [ZnX2L]2. The supramolecule constitutes a characteristically stacked forming both 1D suprachannels and cages. Weak C-H⋯π and inter-digitated π⋯π interactions are main driving forces in the formation of both suprachannels and cages. The slightly different features between the suprachannel and cage have been investigated by 1H NMR and TG analysis, which solvent quantitatively exchange within only suprachannels. Photo-unstable CH2I2 molecules are stabilized via capturing within suprachannels, which is monitored by UV-Vis spectroscopy. Furthermore, the photoluminescence intensity, from the chromophore naphthyl moiety of [ZnCl2L]2, gradually decreases with the addition of CH2I2. And washing off the CH2I2 by dichloromethane returned the PL intensity back to its approximately original signal.

Keywords: metallacyclodimer, suprachannel, π⋯π interaction, molecular recognition

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