Low temperature synthesis and characterization of Mn3O4 nanoparticles

Heating hydrous manganese (II) hydroxide gel at 85 °C for 12 hours produces Mn₃O₄ nanoparticles. They were characterized by X-ray powder diffraction (XRD) and infrared spectroscopy (FTIR). The particle size estimated from the SEM and X-ray peak broadening is approximately 32 nm, showing them to be nanocrystalline. EPR measurements confirm a typical Mn²⁺signal with a highly resolved hyperfine structure.      

Alkylation of ambident indole anion in ionic liquids

Alkylation of indole salts in different ionic liquids is reported. Ionic liquids increase the alkylation reaction rate of ambident indole anion and reduce the effects of counter ions and/or additives, the alkylation reaction rates being independent of the presence of small amounts of protic solvents or water.      

Palladium-catalyzed amination of quinaldine-5-triflate

Palladium-catalyzed amination reactions of quinoline triflate and the effect of a Pd catalyst, its ligands, solvents, bases, and temperature were studied. This method facilitated an easier pathway for the preparation of aminoquinoline derivatives as potential precursors of new serotoninerg agents.      

Review of analytical methods for the determination of chlorine dioxide

The present study reviews more than twenty years (1985-present) of published research on the development and application of analytical procedures for the determination of chlorine dioxide, a widely used disinfectant and bleaching agent. The review covers a variety of techniques including batch and automated spectrophotometry and fluorimetry, electroanalysis and chromatography. The analytical figures of merit to the methods are presented, while critical discussion regarding their advantages and disadvantages is addressed.      

Aminophosphine complex as a catalyst precursor in Suzuki coupling reactions

A palladium complex with an aminophosphine ligand has been prepared and investigated as a catalyst precursor in Suzuki coupling reactions in toluene. Nanoparticles composed of elemental palladium have been isolated from the reaction media and analyzed using transmission electroscopic microscope (TEM), which shows the essential catalysts palladium nanoparticles to have a size of ca. 3.0 nm. dedicate to the 60th birthday of Prof. Dr. Yuan Kou     

Determination of active components in Chinese medicinal preparations by capillary electrophoresis

The determination of paeoniforin, paeonol, and censenoside Rg₁ in traditional Chinese medicinal preparations, Tze Po San Pien pills and Liuwen Dihuang pills has been investigated by micellar electrokinetic capillary electrophoresis with borate buffer (20 mM), sodium dodecylsulfate (30 mM) and acetonitrile (20%) as background electrolytes (pH 9.30), 20 kV applied voltage and 203 nm UV detection. The effects of SDS concentration, borate, buffer pH, and organic modifier on electrophoretic behavior and separation are discussed. Regression equations revealed linear relationships between the peak-area of each component and the content with the correlation coefficients from 0.9982 to 0.9999. In addition, the levels of the active compounds in two kinds of traditional Chinese medicinal preparations were easily determined with the recoveries from 93.1% to 108.2%.      

Separation of Ga(III) from Cu(II), Ni(II) and Zn(II) in aqueous solution using synthetic polymeric resins

Poly (acrylamide-acrylic acid-dimethylaminoethylmethacrylate), p(AM-AA-DMAEM) and Poly(acrylamide-acrylic acid)-ethylenediaminetetracetic acid disodium, p(AM-AA)-EDTANa₂ were prepared by gamma radiation-induced template polymerization technique and used for the separation of Ga (III) from Cu (II), Ni (II), and Zn (II) in aqueous media. The effect of pH and contact time on the separation process was studied. The optimum pH value for the separation process is 3–3.5. The result shows that Ga (III) is first extracted while Cu (II), Ni (II) and Zn(II) are slightly extracted at this pH value. The recovery of metals using HCl, HNO₃ and H₂SO₄ has been studied. The resins may be regenerated using 2M HCl solutions.      

Electrospinning of the hydrophilic poly (2-hydroxyethyl methacrylate) and its copolymers with 2-ethoxyethyl methacrylate

The goal was to electrospin 2-hydroxyethyl methacrylate — based biocompatible polymers and prepare submicron fibres (nanofibers) for biomedicinal applications. Syntheses of poly(2-hydroxyethyl methacrylate) (HEMA) and its copolymer with 2-ethoxyethyl methacrylate (EOEMA), and their characterization by viscometry and molecular weight are described. Their relation to electrospinning is discussed. Electrospinning of HEMA homopolymer from water-ethanol is successful for molecular weights 6.31 × 10⁵ and 1.80 × 10⁶ g/mol. Electrospinning of HEMA/EOEMA copolymers is feasible from ethanol.      

Indirect determination of lutetium by differential pulse anodic stripping voltammetry at a hanging mercury drop electrode

Lutetium has been determined by differential pulse anodic stripping voltammetry in an acidic solution containing Zn-EDTA. Lutetium (III) ions liberated zinc (II), which was preconcentrated on a hanging mercury drop electrode and stripped anodically, resulting in peak current linearly dependent on lutetium (III) concentration. Less than 0.4 ng mL⁻¹ lutetium could be detected after a 2 min deposition.      

Matrix isolation FTIR spectroscopical study of ethene secondary ozonide

A new method is used for the separation of ethene secondary ozonide (SOZ) from the other products of ethene ozonization reaction. The reaction was performed in the neat films of the reactants at 77 K. Ethene SOZ was separated from other products of the reaction by vacuum distillation at 190–210 K and analyzed by means of the matrix isolation IR absorption spectroscopy. Spectroscopic data from photolysis of the matrix isolated ozonide was used as an argument for assignment of the infrared spectral bands either to ethene SOZ or to other products of the reaction. The spectra of ethene SOZ isolated in the Ar matrix were analyzed by combining experimental results with the theoretical calculations performed at the MP2 6-311+G (3df, 3pd) level. A new assignment of some experimental fundamental bands is proposed taking in to account the Fermi resonance between CH stretch and the five membered ring vibrations. For the first time more than 30 weak infrared absorption bands were observed and assigned to various combination vibrations and overtones. By using new spectral information concerning the overtones and the combination bands it is concluded that the dissociation of unstable ethene SOZ involving breaking of any of the four CO bonds of the five membered ring of ethene SOZ has low probability. Dissociation of the ring starts from breaking of the OO bond.      

Analysis of vibratinal spectra of 8-hydroxyquinoline and its 5,7-dichloro, 5,7-dibromo, 5,7-diiodo and 5,7-dinitro derivatives based on density functional theory calculations

The geometry, frequency and intensity of the vibrational bands of 8-hydroxyquinoline and its 5,7-dichloro, 5,7-dibromo, 5,7-diiodo and 5,7-dinitro derivatives were obtained by the density functional theory (DFT) calculations with Becke3-Lee-Parr (B3LYP) functional and 6-31G* basis set. The effects of chloride, bromide, iodide and nitro substituent on the vibrational frequencies of 8-hydroxyquinoline have been investigated. The assignments have been proposed with aid of the results of normal coordinate analysis. The observed and calculated spectra are found to be in good agreement.      

Dopamine and iron mediated fragmentation of galactocerebroside and cardiolipin in micelles

Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) and thin-layer chromatography (TLC) have been used to study dopamine and iron mediated free-radical transformation of lipids in their hydrophilic parts. It has been shown that the action of the dopamine/Fe²⁺ system on galactocerebroside or cardiolipin, which are the components of mixed micelles, results in formation of ceramide or phosphatidic acid and phosphatidylhydroxyacetone, respectively. These data, when combined with results obtained using the ascorbate/Fe²⁺/H₂O₂ oxidizing system with the same substrates, demonstrate that the formation of these products proceeds via an OH-radical induced fragmentation taking place in polar moiety of the starting lipids.      

Synthesis and aqueous solution properties of homologous gemini surfactants with different head groups

A series of homologous gemini surfactants possessing identical hydrophobic chains but different ionic head groups (cationic, anionic, zwitterionic) were synthesized, and their aqueous solution properties were examined. The results showed that the surface activities of gemini surfactants are superior to those of corresponding conventional monomeric surfactants, and molecular arrangements of gemini surfactants at the air-water interface are tighter than those of corresponding conventional surfactants. It was also found that zwitterionic gemini surfactant possesses the highest surface activity among the three surfactants. The behavior at the air-water interface is closely related to the molecular structural features of surfactants, which provide an indication for synthesizing highly-efficient surfactants.      

Influence of surfactants on the fading of malachite green

The kinetics of the reaction between malachite green (MG) and sodium hydroxide (MG fading) was studied using a spectrophotometric method in the presence of two cationic surfactants, cetyl-benzyl-dimethyl-ammonium chloride (CBDAC) and hexadecyl-trimethylammonium bromide (HTAB) and one anionic surfactant, sodium dodecyl sulphate (SDS) at concentrations below and above critical micellar concentrations. The cationic surfactants have a catalytic effect, while the anionic surfactant has an inhibitory effect on the reaction. A kinetic model describing the influence of surfactant on reaction rate was developed. The results are discussed on the basis of electrostatic and hydrophobic interactions between the kinetic micelles and malachite green.      

Surface analysis of the size-fractioned urban aerosols by secondary ion mass spectrometry (ToF-SIMS)

The secondary ion mass spectrometry method (ToF-SIMS) has been applied to the analysis of some mineral and organic species on the surface layers of airborne urban particulates. Particulate matter was collected on aluminum sheets of the 8-stage Anderson type cascade impactor from three different sampling sites in the city of Lodz, Poland, which were different in terms of aerosol source apportionment. The obtained results show that vehicle combustion products occur mainly in fine fraction with aerodynamic diameters below 1μm. The main contribution to the mineral components comes from direct and traffic related soil resuspension.      

Esterification of palmitic acid with epichlorohydrin on anion exchange resin catalyst

The esterification reaction of palmitic acid with epichlorohydrin catalyzed by an anionic macroporous resin was studied. Purolite A-500 resin proved to be a very effective catalyst in the synthesis of 3-chloro-2-hydroxypropyl palmitate. The effects of certain parameters such as speed of agitation, catalyst particle size, catalyst loading, temperature, initial molar ratio between reactants on the rate of reaction were studied. It was found that the overall rate is intrinsically kinetically controlled. The structure of synthesized ester was confirmed by FTIR and ¹H NMR analyses.      

Polyaniline-polypyrrole coating for solid phase microextraction

A procedure for direct electrochemical deposition of polyaniline-polypyrrole blend coating on the surface of stainless steel wire was suggested. Incorporation of polyaniline and polypyrrole into the blend coating was confirmed by infrared spectroscopy. Key parameters (pyrrole, aniline, dopant and sulphuric acid concentrations and deposition potential) influencing the coating’s mechanical stability and surface homogeneity were optimised and thermostability of the coating was investigated. A possibility to apply the coating as a new fibre for solid phase microextraction was demonstrated. The coating showed better selectivity toward aromatic, hydrophobic compounds.      

Ionic liquid-functionalized SBA-15 mesoporous material: efficient heterogeneous catalyst in versatile organic reactions

Ionic liquid-functionalized mesoporous materials exhibited high catalytic activity in versatile organic reactions, such as cycloaddition of carbon dioxide (CO₂) with epoxide, aza-Michael addition of amines to α, β-unsaturated carbonyl compounds, and the Biginelli reaction of aldehyde, ethyl acetoacetate and urea. Recycling of the catalyst in these reactions could be carried out and the catalyst used at least five times without significant loss in activity.      

ICP slurry introduction for simple and rapid determination of Pb, Mg and Ca in plant roots

Pb, Mg and Ca were simultaneously determined in plant roots by slurry introduction into inductively coupled plasma optical emission spectrometry (SS-ICP-OES). Slurries were prepared in 0.5% or 5% (v/v) HNO₃ with 0.5, or 5% (v/v) Triton X-100. Omission of the Triton X-100 improved results. Compared with wet ashing of the root sample followed by ICP-OES, ICP-MS and FAAS, the method offers: comparable results, simplification of sample preparation, less sample contamination, and reduction in the use of dangerous and corrosive reagents. The precisions varied: 1.7% for Mg, 2.8% for Ca and 4.3% for Pb, and were not significantly different (95% confidence level) from those of conventional analysis.      

Differential pulse voltammetric determination of dopamine with the coexistence of ascorbic acid on boron-doped diamond surface

Electrochemical determination of dopamine (DA) in the presence of ascorbic acid (AA) was achieved on boron-doped diamond (BDD) film electrode by differential pulse voltammetry. The experimental results indicated that the oxidative peaks of DA and AA could be separated completely on anodically-treated (BDD) electrode without further modification, although these two peaks can not be separated on glassy carbon electrode. The peak separation of DA and AA was developed to be 0.44 V. High sensitivity was obtained to determine DA selectively with the coexisting of a large excess of AA in acidic media by DPV. The detection limit of DA was achieved to be 1.1 × 10^-6 M in the presence of AA with the concentration of 200 times more than DA. This technique was also applied to the determination of DA in real samples.