The use of ultrasonic treatment for improvement of metrological performance of sorption atomic absorption determination of lead(II) and cadmium(II) traces

The optimal parameters for ultrasonic treatment (frequency 200–300 kHz, intensity 2–4 W cm^?2) were obtained to intensify Pb(II) and Cd(II) sorption concentration by carbon sorbent from apricot pit. The combined action of ultrasonic frequency of 18 kHz and 1 MHz on concentrate slurry increases its sedimentation stability from 3 to 180 minutes and decreases S_r value up to 7% at Pb(II), Cd(II) hybrid sorption atomic absorption determination in natural waters, brines, common salt.      

Nonenzymatic sensor for hydrogen peroxide based on the electrodeposition of silver nanoparticles on poly(ionic liquid)-stabilized graphene sheets

We have developed a nonenzymatic sensor for hydrogen peroxide (HP) that is based on a new kind of nanocomposite consisting of silver nanoparticles (AgNPs) electrodeposited on a basic film of a poly(ionic liquid) containing graphene. The nanocomposite was characterized by scanning electron microscopy, energy dispersive X-ray studies, cyclic voltammetry, and chronoamperometry. The AgNPs on the basic composite film provide the electrode with enhanced sensitivity in that the signal obtained for HP is 10-fold improved in the best case. The sensor exhibits good linear response in the 0.1 μM to 2.2 mM HP concentration range, and the detection limit is 0.05 μM (at S/N?=?3).      

Microstructures and growth characteristics of polyelectrolytes on silicon using layer-by-layer assembly

Growth processes of nanocomposite layers obtained by polyelectrolytes, poly(sodium 4-styrenesulfonate) (PSS) and poly(diallyldimethylammonium chloride) (PDADMAC), self-assembled on silicon surface using layer-by-layer (LbL) technique were investigated, and theoretical and experimental data are herein reported. Complementary microstructural and compositional analyses techniques (scanning electron microscopy, ellipsometry, X-ray reflectivity, zeta (ξ) potential measurements and attenuated total reflection infrared spectroscopy) were used for deep characterization of the multilayer structure formation. Electrophoretic zeta (ξ) potential measurements indicated that the surface charge was either positive or negative, depending on the polyelectrolyte used (PDADMAC or PSS). ATR-IR spectra confirmed the successfully silanization process and then, the building up of the nanocomposite layer. Morphological investigation and X-ray reflectivity demonstrated the growth process and cross-section size of the bilayers. Ellipsometric measurements were in very good agreement with SEM and XRR, showing once again the successful deposition of polyelectrolyte multilayers.      

Polymer conjugates with potential biological activity based on new derivatives of 2-mercaptobenzoxazole-synthesis and characterization

New potentially biologically active compounds derived from 2-mercapto-benzoxazole were synthesized and coupled on polymeric support of poly (maleic anhydride-alt-vinyl acetate) for the preparation of polymer-drug conjugates with controlled drug release. All compounds were characterized by elemental and spectroscopy (FT-IR, ¹H-NMR) analysis. The toxicological tests recommend the products for further laboratory screening.      

Determination of lead in solution by solid phase extraction, elution, and spectrophotometric detection using 4-(2-pyridylazo)-resorcinol

Lead (+2) was selectively adsorbed on a solid phase extraction (SPE) gel (molecular recognition technology, MRT), quantitatively extracted, and spectrophotometrically determined as the Pb(II)-PAR (4-(2-pyridylazo)-resorcinol) complex. The linear range was 0.01 to 0.75 mg L^?1 and the detection limit was 6.4 µg L^?1. The MRT-SPE allows selective Pb(II) extraction from complex ion-rich matrices, which is difficult with other techniques. Interference from common matrix ions such as Fe²⁺, Ni²⁺, Cu²⁺ or Co²⁺ is minimized.      

Synthesis,structure and capacitive properties of cobalt hydroxide films on stainless steel substrates

Cobalt (hydro)oxide films on AISI 304 stainless steel and sintered metal fibre filter Bekipor ST 20AL3 were prepared using electrochemical deposition from neutral cobalt acetate solutions under galvanostatic conditions. Deposited films were structurally characterized using X-ray diffraction, Fourier transform infrared spectroscopy and scanning electron microscopy. All electrochemical measurements were performed in aqueous NaOH solution. Capacitive behavior of different films was evaluated using cyclic voltammetry data. The highest specific capacitance (965 F g^?1) was reached when Bekipor ST 20AL3 mesh was used as a support for electroactive substance.      

Preparation of selectively protected protoescigenin derivatives for synthesis of escin analogs and neoglycoconjugates

Protoescigenin, the main aglycone of horse chestnut saponin mixture known as escin, was selected as substrate for exploratory chemistry towards selective protection, followed by propargyl ether formation and subsequent condensation with azido-monosaccharides, to obtain novel triazole linked conjugates of the triterpene.      

Optimization of synthesis conditions and the study of magnetic and dielectric properties for MgFe2O4 ferrite

Nano-sized magnesium ferrites were synthesized by the sol-gel auto-combustion method using a variety of chelating/combustion agents: tartaric acid, citric acid, cellulose, glycine, urea and hexamethylenetetramine. The original purpose of this work was the synthesis of nano-sized magnesium ferrite by using, for the first time, cellulose and hexamethylenetetramine as chelating/combustion agents. Synthesized samples were subjected to different heat treatments at 773 K, 973 K and, respectively 1173 K in air. The disappearance of the organic phase and nitrate phase with the spinel structure formation was monitored by infrared absorption spectroscopy. Spinel structure, crystallite size and cation distribution were evaluated by X-ray diffraction data. The morphology of as-prepared powders was studied using scanning electron microscopy. The magnetic and dielectric properties were studied for the obtained samples.      

Experimental and computational investigations of a cadmium(II) mononuclear complex with 2,6-Bis(3,5-dimethyl-N-pyrazolyl)pyridine (bdmpp) and selenocyanate as ligands

A new cadmium (II) complex, [Cd(bdmpp)(SeCN)₂(H₂O)] (1) (where bdmpp = 2,6-bis(3,5-dimethyl-N-pyrazolyl)pyridine), has been synthesized and characterized by elemental and spectral (IR, ¹H-NMR and ¹³C-NMR, UV-Vis) analyses, differential scanning calorimetry, and single crystal X-ray diffraction studies. X-ray analysis showed that the structure was crystallized in the monoclinic space group Cc with a = 9.031(2), b = 13.884(3), c = 16.910(3) Å, and Z = 4. The geometry around the cadmium atom is distorted octahedral with a CdN₃Se₂O setup. The N atoms of the SeCN are engaged in two strong intermolecular H-bonding interactions forming a 3D supramolecular polymeric network. The geometry and vibrational frequencies of complex 1 computed with the DFT methods (BLYP, B3LYP, B3PW91, MPW1PW91) are in better agreement with experiment than those obtained with the ab-initio method except for the bond angles. The molecular orbital diagram has been also calculated and visualized at the B3LYP/LanL2DZ level of theory.      

Fabrication of superhydrophobic surface of stearic acid grafted zinc by using an aqueous plasma etching technique

A stable superhydrophobic surface of stearic acid grafted zinc was fabricated with two steps, that is, the zinc surface was firstly treated with glow discharge electrolysis plasma (GDEP) and then followed by a grafted reaction of stearic acid onto the treated zinc surface. Results indicated that the wettability of zinc substrate changed from superhydrophily to superhyphodrobicity with a water contact angle (CA) up to 158° and a water sliding angle (SA) less than 5°. The surface morphology and composition were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD), respectively.      

Biodegradation of Benzo[a]Pyrene through the use of algae

In this work for disposal of the biologically hard decomposed pollutant Benzo[a]Pyrene (BaP) photooxidation Chlorella kessleri was used. The simulation model system under the different experimental conditions (varying biomass and light intensity) was evaluated. For quantitative analysis of the decrease in BaP, GC/MS technique was used. The highest degradation efficiency was achieved in the case of biomass from the culture of live algae (29%) and light intensity at level of 13.5 W m^?2. When the dry biomass was used, degradation under the same conditions was lower because of lack of enzymatic activity in the system.      

New carbon from low cost vegetal precursors: acorn and cypress cone

Thermal-treated carbons from acorn and cypress cone were prepared and characterized. The uptakes of heavy metal ions (Ag⁺, Cd²⁺ and Cr⁺³) and organics (phenol, methylene blue and sodium dodecylbenzenesulfonate) from aqueous solution have been studied. Effects of activation by HCl and HNO₃ acids on the sorption properties of these carbons were investigated by mass titration, sorption isotherms, IRS, SEM and XRS. The models of Langmuir and Freundlich do not represent our sorption data very well. An earlier proposed empirical correlation is applied successfully to carry out a parameter of comparison between the studied carbons. The acidic treatment changes the surface chemical properties of the two thermal-treated carbons lowering their sorption performances. The carbons show good capacities to uptake metals, phenol and methylene blue, but sodium dodecylbenzenesulfonate is removed from its solutions to minor extent. The up-taking properties are found similar to those of two worldwide used commercial grade carbons.      

Synthesis of terbium(III) complex with a biscoumarin derivative and its immobilization in PMMA-based composite thin films with fluorescent properties

An amorphous complex of Tb(III) with the biscoumarin derivative 3,3′-[(4-hydroxyphenyl)methylene)]bis-(4-hydroxy-2H-1-benzopyran-2-one), Tb(H₂L)₃, was successfully synthesized and characterized. IR- and ¹H-NMR-spectroscopy were used to investigate the coordination of the ligand around the Tb(III) ion. Values for the quantum yield and the life time of the excited state of the complex were obtained. The complex was immobilized in transparent and flexible PMMA-based films by a simple casting technique. PMMA/chloroform solutions were used in synthetic procedures that resulted in both glass-supported and self-supporting nanocomposite films. The morphology of the films was studied by scanning electron microscopy, atomic force microscopy and transmission electron microscopy, showing the formation of crack-free films. The presence of the Tb(III) complex in the matrix was proven by the presence of characteristic bands in the IR spectra. Fluorescence microscopy and fluorescence spectroscopy demonstrated the promising optical properties of the films showing the characteristic emission bands of the Tb(III) ions. The longer life time of the excited state of the immobilized complex confirmed the protective role of the PMMA matrix on the optical properties of the complex. The composite films possessing optical properties have the potential for application as active components in optical devices.      

Biosorption of reactive dye from aqueous media using Saccharomyces cerevisiae biomass. Equilibrium and kinetic study

The biosorption Brilliant Red HE-3B reactive dye by nonliving biomass, Saccharomyces cerevisiae, in batch procedure was investigated. Equilibrium experimental data were analyzed using Freundlich, Langmuir and Dubinin — Radushkevich isotherm models and obtained capacity about 104.167 mg g^?1 at 20°C. The batch biosorption process followed the pseudo-second order kinetic model. The multi-linearity of the Weber-Morris plot suggests the presence of two main steps influencing the biosorption process: the intraparticle diffusion (pore diffusion), and the external mass transfer (film diffusion). The results obtained in batch experiments revealed that the biosorption of reactive dye by biomass is an endothermic physical-chemical process occurring mainly by electrostatic interaction between the positive charged surface of the biomass and the anionic dye molecules. The biosorption mechanism was confirmed by FT-IR spectroscopy and microscopy analysis      

Electrode processes of selected redox active substances on poly(o-aminophenol) film electrode

Using the method of cyclic voltammetry, the electrode process of Ni²⁺, Pb²⁺, Cu²⁺ and pyrocatechin on a poly(o-aminophenol) (PoAP) modified glassy carbon electrode (GCE) was investigated. The PoAP polymer was found to affect the redox process of copper and pyrocatechin. The use of polymer of different thicknesses showed that the obtained film has a dense, nonporous structure. The redox process of the examined substances may be considered as proceeding on the polymer surface. The PoAP polymer obtained in the described conditions takes part in charge transfer.      

Mechanical, thermal and surface properties of polyacrylamide/dextran semi-interpenetrating network hydrogels tuned by the synthesis temperature

The mechanical, rheological, thermal, and surface behaviors of three polyacrylamide/dextran (PAAm/Dx) semi-interpenetrating polymer network (semi-IPN) hydrogels, prepared at 22°C, 5°C and ?18°C, were investigated. The results were compared with those obtained on cross-linked PAAm without Dx synthesized under the same conditions. Hydrogels prepared at the lowest temperature were the most mechanically stable. The thermal stability of the semi-IPN hydrogels is slightly lower than the corresponding PAAm gels, irrespective of preparation temperature. The water vapor sorption capacity depended on the presence of Dx as well as preparation temperature, which determines the network morphology.      

Metals content of soil,leaves and wild fruit from Serbia

The concentrations of Zn, Mn, Fe, Pb, Ni, Cu and Cd in soil, leaves and edible wild fruit (Crataegus laevigata L., Cornus mas L. and Prunus spinosa L.) from southeast Serbia were determined by atomic absorption spectroscopy. Metal translocations from soil to fruit were calculated as well as their oral intake and health risk indices. Positive correlations were found among metal concentrations in soil, leaves and fruit.      

Use of peat-based sorbents for removal of arsenic compounds

It is important to apply sorbent materials for purification of water from arsenic contamination due to serious arsenic pollution worldwide. We have developed new sorbents based on natural materials that provide a cheap and environmentally friendly alternative. For the first time, peat modified with iron compounds and iron humates were tested for sorption of arsenic compounds. The highest sorption capacity was found in peat modified with iron compounds. We have found that sorption of different arsenic speciation forms was strongly dependent on solution pH, reaction time and temperature. Calculations of the sorption process using thermodynamic parameters indicate the spontaneity of sorption process and its endothermic nature. Sorption kinetics showed that most arsenates are removed within 2 hours, and the kinetics of arsenate sorption on modified peat can be described by the pseudo-second order mechanism.      

Optimization methodology based on neural networks and genetic algorithms applied to electro-coagulation processes

An optimization methodology based on neural networks and genetic algorithms was developed and used to optimize a real world process — an electro-coagulation process involving three pollutants at different concentrations: kaolin (250–1000 mg L^?1), Eriochrome Black T solutions (50–200 mg L?1), and oil/water emulsion (1500–4500 mg L^?1). Feed-forward neural networks using heterogeneous combination of transfer functions were developed, leading to good results in the validation stage (relative error about 8%). The parameters of the process (concentration of pollutant, time, pH₀, conductivity and current density) were optimized handling the genetic algorithm parameters, in order to obtain a maximum removal efficiency for each pollutant. Therefore, the optimization methodology combines neural networks as modeling tools with genetic algorithms as solving method. Validation of the optimization results using supplementary experimental data reveals errors under 11%.