A convergent paired electrochemical synthesis of new heterocyclic compounds. Reaction of benzoquinones with 3-Amino-4-hydroxycoumarin

Electrochemical oxidation of catechols (1) has been studied in the presence of cathodically generated 3-amino-4-hydroxycoumarin (3a) as a nucleophile in aqueous solutions, using cyclic voltammetry and controlled-potential coulometry. The results indicate that the o-benzoquinones derived from catechols (1) participate in Michael addition reaction with 3-amino-4-hydroxycoumarin (3a) to form the corresponding new heterocyclic compounds (7) (oxidized form of coumestan derivatives). The electrochemical process consists of a multi-step including (a) cathodic reduction of 4-hydroxy-3-nitrocoumarin (3) to 3-amino-4-hydroxycoumarin (3a), (b) anodic oxidation of catechols (1) to related o-benzoquinone (2), (c) the Michael addition reaction of 3-amino-4-hydroxycoumarin (3a) to o-benzoquinone (2), and (d) anodic oxidation of formed adduct. The paired electrochemical synthesis of compounds 7a and 7b has been successfully performed in a one-pot process at carbon rods as working and counter electrodes in an undivided cell.     

Observation of transverse Anderson localization in an optical fiber

We utilize transverse Anderson localization as the waveguiding mechanism in optical fibers with random transverse refractive index profiles. Using experiments and numerical simulations, we show that the transverse localization results in an effective propagating beam diameter that is comparable to that of a typical index-guiding optical fiber.     

Effects of Some Parameters on Particle Size Distribution of Chitosan Nanoparticles Prepared by Ionic Gelation Method

In this research, chitosan nanoparticles were prepared based on the ionic gelation of chitosan with tripolyphosphate anions. Effects of parameters such as chitosan concentration, tripolyphosphate concentration, and reaction time on the particle size distribution were investigated. In order to determine optimum conditions, tests were designed by Qualitek-4 software, using Taguchi method. The best conditions were determined based on three factors at three levels. Therefore, the main object was to investigate the effect of some parameters on particle size distribution and determine the optimum conditions for preparing chitosan nanoparticles by ionic gelation, followed by evaluation of the physicochemical and structural properties. The size distribution of original chitosan and chitosan nanoparticles were determined by Laser Diffraction and Dynamic Light Scattering, respectively. The physicochemical properties of the chitosan nanoparticles were studied using SEM, TEM, XRD pattern, FTIR, UV–vis, TGA, and NMR spectra. The optimum chitosan concentration, tripolyphosphate concentration, and reaction time were found to be 1.0 mg/ml, 1.0 mg/ml, and 60 min, respectively.     

Single granular activated carbon microextraction and graphite furnace atomic absorption spectrometry determination for trace amount of gold in aqueous and geological samples

A new and simple method was developed for preconcentration trace amount of gold in aqueous and mineral samples. The method was based on the sorption of gold on granular activated carbon (AC) in acidic medium (hydrochloric acid) and subsequently direct determination by graphite furnace atomic absorption spectrometry (GFAAS). A small particle of adsorbent was delivered to small volume of sample. After extraction, AC removed and analyzed directly by GFAAS. Several factors influencing the extraction efficiency, such as the hydrochloric acid concentration, sample volume and extraction time were studied as well as effect of potential interfering ions. The preconcentration factor 50 was obtained. The limit of detection (LOD) of gold in water and soil samples was 0.007 μg L^− 1 and 0.9 ng g^− 1, respectively. The proposed method was applied successfully to the determination of trace amount of gold in environmental and geological samples. In order to validate the developed method, two certified reference materials: Platinum Ore (SARM-7B) and Copper Ore Mill Heads (No. 330) were analyzed and the determined values obtained were in good agreement with the certified values and recovery was obtained in the range of 80-118%. The relative standard deviations (RSD) for the spiking levels of 0.5 μg L^− 1 in the real samples was 4%, (n = 15).     

On-line preconcentration system for lead(II) determination in waste water by atomic absorption spectrometry using active carbon loaded with Pyrogallol Red.

An on-line system for enrichment and determination of lead(II) is presented. It is based on the adsorption of lead(II) ions on a minicolumn packed with active carbon loaded with Pyrogallol Red. After preconcentration step, the metal ions are eluted automatically by 5.0 ml of 0.50 M nitric acid solution and the lead ion contents were determined by atomic absorption spectrometry. The influence of chemicals, pH and flow variables were studied as well as effect of potential interfering ions. Under the optimum conditions, the lead ions in aqueous samples were concentrated about 100 fold by the column. The detection limit was 0.001 microg ml(-1). The recovery percent of spliced lead(II) was in the range of 98%-103%.     

Fabrication and characterization of chitosan-gelatin/single-walled carbon nanotubes electrospun composite scaffolds for cartilage tissue engineering applications

Cartilage is a connective tissue with a slow healing rate due to lack in blood circulation and slow metabolism. Designing tissue engineering scaffolds modified based on its specific features can assist its natural regeneration process. In this study, the chitosan-gelatin/single-walled carbon nanotubes functionalized by COOH (SWNTs-COOH) nanocomposite scaffolds were fabricated through electrospinning. The effect of each component and different duration of cross-linking were assessed in terms of morphology, porosity, chemical structure, thermal behavior, mechanical properties, wettability, biodegradability, and in vitro cell culture study. Adding SWNTs-COOH decreased fiber diameter, water contact angle and degradation rate while increased tensile strength, hydrophilicity, stability and cell viability, due to their high intrinsic electrical conductivity, and mechanical properties and the presence of COOH functional groups in its structure. All the sample presented a porosity percentage of more than 80%, which is essential for tissue engineering scaffolds. The presence SWNTs-COOH did not have any adverse effect on cytocompatibility. The optimal cross-linking time increased the stability of the scaffolds in PBS. It can be concluded that the chitosan-gelatin/1wt% SWNTs-COOH scaffold can be appropriate for cartilage tissue engineering applications.     

Solid-Phase Extraction of Copper with Cupron on Octadecyl Silica Cartridge and its Determination with Atomic Absorption Spectrometry

Solid-phase extraction of trace amounts of copper from large volumes of aqueous solutions was studied. The extraction was carried out by means of an octadecyl silica cartridge modified with cupron. The effect of different parameters such as sample matrix, flowrates of sample solution and eluent, pH, breakthrough volume, and potentially interfering ions was examined. Cu²⁺ was extracted from solution in the pH range of 6–8.5 on a modified cartridge. Elution was accomplished using 2mL of 0.2M HNO₃. Hence, with a typical preconcentration factor of 1000, a detection limit of 0.02ngmL^–1 was obtained. The method was applied to the determination of copper in natural water samples.