Pd-catalyzed synthesis of 3-(diarylmethylene)-2-oxindoles and 3-(arylmethylene)-2-oxindoles

An efficient method for the stereoselective synthesis of 3-(diarylmethylene)-2-oxindoles and 3-(arylmethylene)-2-oxindoles via carbopalladation is described. In this approach, an Ugi-4-component reaction (4-CR) adduct was used as the starting material. A one-pot sequence involving intermolecular carbopalladation C-H activation/C-C bond formation efficiently afforded the oxindole derivatives.     

Efficient iodination of aromatic compounds using potassium ferrate supported on montmorillonite

Potassium ferrate impregnated on montmorillonite is a mild,cheap,and non-toxic reagent for the iodination of phenols, including naphthol,aromatic amines,and heterocyclic substrates in fair to excellent yields by a simple isolation procedure.     

Flame atomic absorption spectrometric determination of trace amounts of palladium,gold and nickel after cloud point extraction

In this article, a sensitive cloud point extraction procedure for the preconcentration of trace amounts of palladium, gold and nickel prior to their determination by flame atomic absorption spectrometry has been developed. The cloud point extraction method is based on the complexation of Pd(II), Au(II), and Ni(II) ions with 1-(2-pyridylazo)-2-naphthol and entrapping in non-ionic surfactant Triton X-114. The main factors affecting cloud point extraction efficiency, such as pH of sample solution, concentration of 1-(2-pyridylazo)-2-naphthol and Triton X-114, equilibration temperature and time, were investigated in detail. Under the optimized conditions, calibration curves were constructed for the determination of palladium, gold and nickel according to the general procedure. Linearity was maintained from 0.01 to 1.0 μg/mL for palladium, 10.0 μg/mL to 1.5 μg/mL for gold, and 10.0 μg/mL to 0.5 μg/mL for nickel. Detection limits based on three times the standard deviation of the blank divided by the slope of analytical curve (3Sb/m) for Pd(II), Au(III), and Ni(11) ions were 3.4, 3.9, and 2.4 μg/mL, respectively. Seven replicate determination of a mixture of 0.5 μg/mL palladium and gold and 0.2 μg/mL nickel gave a mean absorbance of 0.174, 0.150, and 0.201 with relative standard deviation ±1.5, ±1.3, and ±1.8%, respectively. The high efficiency of cloud point extraction to carry out the determination of analytes in complex matrices was demonstrated. The proposed method has been applied for determination of trace amount of palladium, gold and nickel in certified reference material and water samples with satisfactory results.     

Rapid green synthesis of gold nanoparticles using Rosa hybrida petal extract at room temperature

This study reports a green method for the synthesis of gold nanoparticles using the aqueous extract of rose petals. The effects of gold salt concentration, extract concentration and extract quantity were investigated on nanoparticles synthesis. Gold nanoparticles were characterized with different techniques such as UV-vis spectroscopy, FT-IR spectroscopy, X-ray diffraction, energy dispersive X-ray spectroscopy, dynamic light scattering and transmission electron microscopy. Transmission electron microscopy experiments showed that these nanoparticles are formed with various shapes. FT-IR spectroscopy revealed that gold nanoparticles were functionalized with biomolecules that have primary amine group (-NH2), carbonyl group, -OH groups and other stabilizing functional groups. X-ray diffraction pattern showed high purity and face centered cubic structure of gold nanoparticles. Dynamic light scattering technique was used for particle size measurement, and it was found to be about 10nm. The rate of the reaction was high and it was completed within 5 min.     

Ionic liquid-based dispersive liquid–liquid microextraction for the separation and preconcentration of lead in water samples prior to FAAS determination without chelating agent

In the present study, an environment-friendly sample preparation method termed ionic liquid-based dispersive liquid–liquid microextraction combined with flame atomic absorption spectrometry has been developed for the determination of Pb(II) ion in water samples prior to flame atomic absorption spectrometry determination. In this method, ionic liquid was used as an extraction solvent instead of the organic solvent used in the conventional dispersive liquid–liquid microextraction (DLLME) assay, and there is no need for a chelating agent. Several variables that may affect extraction efficiencies, including pH, the volume of ionic liquid, the type and volume of disperser solvent, salt addition, and the time for centrifugation and extraction were studied and optimised. Under the optimised conditions, the calibration curve exhibited linearity over the range of 20.0–1000.0 μg L^?1. The enrichment factor and the limit of detection based on 3S_b/m were 35.0 and 5.9 μg L^?1, respectively. Seven replicate determination of a solution containing of 100.0 μg L^?1 Pb(II) ions gave a relative standard deviation of ±2.1%. Finally, the feasibility of the proposed method for Pb(II) determination was assessed by the analysis of certi?ed reference material and various water samples and the satisfactory results were obtained.     

A UV-vis spectroscopic study of 1:2 adduct formation of some free-base meso-tetraaryl- and meso-tetraalkylporphyrins with PhSnCl3 and (CH3)2SnCl2

Molecular complexation of meso-tetraalkylporphyrins (with primary alkyl residues) (alkylpor), para-substituted meso-tetraphenylporphyrins (para=H, CH(3), Cl, OCH(3), NO(2)) (arylpor) and meso-teramesitylporphyrin (H(2)tmp) with PhSnCl(3) (A(I)) and (CH(3))(2)SnCl(2) (A(II)) led to the red shift of the Soret bands. Comparison of the Soret bands of A(I) (or A(II))(2)arylpor with those of (A(I) or A(II))(2)alkylpor shows a red shift of ca. 10-20nm for the formers with respect to the latters. According to the very similar saddled porphyrin core reported for the dications of H(2)tpp and H(2)t(n-Pr)p with CF(3)COOH, it may be concluded that in addition to the Q(0,0) bands the Soret bands may be also affected by the pi-donation of meso-aryl substituents to the porphyrin aromatic system. An overlap between one of the e(1g) orbital of phenyl groups and the a(1u) orbital of porphyrin core is suggested to explain the observed red shifts in the case of pi-donor para-substituents. Very similar red shift of the Soret bands of (A(I) or A(II))(2)H(2)t(4-OMe)pp and (A(I) or A(II))(2)H(2)t(4-NO(2))pp with respect to that of (A(I) or A(II))(2)H(2)t(n-Pr)p, in spite of the pi-electron withdrawing effects of para-NO(2) groups, seems to be resulted in by the pi-interaction of LUMOs of (4-NO(2))phenyl substituent with e(g) orbital of porphyrin core; this interaction would lead to the stabilization of e(g) orbital and the observed red shift of the Soret band. However, due to the distribution of electron densities of the a(2u) orbital on meso-positions, as well as the central nitrogens, the Q(0,0) bands are more strongly affected by the pi-donation of meso-aryl groups to the porphyrin core.     

Ultrasound- assisted emulsification microextraction for separation of trace amounts of antimony prior to FAAS determination

We describe a simple and rapid method for the ultrasound-assisted microextraction of antimony using the solidified floating organic drop method. The effects of pH, type and volume of the extractant, time of sonication, amount of chelating agent, type and amount of surfactant were investigated and optimized. Bromopyrogollol red is acting as the chelating agent. Antimony(III) ion was extracted into finely dispersed droplets of undecanol after ion-pair formation with the water soluble chelator and the cationic detergent benzyldimethyltetradecylammonium chloride. Flame atomic absorption spectrometry was used for the detection. The resulting calibration is linear in the concentration range from 4.0 to 900?ng?mL^-1 of Sb(III) with a correlation coefficient of 0.9981. The enrichment factor is 67, the detection limit is 0.62?ng?mL^-1, and the relative standard deviation is?±?3.6% (at 100?ng?mL^-1; for n?=?10). The method was successfully applied to the determination of antimony in water samples.

Preconcentration procedure trace amounts of palladium using modified multiwalled carbon nanotubes sorbent prior to flame atomic absorption spectrometry: 1st Nano Update

A method for preconcentration of palladium at trace level on modified multiwalled carbon nanotubes columns and determination by flame atomic absorption spectrometry (FAAS) has been developed. Multiwalled carbon nanotubes (MWCNTs) were oxidized with concentrated HNO₃ and the oxidized multiwalled carbon nanotubes were modified with 5-(4′-dimethylamino benzyliden)-rhodanine, and then were used as a solid sorbent for preconcentration of Pd(II) ions. Factors influencing sorption and desorption of Pd(II) ions were investigated. The sorption of Pd(II) ions was quantitative in the pH range of 1.0–4.5, whereas quantitative desorption occurs with 3.0 mL 0.4 mol L^?1 thiourea. The amount of eluted palladium was measured using flame atomic absorption spectrometry. The effects of experimental parameters, including sample flow rate, eluent flow rate, and eluent concentration were investigated. The effect of coexisting ions showed no interference from most ions tested. The proposed method permitted a large enrichment factor (about 200). The relative standard deviation of the method was ±2.73% (for eight replicate determination of 2.0 μg mL^?1 of Pd(II)) and the limit of detection was 0.3 ng mL^?1. The method was applied to the determination of Pd(II) in water, road dust, and standard samples.     

Application of organo-nanoclay as a solid sorbent for rhodium complex separation and preconcentration

An organo-nanoclay is used as a new, easily accessible, and stable solid sorbent for the preconcentration of trace amounts of rhodium ions from aqueous solution, this followed by its determination by flame atomic absorption spectrometry (FAAS). Rh(III) ion was first complexed with 2,3,5,6-tetra(2-pyridyl) pyrazine (TPPZ) at pH values between 3.0 and 4.7, and then the complex was then adsorbed onto the nanoclay. The rhodium ions were eluted from the sorbent with HCl. The rhodium in the effluent was determined by FAAS. The linear analytical range is between 0.14 ng mL^?1 and 20.0 μg mL^?1 in the initial solution, the relative standard deviation at 2.0 μg mL^?1 of rhodium is 2.6% (n?=?8), the detection limit is 0.03 ng mL^?1, and the preconcentration factor is 140. Experimental parameters including the pH, eluent type, interference by other ions and breakthrough volume were optimized. The method was applied to the determination of rhodium in water, road dust and synthetic samples.