Removal of Pb and Cd from aqueous media and fish liver using novel polyurethane foam functionalized with pyrazolone as a new metal ion collector

In the present paper, an off-line preconcentration procedure for the determination of cadmium and lead by flame atomic absorption spectrometry (FAAS) is proposed. Polyurethane foam (PUF) functionalized with o-aminophenol (o-AP) followed by Pyrazolone (Pyr) packed in a minicolumn was used as a sorbent material. The metals were retained on the modified PUF, from which it could be eluted and effectively preconcentrated. The detection limits were 0.072 and 0.016 μg L⁻¹ for Pb and Cd respectively. Enrichment factors were 250 and 319 for lead and cadmium respectively. The procedure has been applied successfully to metal determination in water samples, fish liver and reference material.      

Cloud point extraction-preconcentration and flame atomic absorption spectrometric determination of low levels of zinc in water and blood serum samples

A simple, sensitive and selective flotation method is described for the preconcentration and atomic absorption spectrometric determination of zinc ion in water and blood samples. At a solution pH of 5.2, 4-(2-pyridylazo-resorcinol) and Triton X-114 were used as hydrophobic ligand and non-ionic surfactant, respectively. The chemical variables affecting the preconcentration process were optimized. Under the optimized experimental conditions, the selective preconcentration and determination of as low zinc concentration as 6.5 μg L⁻¹ can be made. The proposed method was successfully applied to the preconcentration and low-level determination of zinc in different water and blood serum samples.      

Dispersive liquid-liquid microextraction and liquid chromatographic determination of pentachlorophenol in water

A simple and sensitive dispersive liquid-liquid microextraction method for extraction and preconcentration of pentachlorophenol (PCP) in water samples is presented. After adjusting the sample pH to 3, extraction was performed in the presence of 1% W/V sodium chloride by injecting 1 mL acetone as disperser solvent containing 15 μL tetrachloroethylene as extraction solvent. The proposed DLLME method was followed by HPLC-DAD for determination of PCP. It has good linearity (0.994) with wide linear dynamic range (0.1–1000 μg L⁻¹) and low detection limit (0.03 μg L⁻¹), which makes it suitable for determination of PCP in water samples.      

Flame atomic absorption spectrometric determination of trace amounts of lead, cadmium and nickel in different matrixes after solid phase extraction on modified multiwalled carbon nanotubes

The potential of modified multiwalled carbon nanotubes (a solid-phase extraction sorbent), for the simultaneous separation and preconcentration of lead, cadmium and nickel; has been investigated. Lead, cadmium and nickel, were adsorbed quantitatively; on modified multiwalled carbon nanotubes (in the pH range of 2–4). Parameters influencing, the simultaneous preconcentration of Pb(II), Ni(II) and Cd(II) ions (such as pH of the sample, sample and eluent flow rate, type and volume of elution solution and interfering ions), have been examined and optimized. Under the optimum experimental conditions, the detection limits of this method. for Pb(II), Ni(II) and Cd(II) ions, were 0.32, 0.17 and 0.04 ng mL⁻¹ in original solution, respectively. Seven replicate determinations, of a mixture of 2.0 μg mL⁻¹ lead and nickel, and 1.0 μg mL⁻¹ cadmium; gave a mean absorbance of 0.074, 0.151 and 0.310, with relative standard deviation 1.7%, 1.5% and 1.2%, respectively. The method has been applied, to the determination of trace amounts of lead, cadmium and nickel; in biological and water samples, with satisfactory results.      

Ionic liquid promoted Diels-Alder Reaction between anthrone and maleimides

Ionic liquids (IL) are gaining importance as green solvents. Imidazolium ionic liquid [bmim]⁺[Cl]⁻, an environmentally benign solvent, was found to promote the Diels-Alder reaction between anthrone and maleimides at room temperature with excellent yields. The ionic liquid played a dual role as solvent and catalyst.      

Structure, conformation and hydrogen bonding of two amino-cycloalkanespiro-5-hydantoins

The crystal structures of 3-amino-cycloheptanespiro-4′-imidazolidine-2′,5′-dione (I) {systematic name: 3-amino-1,3-diazaspiro[4.6] undecane-2,4-dione} and 3-amino-cyclooctanespiro-4′-imidazolidine-2′,5′-dione (II) {systematic name: 3-amino-1,3-diazaspiro[4.7] dodecane-2,4-dione}, have been determined. In both compounds the polar hydantoin groups cause molecules to aggregate via N-H...O and N-H...N interactions, forming a layer structure, in which the cycloalkane rings project outwards from the central, more polar, region. The observed molecular structure is compared with that calculated by density functional theory methods.      

Unusual reaction of 3,4-bis(3-nitrofurazan-4-yl)furoxan with ammonia,primary amines and hydrazine

The nucleophilic displacement of two nitro groups in 3,4-bis(3-nitrofurazan-4-yl)furoxan with ammonia, primary aliphatic amines and hydrazine leads to formation of a novel heterocyclic system, 7H-tris[1,2,5]oxadiazolo[3,4-b:3′,4′-d:3″,4″-f]azepine. The reaction of compound 1 with secondary aliphatic amines proceeds in a typical way for nitrofurazans when the nitro-group in the starting compound is substituted by RR’N-group.      

Preliminary results of a quick,simple method of detecting antimony in water samples

Preliminary results of development of a direct and fast method of determination of antimony in samples of tap water using GFAAS are presented. The found levels of antimony were lower than permitted for human consumption. A mixture of Pd and Mg(NO₃)₂ (concentrations in the injected solution: 8.6 μg mL⁻¹ and 5.8 μg mL⁻¹ respectively) was used as the chemical modifier. The pyrolysis and atomization temperatures were 1000 and 1700°C, respectively and the mean analytical recovery 98.2%.      

Cobalt(II) ion-selective electrode with solid contact

A new all plastic sensor for Co²⁺ ions based on 2-amino-5 (hydroxynaphtyloazo-1′)-1,3,4 thiadiazole (ATIDAN) as ionophore was prepared. The electrode exhibits a low detection limit of 1.5 × 10⁻⁶ mol L⁻¹ and almost theoretical Nernstian slope in the activity range 4.0 × 10⁻⁶–1 × 10⁻¹ mol L⁻¹ of cobalt ions. The response time of the sensor is less than 10 s and it can be used over a period of 6 months without any measurable divergence in potential. The proposed sensor shows a fairly good selectivity for Co(II) over other metal ions. The electrode was successfully applied for determination of Co²⁺ in real samples and as an indicator electrode in potentiometric titration of Co²⁺ ions with EDTA.      

Determination of diclofenac in pharmaceuticals and urine samples using a membrane sensor based on the ion associate of diclofenac with Rhodamine B

The potentiometric response characteristics of a diclofenac selective electrode, based on ion association in different plasticizers, were compared. The sensitivity, working range, detection limit and selectivity of membrane sensors demonstrated significant dependence on the type of plasticizers. The potentiometric unit presented a linear response toward diclofenac concentrations between 1 × 10⁻⁵ − 5 × 10⁻² mol L⁻¹, with slopes of approximately 60 mV dec⁻¹, and exhibited a response time of 3 s. The potentiometric analysis of sodium diclofenac in pharmaceutical formulations was perfomed by the membrane electrode proposed and compared with the results of potentiometric titration given by the Pharmacopoeia of Ukraine.      

Diironcarbonyl-coumarin complex: preparation, intramolecular electron transfer, and electro-generation of hydrogen

A new organometallic complex coupling photoactive coumarin to a diironhexacarbonyl unit has been successfully prepared and its composition and electronic structure confirmed by elemental and spectroscopic analyses. Emission spectral analysis of the complex reveals photoinduced intramolecular electron transfer from coumarin to the iron-carbonyl moiety. The compound is electrochemically reduced at −1.24 V vs. Fc/Fc⁺. This reduction is irreversible, attesting to the instability of the complex. Electrochemical evolution of hydrogen in the presence of the complex has been studied and results are discussed.      

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.      

One-pot, three-component condensation of 2-hydroxybenzaldehyde derivatives, primary amines with alkyl isocyanides to N-alkyl-2-(2-hydroxyphenyl)-2-imino-acetamides

One-pot, three-component condensation of 2-hydroxybenzaldehyde derivatives, primary amines with alkyl isocyanides is reported. N-alkyl-2-(2-hydroxyphenyl)-2-iminoacetamide derivatives are generated presumably via the preliminary formation of N, N′-disubstituted benzo[b]furan-2,3-diamines and subsequent oxidation with molecular oxygen.      

Meldola’s Blue — doped titania sol-gel sensor for NADH determination

Titania layers obtained by a sol-gel technique doped with redox mediator, Meldola’s Blue, were employed for construction of a new NADH senor. Optimization of preparation process as well as experimental conditions affecting the response of the sensor were examined. Under optimal conditions NADH could be determined in the wide linear range from 90 to 2300 μM with detection limit 12 μM and a high sensitivity 12.5 nA μM⁻¹. The usefulness of developed sensor was preliminarily checked in determination of NADH forming during enzymatic oxidation of ethanol catalyzed by alcohol dehydrogenase (ADH).      

Immobilization of quaternary ammonium salts on silica gel for perchlorate ions removal

Silica surface was modified with quaternary ammonium salts to give three matrices of different chain length. The synthesized supports were characterized by elemental analysis and infrared spectroscopy, as well as scanning electron microscopy and semi-empirical parametric method 5. Their exchange capacities for ClO₄ ⁻, F⁻, NO₃ ⁻ and CH₃COO⁻ ions were investigated by conductometric titration. The amount of exchanged chloride ions from the matrix was studied for different initial anions concentration. The functionalized silica gel showed very good ability of perchlorate ions exchange from the water solution in room temperature. The anion-exchange properties were also studied in comparison to different number of reactive sites in the matrices. The increased number of chloride at the silica surface took effect on increased ability of ClO₄ ⁻ anion exchange      

Hollow fibre liquid phase microextraction of parabens

A hollow fibre liquid phase microextraction for gas chromatographic determination of some p-hydroxybenzoic acid esters has been developed. Chlorobenzene containing tetradecane as internal standard was used for the extraction. Optimized extraction was carried out at room temperature for 40 min in the presence of 0.4 g mL⁻¹ NaCl in the sample solution. Calibration was linear up to 30 mg L⁻¹. Correlation coefficients were 0.996–0.998. Enrichment factors were 21, 95 and 154, and detection limits were 0.20, 0.03 and 0.01 μg mL⁻¹ for methylparaben, ethylparaben and propylparaben, respectively. Reproducibility was acceptable with relative standard deviations up to 11.7%. The technique was tested for water and urine analysis.      

Density functional theory study of the photosensitization mechanisms of indigo

The triplet excited state properties and photosensitization mechanisms of indigo were investigated based on density functional theory calculations. The solvent effects on the photosensitization mechanisms of indigo have also been considered. The thermodynamic feasibility of the possible ¹O₂ and O₂·⁻-photogeneration pathways by triplet excited state indigo in different solvents was explored, in order to gain some deeper insights into the photosensitization characters of the dye.      

Nickel and palladium complexes of enolatefunctionalised N-heterocyclic carbenes

The reaction of chloroethyltrimethylsilylether with 1-methylimidazole furnishes an ionic liquid that undergoes methanolysis to crystalline 2-hydroxyethylimidazolium chloride (crystal structure presented). Conversion to defined hydroxyethylimidazol-2-ylidene nickel complexes failed, but was accomplished with 1-methyl-3-acetophenyl-imidazolium bromide. The bis(NHC^⋂O⁻) nickel(II) chelate is formed, rather than a methallylnickel monochelate, but with nickelocene a monochelate NiCp complex was detected. The bulky 1-(2,6-diisopropylphenyl)-3-(2’-phenyl-enolato)-imidazol-2-ylidene allylpalladium chloride was obtained in pure form. Attempts to generate catalysts for ethylene oligomerization by in situ techniques have failed so far whereas P^⋂O⁻ ligands, comparable by the P-C diagonal relationship, provide active catalysts.      

Determination of submillimolar concentration of ferrate(VI) in alkaline solutions by amperometric titration

A new amperometric titration method was developed for quantitative determination of ferrate(VI) (Fe^VIO₄ ²⁻) in the 7.06×10⁻⁵−5.73×10⁻³ M concentration range. Chromium(III) hydroxide solution was used as the titrant. The diffusion current (Id) had a linear relationship with the concentration of ferrate(VI) and slopes were dependent on the concentration of NaOH. The amperometric titration could detect a lower concentration of ferrate(VI) than could potentiometric and colorimetric titrations. The method was applied successfully to determine concentrations of ferrate(VI), generated electrochemically, in strong alkaline solutions.      

Synthesis by self-assembly and structural characterization of a new co-crystal system {[Cu(NO3)2(H2O)2]L1(NO3)2} (L1 = 1,1′-dibenzyl-3,3′-butyl-diimidazolium-2,2′-diylidene) from copper nitrate and a carbene precursor

Herein, the first example of a co-crystal system formed by an imidazolium nitrate, a carbene precursor, and copper (II) nitrate, {[Cu(NO₃)₂(H₂O)₂]L1(NO₃)₂} (1) (L1 = 1,1′-dibenzyl-3,3′-butyl-diimidazolium-2,2′-diylidene) is reported. These two building blocks are connected in the solid state through hydrogen bonds to generate a three-dimensional supramolecular network.