Two nickel(II) complexes of [1 + 1] macrocyclic Schiff base ligand (L) have been prepared by cyclocondensation reactions between 1,3-diamino-2-propanol and 2-[3-(2-formylphenoxy)-2-hydroxypropoxy] benzaldehyde, using NiX2 (X = Br, and I) salts as template agents, and characterized by elemental analyses, IR, molar conductivity and electronic spectra in both solid and solution states. The single-crystal X-ray diffractions of the complexes are also reported that contain nickel(II) ion in a distorted octahedral geometry coordination of N2O3X (X = Br, I and NO3). In all complexes the ligand behaves as a pentadentate ligand. Cyclic voltammetric studies of nickel(II) complexes indicate a quasi-reversible redox wave in the negative potential range. 相似文献
Molecular interactions of five thiazine dyes with increasing alkyl substitution have been studied in aqueous and microemulsion media at 303 K within a concentration range of (1.35–7.00) × 10?4 M. The dimerization constant (Kd) values for the five dyes are ranged between 1.761 and 6.258 × 103 l mol?1 in bulk water media, where as in microemulsion media, Kd's are ranged between 1.760 and 4.110 × 103 l mol?1. Thionine (with no methyl substitution) and azure A (with two methyl substitution) displayed slightly larger Kd values in microemulsion water pools compared to bulk water while other dyes recorded significant drop in Kd values. The influence of microemulsion media on the molecular interaction of dyes has been explained in terms of electrostatic and hydrophobic factors. The monomer and the dimer spectra are explained in terms of molecular exciton model and the optical absorption parameters of both the species are reported in bulk and confined media. 相似文献
We report the energy and power voltage-dependencies of supercapacitors using single-walled carbon nanotube electrodes. The energy density was dependent on the cell-voltage cubed (up to 4 V: E = 1.43 × V3). The cubic relationship was attributed to the linear increase of the capacitance as a function of voltage, enabled by electrochemical doping. Furthermore, while up to 3.5 V, the maximum power rating of the nanotube electrodes increased as a function of the cell-voltage squared, beyond 3.5 V, a decline in power was observed as a result of depletion of the electrolyte's ions. 相似文献
Changes in the thermal conductivities of paraffin and mono ethylene glycol (MEG) as a function of β-SiC nanoparticle concentration
and size was studied. An enhancement in the effective thermal conductivity was found for both fluids (i.e., both paraffin
and MEG) upon the addition of nanoparticles. Although an enhancement in thermal conductivity was found, the degree of enhancement
depended on the nanoparticle concentration in a complex way. An increase in particle-to-particle interactions is thought to
be the cause of the enhancement. However, the enhancement became muted at higher particle concentrations compared to lower
ones. This phenomenon can be related to nanoparticles interactions. An improvement in the thermal conductivities for both
fluids was also found as the nanoparticle size shrank. It is believed that the larger Brownian motion for smaller particles
causes more particle-to-particle interactions, which, in turn, improves the thermal conductivity. The role that the base-fluid
plays in the enhancement is complex. Lower fluid viscosities are believed to contribute to greater enhancement, but a second
effect, the interaction of the fluid with the nanoparticle surface, can be even more important. Nanoparticle-liquid suspensions
generate a shell of organized liquid molecules on the particle surface. These organized molecules more efficiently transmit
energy, via phonons, to the bulk of the fluid. The efficient energy transmission results in enhanced thermal conductivity.
The experimentally measured thermal conductivities of the suspensions were compared to a variety of models. None of the models
proved to adequately predict the thermal conductivities of the nanoparticle suspensions. 相似文献
A carbon past electrode modified with [Mn(H2O)(N3)(NO3)(pyterpy)],
( \textpyterpy = 4¢- ( 4 - \textpyridyl ) - 2,2¢:\text6¢,\text2¢¢- \textterpyridine ) \left( {{\text{pyterpy}} = 4\prime - \left( {4 - {\text{pyridyl}}} \right) - 2,2\prime:{\text{6}}\prime,{\text{2}}\prime\prime - {\text{terpyridine}}} \right) complex have been applied to the electrocatalytic oxidation of nitrite which reduced the overpotential by about 120 mV with
obviously increasing the current response. Relative standard deviations for nitrite determination was less than 2.0%, and
nitrite can be determined in the ranges of 5.00 × 10−6 to 1.55 × 10−2 mol L−1, with a detection limit of 8 × 10−7 mol L−1. The treatment of the voltammetric data showed that it is a pure diffusion-controlled reaction, which involves one electron
in the rate-determining step. The rate constant k′, transfer coefficient α for the catalytic reaction, and diffusion coefficient of nitrite in the solution, D, were found to be 1.4 × 10−2, 0.56× 10−6, and 7.99 × 10−6 cm2 s−1, respectively. The mechanism for the interaction of nitrite with the Mn(II) complex modified carbon past electrode is proposed.
This work provides a simple and easy approach to detection of nitrite ion. The modified electrode indicated reproducible behavior,
anti-fouling properties, and stability during electrochemical experiments, making it particularly suitable for the analytical
purposes. 相似文献
In this work, we propose chlorpromazine as a new mediator for the rapid, sensitive, and highly selective voltammetric determination of glutathione (GSH) using multiwall carbon nanotubes paste electrode (MWCNTPE). The experimental results showed that the carbon nanotubes paste electrode has a highly electrocatalytic activity for the oxidation of GSH in the presence of chlorpromazine as a mediator. Cyclic voltammetry, double potential step chronoamperometry, and differential pulse voltammetry (DPV) are used to investigate the suitability of chlorpromazine at the surface of MWCNTPE as a mediator for the electrocatalytic oxidation of GSH in aqueous solutions. It is shown that chlorpromazine can catalyze the oxidation of GSH in an aqueous buffer solution to produce a sharp oxidation peak current at about +0.70 versus Ag/AgCl as a reference electrode. Kinetic parameters such as electron transfer coefficient and catalytic reaction rate constant, k/h, are also determined. Using DPV and under the optimum conditions at pH 4.0, the electrocatalytic oxidation peak current of GSH shows a linear dependence on GSH concentration in the GSH concentration range of 0.3 to 18.3 µM. The detection limit (3σ) is determined to be 0.16 µM. The relative standard deviation for 1.5 and 5.0 µM GSH are found to be 3.7% and 2.5%, respectively. The proposed method may, thus, also be used as a novel, selective, simple, and precise method for the voltammetric determination of GSH in such real samples as hemolyzed erythrocyte. 相似文献
In this study, an oxadiazole multi-wall carbon nanotube-modified glassy carbon electrode (OMWCNT−GCE) was used as a highly sensitive electrochemical sensor for hydrazine determination. The surface charge transfer rate constant, ks, and the charge transfer coefficient, α, for electron transfer between GCE and electrodeposited oxadiazole were calculated as 19.4 ± 0.5 s−1 and 0.51, respectively at pH = 7.0. The obtained results indicate that hydrazine peak potential at OMWCNT−GCE shifted for 14, 109, and 136 mV to negative values as compared with oxadiazole-modified GCE, MWCNT−GCE, and activated GCE surface, respectively. The electron transfer coefficient, α, and the heterogeneous rate constant, k′, for the oxidation of hydrazine at OMWCNT−GCE were also determined by cyclic voltammetry measurements. Two linear dynamic ranges of 0.6 to 10.0 μM and 10.0 to 400.0 μM and detection limit of 0.17 μM for hydrazine determination were evaluated using differential pulse voltammetry. In addition, OMWCNT−GCE was shown to be successfully applied to determine hydrazine in various water samples.
A triterpenoid saponin, guaianin O (1), oleanolic acid 3-O-{α-L-rhamnopyranosyl-(1 → 2)-[β-D-glucopyranosyl-(1 → 3)]-α-L-arabinopyranoside}-28- O-[β-D-glucopyranosyl]-ester, was isolated from the n-butanol extract of flowers of Guaiacum officinale L. The structural elucidation of 1 was accomplished by extensive studies of both one and two dimensional 1H, 13C-NMR spectra, the FAB mass spectrum, and alkaline and acid hydrolyses. 相似文献
A simple, rapid and efficient sample preparation technique, dispersive liquid-liquid microextraction, coupled with gas chromatography-flame ionization detection has been developed to determine N-methylpyrrolidine in cefepime. The effect of various experimental factors on the preparation procedure, such as the nature and volume of extraction and disperser solvents, extraction time, the nature of buffer and its pH, and salt effect, was investigated, optimized and the following results were obtained: extraction solvent, chloroform; dispersive solvent and solvent for dissolving cefepime, a mixture of methanol/water (88:12, v/v); salting out agent, NaCl; and buffer, carbonate/bicarbonate (C=0.5?M, pH=12). The optimized conditions were applied to the real sample (cefepime) for the extraction and determination of N-methylpyrrolidine. The calibration graph is linear from 0.02 to 850?mg/L with the square of correlation coefficient 0.999. LOD and LOQ are 6.4 and 21.2?μg/L in solution, respectively, and 0.2 (2×10(-5) ) and 0.6 (6×10(-5) ) μg/g (%, w/w) in cefepime powder, respectively, using sample size 50?mg. Repeatability of the method is good and RSD% for six repeated experiments (C=170?mg/L) is 6.35%. 相似文献
This study investigated the use of ultrasound‐assisted extraction to improve the extraction efficiency of morphine, codeine and thebaine from the papaver plants. Extraction conditions such as type of solvent, temperature, duration, frequency and power level of ultrasonic were optimized and the influences of different parameters on resolution of alkaloids in CE were studied. The optimized condition for CE separation includes a sodium phosphate buffer (100 mM, pH 3.0) containing 5 mM α‐CD. The optimized extraction conditions for ultrasound‐assisted extraction was an extraction time of 1 h, an ultrasonic frequency of 60 kHz with water–methanol (80:20) at 40°C as the extraction solvent. The LOD for alkaloids was found to be 0.1 μg/mL at a signal‐to‐noise ratio of 3:1. The RSDs for peak areas were in the range of 1.4–4.4%. The amounts of opium alkaloids (mg/100 g dried sample) in four Iranian papaver plants were found to be in the range of 7.8–8.7 (morphine), 5.5–9.5 (codeine) and 1.4–10.4 (thebaine). It should be emphasized that no cleanup of the filtered extract was required; hence, direct determination after extraction drastically simplifies the analytical process. 相似文献