Determination of trace amounts of cadmium and copper by atomic absorption spectrometry after simultaneous extraction and preconcentration using a new water-soluble polyacrylic acid/alumina sorbent

An analytical method using alumina modified with water-soluble polyacrylic acid polymer for the simultaneous separation and preconcentration of trace Cu and Cd in a column system, and their determination by flame atomic absorption spectrometry was developed. The conditions for coating Al₂O₃ with polyacrylic acid were optimized, then the column was packed with 50 mg of this sorbent. Cd and Cu solution was passed through a glass column at pH 4.5, and elution was carried out with 5 mL of 0.05 M HCl at a flow rate of 1 mL min⁻¹. A sorption capacity of 10 mg Cu and 12 mg Cd was obtained for 1 g sorbent. The detection limit was calculated as 4.5 μg L⁻¹ for Cu and 1.54 μg L⁻¹ for Cd in the final solution. Enrichment factors of 300 for Cd and 400 for Cu were obtained.     

Ionic Liquids Modify the Performance of Carbon Based Potentiometric Sensors

A new type of potentiometric sensor based on a recently constructed carbon ionic liquid electrode (CILE) is described. Two kinds of ionic liquids, i.e., N‐octylpyridinium hexafluorophosphate (OPFP) and 1‐butyl‐3‐methylimidazoluim hexafluorophosphate (BMFP) were tested as binder for construction of the carbon composite electrode. The characteristics of these electrodes as potentiometric sensors were evaluated and compared with those of the traditional carbon paste electrode (CPE). The results indicate that potentiometric sensors constructed with ionic liquid show an increase in performance in terms of Nernstian slope, selectivity, response time, and response stability compared to CPE.     

A study on the intermolecular hydrogen bonds of alpha-glycylglycine in its actual crystalline phase using ab initio calculated 14N and 2H nuclear quadrupole coupling constants

alpha-Glycylglycine in its actual crystalline phase is studied by ab initio calculated nuclear quadrupole coupling constants. These physical quantities are computed for 2H and 14N in the hydrogen bonds. The type of hydrogen bond is the N-H...O type. The computations are performed with the RHF and B3LYP methods and 6-31++G** and 6-311++G** basis sets using the Gaussian 98 program. Values of the calculated nuclear quadrupole coupling constants are shown in Tables 1-3. The aim of this work is the study of 2H and 14N quadrupole coupling constants which contribute in the CON2H...O=CN2H type of hydrogen bond. The computed nuclear quadrupole coupling constants of 2H nuclei meet the related experimental values. In addition, the computed chi value of 14N belonging to the -CO-14NH- group agrees well with values obtained experimentally. However, there are some discrepancies between calculated 14N chi values of the N+H3 residue and experiments. Also, the values of these physical parameters are calculated for >C2H2 of alpha-glycylglycine in its crystalline phase. Calculations for these parameters are carried out in a single molecule using X-ray diffraction coordinates, too.     

Preparation and characterization of Cu (II) supported on poly(8‐hydroxyquinoline‐p‐styrene sulphonate) and its application as catalyst for the synthesis of hexahydroquinolines

Cu ( II ) supported on poly(8‐hydroxyquinoline‐p‐styrenesulfonate) (Cu ( II )@PHQSS) was prepared and fully characterized by the different techniques including fourier transform infrared spectroscopy (FT‐IR), ¹H NMR, ¹³C NMR, thermal gravimetric analysis (TGA), differential thermal gravimetric (DTG), differential thermal analysis (DTA), scanning electron microscope (SEM) and energy dispersive X‐ray analysis (EDS). Afterward, the Cu ( II )@PHQSS as nanostructured catalyst was used as catalyst for the synthesis of hexahydroquinolines.     

Highly effective and regioselective Michael addition of indoles to α,β-unsaturated ketones promoted by pentafluorophenylammonium triflate

A simple, inexpensive, environmentally friendly and efficient route for Michael addition of indoles to α,β-unsaturated ketones using pentafluorophenylammonium triflate (PFPAT) as a catalyst is described. Various indole derivatives were synthesized in good to excellent yields. The preparation of PFPAT catalyst from simple and readily available starting materials makes this method more affordable.     

Low Temperature Preparation of 3D Solid and Hollow ZnS Nanosphere Self-Assembled from Nanoparticles by Varying Sulfur Source

In this work, we report a facile hydrothermal method for the preparation of three dimensional hollow ZnS nanostructures, using Zinc bis(salicyle aldehitato), Zn(Sal)₂, thioacetamide (TAA) and thioglycolic acid (TGA) as Zn²⁺, sulfur source and capping agent, respectively. The ZnS solid and hollow sphere was produced from the self-assembly of nanoparticles with diameters of 11 ± 2 nm with TGA and TGA, TAA, respectively. Furthermore, with changing zinc precursor from Zn(Sal)₂ to zinc acetate [Zn(OAC)₂], ZnS nanorods were obtained. The products were characterized by XRD, SEM, TEM, selected area electron diffraction, and FT-IR spectra. The influence of surfactant (Polyethylene glycol) on the morphology of the products was also investigated. Possible formation mechanism and optical properties of these architectures were also reported.     

Solvothermal Synthesis and Characterization of PbSe Nanostructures with the Aid of Schiff-base Ligand

In this work, Pb(II)N,N-bis(salicylidene)-ethylenediamine; [Pb(salen)]; was applied as lead precursor to synthesis PbSe nanostructures. Besides [Pb(salen)], SeCl₄ and reducing agents like N₂H₄·H₂O have been employed for the production of PbSe nanostructures via a solvothermal route at 180 °C for 3 h in propylene glycol. The effect of preparation factors such as temperature, reaction time, and surfactant on the morphology of PbSe nanostructures was investigated. The experimental results indicated that PbSe synthesized at 150 and 210 °C was composed of agglomerated particles. On the other hand, the use of KBH₄ as reducing agent led to produce PbSe with higher particle size and agglomeration. The as-prepared PbSe nanostructures were characterized by XRD, SEM, TEM, EDS, and FT-IR.     

Preparation and characterization of nano-Co-[4-chlorophenyl-salicylaldimine-methyl pyranopyrazole]Cl2 as a new Schiff base complex and catalyst for the solvent-free synthesis of 1-amidoalkyl-2-naphthols

By the reaction of 4-chlorobenzaldehyde with ethyl acetoacetate, malononitrile, and hydrazine hydrate, 6-amino-4-(4-chlorophenyl)-3-methyl-2,4-dihydropyrano[2,3-c]pyrazole-5-carbonitrile was prepared and then reacted with salicylaldehyde and CoCl₂·6H₂O to produce nano-Co-[4-cholorophenyl-salicylaldimine-methylpyranopyrazole]Cl₂ (nano-[Co-4CSMP]Cl₂). The prepared nano-Schiff base complex was reported for the first time and fully characterized by Fourier transform-infrared spectroscopy, thermal gravimetric analysis, differential thermal gravimetric analysis, scanning electron microscopy, energy-dispersive X-ray spectroscopy, transmission electron microscopy, and Brunner–Emmett–Teller analyses and applied as an efficient catalyst for the synthesis of some 1-amidoalkyl-2-naphthol derivatives.