RESUMO
An antibacterial and conductive bionanocomposite (BNC) film consisting of polypyrrole (Ppy), zinc oxide (ZnO) nanoparticles (NPs), and chitosan (CS) was electrochemically synthesized on indium tin oxide (ITO) glass substrate by electrooxidation of 0.1 M pyrrole in aqueous solution containing appropriate amounts of ZnO NPs uniformly dispersed in CS. This method enables the room temperature electrosynthesis of BNC film consisting of ZnO NPs incorporated within the growing Ppy/CS composite. The morphology of Ppy/ZnO/CS BNC was characterized by scanning electron microscopy. ITO-Ppy/CS and ITO-Ppy/ZnO/CS bioelectrodes were characterized using the Fourier transform infrared technique, X-ray diffraction, and thermogravimetric analysis. The electrical conductivity of nanocomposites was investigated by a four-probe method. The prepared nanocomposites were analyzed for antioxidant activity using the 2,2-diphenyl-1-picrylhydrazyl assay. The results demonstrated that the antioxidant activity of nanocomposites increased remarkably by addition of ZnO NPs. The electrical conductivity of films showed a sudden decrease for lower weight ratios of ZnO NPs (5 wt%), while it was increased gradually for higher ratios (10, 15, and 20 wt%). The nanocomposites were analyzed for antibacterial activity against Gram-positive and Gram-negative bacteria. The results indicated that the synthesized BNC is effective against all of the studied bacteria, and its effectiveness is higher for Pseudomonas aeruginosa. The thermal stability and physical properties of BNC films were increased by an increase in the weight ratio of ZnO NPs, promising novel applications for the electrically conductive polysaccharide-based nanocomposites, particularly those that may exploit the antimicrobial nature of Ppy/ZnO/CS BNCs.
Assuntos
Materiais Biocompatíveis/química , Quitosana/química , Nanocompostos/química , Polímeros/química , Pirróis/química , Óxido de Zinco/química , Antibacterianos/química , Antibacterianos/farmacologia , Antioxidantes/química , Antioxidantes/farmacologia , Microscopia Eletrônica de Varredura , Nanopartículas/química , Pseudomonas aeruginosa/efeitos dos fármacos , Difração de Raios XRESUMO
Lipase-catalyzed production of triethanolamine-based esterquat by esterification of oleic acid (OA) with triethanolamine (TEA) in n-hexane was performed in 2 L stirred-tank reactor. A set of experiments was designed by central composite design to process modeling and statistically evaluate the findings. Five independent process variables, including enzyme amount, reaction time, reaction temperature, substrates molar ratio of OA to TEA, and agitation speed, were studied under the given conditions designed by Design Expert software. Experimental data were examined for normality test before data processing stage and skewness and kurtosis indices were determined. The mathematical model developed was found to be adequate and statistically accurate to predict the optimum conversion of product. Response surface methodology with central composite design gave the best performance in this study, and the methodology as a whole has been proven to be adequate for the design and optimization of the enzymatic process.
Assuntos
Reatores Biológicos , Etanolaminas/química , Lipase/metabolismo , Análise de Variância , Catálise , Esterificação , Ésteres , Etanolaminas/síntese química , Modelos Químicos , Ácido Oleico , Reprodutibilidade dos TestesRESUMO
Novel ionophores comprising various hydroxide and amine structures were immobilized onto poly(vinyl chloride) (PVC) matrices, and these were examined to determine Ti(III) selectivity. To predict the selectivity of Ti(III), a PVC membrane was used to investigate the binding of Ti(III) to c-methylcalix[4]resorcinarene (CMCR). The study showed that the chelating ligand, CMCR, was coordinated selectively to Ti(III) at eight coordination sites involving the oxygen atoms at the interface of the membrane/solution. The membrane was prepared, based on CMCR as an ionophore, sodium tetrakis(4-fluorophenyl) borate (NaTFPB) as a lipophilic ionic additive, and dioctylphthalate (DOP) as a plasticizer. The immobilization of the ionophore and surface characterization studies revealed that the performance of CMCR-immobilized PVC was equivalent to that of mobile ionophores in supported liquid membranes (SLMs). The strengths of the ion-ionophore (CMCR-Ti(OH)(OH(2))(5) (2+)) interactions and the role of ionophores on membranes were studied via UV-Vis, Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and and X-ray diffraction (XRD).
RESUMO
BACKGROUND: Due to the increasing industrial use of titanium compounds, its determination is the subject of considerable efforts. The ionophore or membrane active recognition is the most important component of any polymeric membrane sensor. The sensor's response depends on the ionophore and bonding between the ionophore and the target ion. Ionophores with molecule-sized dimensions containing cavities or semi-cavities can surround the target ion. The bond between the ionophore and target ion gives different selectivity and sensitivity toward the other ions. Therefore, ionophores with different binding strengths can be used in the sensor. RESULTS: In the present work, poly (vinyl chloride) (PVC) based membrane incorporating tris (2 pyridyl) methylamine (tpm) as an ionophore has been prepared and explored as a titanium(III) selective sensor. CONCLUSIONS: The strengths of the ion-ionophore (Ti(OH)2+-tpm) interactions and the role of ionophore on membrane were tested by various techniques such as elemental analysis, UV-vis, Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), and powder X-ray diffraction (XRD). All data approved the successful incorporation of organic group via covalent bond.
RESUMO
Fatty hydroxamic acids derivatives based on palm kernel oil which are phenyl fatty hydroxamic acids (PFHAs), methyl fatty hydroxamic acids (MFHAs), isopropyl fatty hydroxamic acids (IPFHAs) and benzyl fatty hydroxamic acids (BFHAs) were applied as chelating agent for copper liquid-liquid extraction. The extraction of copper from aqueous solution by MFHAs, PFHAs, BFHAs or IPFHAs were carried out in hexane as an organic phase through the formation of copper methyl fatty hydroxamate (Cu-MFHs), copper phenyl fatty hydroxamate (Cu-PFHs), copper benzyl fatty hydroxamate (Cu-BFHs) and copper isopropyl fatty hydroxamate (Cu-IPFHs). The results showed that the fatty hydroxamic acid derivatives could extract copper at pH 6.2 effectively with high percentage of extraction (the percentages of copper extraction by MFHAs, PFHAs, IPFHs and BFHAs were found to be 99.3, 87.5, 82.3 and 90.2%, respectively). The extracted copper could be quantitatively stripped back into sulphuric acid (3M) aqueous solution. The obtained results showed that the copper recovery percentages from Cu-MFHs, Cu-PFHs, Cu-BFHs and Cu-IPFHs are 99.1, 99.4, 99.6 and 99.9 respectively. The copper extraction was not affected by the presence of a large amount of Mg (II), Ni (II), Al (III), Mn (II) and Co (II) ions in the aqueous solution.
Assuntos
Cobre/química , Ácidos Graxos/química , Ácidos Hidroxâmicos/química , Óleos de Plantas/química , Cobre/isolamento & purificação , Ácidos Graxos/síntese química , Ácidos Hidroxâmicos/síntese química , Óleo de PalmeiraRESUMO
Liquid-liquid iron(III) extraction was investigated using benzyl fatty hydroxamic acids (BFHAs) and methyl fatty hydroxamic acids (MFHAs) as chelating agents through the formation of iron(III) methyl fatty hydroxamate (Fe-MFHs) or iron(III) benzyl fatty hydroxamate (Fe-BFHs) in the organic phase. The results obtained under optimized conditions, showed that the chelating agents in hexane extract iron(III) at pH 1.9 were realized effectively with a high percentage of extraction (97.2% and 98.1% for MFHAs and BFHAs, respectively). The presence of a large amount of Mg(II), Ni(II), Al(III), Mn(II) and Co(II) ions did affect the iron(III) extraction. Finally stripping studies for recovering iron(III) from organic phase (Fe-MFHs or Fe-BFHs dissolved in hexane) were carried out at various concentrations of HCl, HNO(3) and H(2)SO(4). The results showed that the desired acid for recovery of iron(III) was 5 M HCl and quantitative recovery of iron(III) was achieved from Fe(III)-MFHs and Fe(III)-BFHs solutions in hexane containing 5 mg/L of Fe(III).
Assuntos
Compostos de Benzil/química , Ácidos Hidroxâmicos/química , Quelantes de Ferro/química , Ferro/isolamento & purificação , Extração Líquido-Líquido/métodos , Óleos de Plantas/química , Alcanos/química , Clorofórmio/química , Compostos Férricos/química , Heptanos/química , Hexanos/química , Concentração de Íons de Hidrogênio , Íons , Óleo de Palmeira , Xilenos/químicaRESUMO
Nanocrystalline SnO(x) (x = 1-2) thin films were prepared on glass substrates by a simple chemical bath deposition method. Triethanolamine was used as complexing agent to decrease time and temperature of deposition and shift the pH of the solution to the noncorrosive region. The films were characterized for composition, surface morphology, structure and optical properties. X-ray diffraction analysis confirms that SnO(x) thin films consist of a polycrystalline structure with an average grain size of 36 nm. Atomic force microscopy studies show a uniform grain distribution without pinholes. The elemental composition was evaluated by energy dispersive X-ray spectroscopy. The average O/Sn atomic percentage ratio is 1.72. Band gap energy and optical transition were determined from optical absorbance data. The film was found to exhibit direct and indirect transitions in the visible spectrum with band gap values of about 3.9 and 3.7 eV, respectively. The optical transmittance in the visible region is 82%. The SnO(x) nanocrystals exhibit an ultraviolet emission band centered at 392 nm in the vicinity of the band edge, which is attributed to the well-known exciton transition in SnO(x). Photosensitivity was detected in the positive region under illumination with white light.
Assuntos
Nanopartículas/química , Nanotecnologia/métodos , Temperatura , Compostos de Estanho/síntese química , Absorção , Análise Diferencial Térmica , Concentração de Íons de Hidrogênio , Medições Luminescentes , Microscopia de Força Atômica , Nanopartículas/ultraestrutura , Fenômenos Ópticos , Espectrometria por Raios X , Propriedades de Superfície , Termogravimetria , Fatores de Tempo , Compostos de Estanho/química , Difração de Raios XRESUMO
The complexation reactions between the macrocyclic ionophore, p-isopropylcalix[6]arene and Cs+ cation were studied in dimethylsulfoxide-acetonitrile (DMSO-AN) binary non-aqueous solvents at different temperatures using a conductometry method. The conductance data show that the stoichiometry of the (p-isopropylcalix[6]-arene·Cs)+ complex in all binary mixed solvents is 1:1. The stability of the complexes is affected by the composition of the binary solvent media and a non-linear behavior was observed for changes of log K(f) of the complex versus the composition of the binary mixed solvents. The thermodynamic parameters (DH°(c) and DS°(c)) for formation of (p-isopropyl-calix[6]arene·Cs)+ complex were obtained from temperature dependence of the stability constant and the obtained results show that the (p-isopropylcalix[6]arene·Cs)+ complex is enthalpy destabilized, but entropy stabilized, and the values of the mentioned parameters are affected strongly by the nature and composition of the binary mixed solvents.
Assuntos
Acetonitrilas/química , Calixarenos/química , Césio/química , Quelantes/química , Cloretos/química , Complexos de Coordenação/química , Dimetil Sulfóxido/química , Cátions , Condutometria , Solventes , TermodinâmicaRESUMO
An Artificial Neural Network (ANN) based on the Quick Propagation (QP) algorithm was used in conjunction with an experimental design to optimize the lipase-catalyzed reaction conditions for the preparation of a triethanolamine (TEA)-based esterquat cationic surfactant. Using the best performing ANN, the optimum conditions predicted were an enzyme amount of 4.77 w/w%, reaction time of 24 h, reaction temperature of 61.9 °C, substrate (oleic acid: triethanolamine) molar ratio of 1:1 mole and agitation speed of 480 r.p.m. The relative deviation percentage under these conditions was less than 4%. The optimized method was successfully applied to the synthesis of the TEA-based esterquat cationic surfactant at a 2,000 mL scale. This method represents a more flexible and convenient means for optimizing enzymatic reaction using ANN than has been previously reported by conventional methods.
Assuntos
Etanolaminas/química , Análise Multivariada , Redes Neurais de Computação , Tensoativos/síntese químicaRESUMO
A Taguchi robust design method with an L9 orthogonal array was implemented to optimize experimental conditions for the biosynthesis of triethanolamine (TEA)-based esterquat cationic surfactants using an enzymatic reaction method. The esterification reaction conversion% was considered as the response. Enzyme amount, reaction time, reaction temperature and molar ratio of substrates, [oleic acid: triethanolamine (OA:TEA)] were chosen as main parameters. As a result of the Taguchi analysis in this study, the molar ratio of substrates was found to be the most influential parameter on the esterification reaction conversion%. The amount of enzyme in the reaction had also a significant effect on reaction conversion%.
Assuntos
Cátions/química , Química/métodos , Etanolaminas/química , Lipase/metabolismo , Tensoativos/síntese química , Catálise , Modelos Estatísticos , Ácido Oleico/química , Reprodutibilidade dos TestesRESUMO
Fatty hydroxamic acid derivatives were synthesized using Lipozyme TL IM catalyst at biphasic medium as the palm kernel oil was dissolved in hexane and hydroxylamine derivatives were dissolved in water: (1) N-methyl fatty hydroxamic acids (MFHAs); (2) N-isopropyl fatty hydroxamic acids (IPFHAs) and (3) N-benzyl fatty hydroxamic acids (BFHAs) were synthesized by reaction of palm kernel oil and N-methyl hydroxylamine (N-MHA), N-isopropyl hydroxylamine (N-IPHA) and N-benzyl hydroxylamine (N-BHA), respectively. Finally, after separation the products were characterized by color testing, elemental analysis, FT-IR and 1H-NMR spectroscopy. For achieving the highest conversion percentage of product the optimum molar ratio of reactants was obtained by changing the ratio of reactants while other reaction parameters were kept constant. For synthesis of MFHAs the optimum mol ratio of N-MHA/palm kernel oil = 6/1 and the highest conversion was 77.8%, for synthesis of IPFHAs the optimum mol ratio of N-IPHA/palm kernel oil = 7/1 and the highest conversion was 65.4% and for synthesis of BFHAs the optimum mol ratio of N-BHA/palm kernel oil = 7/1 and the highest conversion was 61.7%.
Assuntos
Ácidos Graxos/síntese química , Ácidos Hidroxâmicos/síntese química , Lipase/metabolismo , Óleos de Plantas/química , Elementos Químicos , Óleo de Palmeira , Espectroscopia de Prótons por Ressonância Magnética , Espectroscopia de Infravermelho com Transformada de FourierRESUMO
Formulations containing engkabang fat and engkabang fat esters, F10 and E15 respectively were prepared using a high-shear homogenizer, followed by a high-pressure homogenizer. Both formulations were stable at room temperature, at 45 degrees C, and after undergoing freeze-thaw cycles. The particle sizes of F10 and E15 after high pressure were 115.75 nm and 148.41 nm respectively. The zeta potentials of F10 and E15 were -36.4 mV and -48.8 mV respectively, while, the pH values of F10 and E15 were 5.59 and 5.81 respectively. The rheology of F10 and E15 showed thixotropy and pseudoplastic behavior respectively. There were no bacteria or fungal growths in the samples. The short-term moisturizing effect on 20 subjects analyzed by analysis of variance (ANOVA), gave p-values of 7.35 x 10(-12) and 2.77 x 10(-15) for F10 and E15 respectively. The hydration of the skins increased after application of F10 and E15 with p-value below 0.05.
Assuntos
Dipterocarpaceae/química , Extratos Vegetais/química , Extratos Vegetais/farmacologia , Pele/efeitos dos fármacos , Pele/metabolismo , Bactérias/efeitos dos fármacos , Química Farmacêutica , Emulsões , Ácidos Graxos/química , Ácidos Graxos/farmacologia , Ácidos Graxos/toxicidade , Fungos/efeitos dos fármacos , Humanos , Concentração de Íons de Hidrogênio , Nanotecnologia , Tamanho da Partícula , Extratos Vegetais/toxicidade , Reologia , Dermatopatias , Testes de Irritação da Pele , Propriedades de SuperfícieRESUMO
Mixed dye consists of six commercial dyes and textile effluents from cotton dyeing process were treated by electrochemical-assisted photodegradation under halogen lamp illumination. Two types of effluents were collected which are samples before and after undergone pre-treatment at the factory wastewater treatment plant. The photodegradation process was studied by evaluating the changes in concentration employing UV-vis spectrophotometer (UV-vis) and total organic carbon (TOC) analysis. The photoelectrochemical degradation of mixed dye was found to follow the Langmuir Hinshelwood pseudo-first order kinetic while pseudo-second order kinetic model for effluents by using TOC analyses. The chemical oxygen demand (COD) and biochemical oxygen demand (BOD) values of mixed dye and raw effluents were reported. Photoelectrochemical characteristic of pollutants was studied using the cyclic voltammetry technique. Raw effluent was found to exhibit stronger reduction behaviour at cathodic bias potential but slightly less photoresponse at anodic bias than mixed dye.
Assuntos
Corantes/química , Corantes/efeitos da radiação , Poluentes Químicos da Água/química , Poluentes Químicos da Água/efeitos da radiação , Eletroquímica , Resíduos Industriais , Fotoquímica , Têxteis , Titânio/química , Eliminação de Resíduos Líquidos/métodos , Purificação da Água/métodosRESUMO
Electrochemical-assisted photodegradation of methyl orange has been investigated using TiO2 thin films. The films were prepared by sol-gel dip-coating method. Several operational parameters to achieve optimum efficiency of this electrochemical-assisted photodegradation system have been tested. Photoelectrochemical degradation was studied using different light sources and light intensity. The light sources chosen ranged from ultraviolet to visible light. The effect of agitation of the solution at different speeds has also been studied. Slight improvement of photodegradation rate was observed by applying higher agitation speed. Investigation on the electrode after repeated usages show the electrode can be reused up to 20 times with percentage of deficiency less than 15%. The study on the effect of solution temperature indicated that the activation energy of the methyl orange degradation is 18.63 kJ mol(-1).