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1.
Trimethylsulfonium triiodide (I) and p-xylylene-bis-(tetrahydrothiophenium) triiodide (II) were identified and determined by capillary electrophoresis with the resolution R s = 4.86 using an unmodified quartz capillary. The procedure ensures the determination of sulfur-containing organic compounds in a concentration range of 1.0 × 10?5–5.0 × 10?4 M RSD ≤ 5%). The high stability of trimethylsulfonium triiodide and p-xylylene-bis-(tetrahydrothiophenium) triiodide in chloroform and acetonitrile solutions was found by spectrophotometry. A procedure was proposed for the spectrophotometric determination of compounds I and II as ion associates of sulfur-containing cations with a sulfophthalein dye, Bromocresol Purple (c min (I) = 1.32 × 10?5 M, c min (II) = 7.1 × 10?6 M, RSD = 5%), and by the characteristic absorption of the triiodide anion in acetonitrile (c min (I) = 3.18 × 10?6 M, c min (II) = 2.76 × 10?6 M, RSD <-3%).  相似文献   

2.
The equilibria and kinetics of the reaction of Pd(gly)2 complexes with hydrogen ions and chloride ions has been studied by a potentiometric method. The underlying idea of the method is the measurement of solution pH as a function of reaction time t using a glass electrode. The solutions used had the following initial compositions: xM Pd(gly)2, xM Hgly, and 1 M NaCl with x = 1 × 10?4, 5 × 10?4, and 1 × 10?3; initial pH0 was from ~3.5 to ~4.4. The experimentally determined pH versus t dependences and the rate equation for a pseudo-second-order reaction were used to determine the equilibrium constant of formation of Pd(gly)(Hgly)Cl complexes from Pd(gly)2 complexes and the observed rate constant for this reaction, k obs. The dependence of k obs on the pH of the acid solutions studied was assigned to a change in the sequence of the reactions of addition of a hydrogen ion and a chloride ion to the complex Pd(gly)2.  相似文献   

3.
A mixed oxide-covered mesh electrode composed of NiCo2O4 (MOME-NiCo2O4) was prepared on a stainless-steel substrate using thermal decomposition (slow-cooling rate method). Surface, bulk and electrochemical properties of MOME were studied using different techniques, namely scanning electron microscopy (SEM), X-ray diffraction (XRD), cyclic voltammetry (CV) with determination of the electrochemical porosity (?) and morphology factor (φ) parameters, quasi-stationary polarisation curves (PC) and electrochemical impedance spectroscopy (EIS). SEM images revealed a good coverage of the metallic wires by a compact oxide layer (absence of cracks). XRD analysis confirmed the formation of the spinel NiCo2O4 with the presence of NiO. The ‘in situ’ surface parameters denoted as ? and φ exhibited values of 0.39 and 0.33, respectively, revealing that the electrochemically active surface area is mainly confined to the ‘outer/external’ surface regions of the oxide layer. The PC was characterised by two Tafel slopes distributed in the low (b 1 = 46 mV dec?1) and high (b 2 = 59 mV dec?1) overpotential domains. The corresponding apparent exchange current densities were j 0(1) = (3.43 ± 0.11) × 10?6 A cm?2 and j 0(2) = (6.70 ± 0.08) × 10?6 A cm?2, respectively. The EIS study accomplished in the low-overpotential domain revealed a Tafel slope (b 1) of 51 mV dec?1. According to the spin-trapping reaction using N,N-dimethyl-p-nitrosoaniline (RNO), the MOME-NiCo2O4 electrode exhibited good performance for the generation of weakly adsorbed hydroxyl radicals (HO?) during the OER in electrolyte-free water.  相似文献   

4.
By using dc and ac polarography, the kinetics of electroreduction of the palladium (II) complexes with β-alanine at a dropping mercury electrode was studied in solutions with the palladium (II) concentration from 2 × 10?5 to 2 × 10?4 M and variable β-alanine and sodium perchlorate concentrations (pH 6–12). One polarographic wave was observed in solutions with pH 9 and 10 at the β-alanine overall concentration of c βala = 1 × 10?3 to 5 × 10?2 M; two waves, at lower pH or higher c βala. It was concluded on the formation of different forms of palladium (II) complexes in the studied solutions; the complexes contained two to four β-alanine coordinated anions. Using the limiting diffusion currents for the two waves at pH 9–11 and c βala = 0.1 and 0.5 M, the stepwise stability constant for the Pd(βala) 4 2? complex was calculated. Using two ac peaks observed at pH 7–8 and c βala = 1 × 10?2 to 0.1 M, the stepwise stability constant for the Pd(βala) 3 ? . was calculated. The perchlorate ions adsorbed at the dropping mercury electrode, as well as βala? anions at their higher concentrations, hamper the electroreduction of the palladium (II) complexes with β-alanine.  相似文献   

5.
A sensitive and selective method for determination of mercury(II) with “4-(4-methylphenyl aminoisonitrosoacetyl)biphenyl (TKO)-modified pencil graphite electrode” was developed. All factors affecting determination process were optimized. Differential pulse voltammetry with 4-(4-methylphenyl aminoisonitrosoacetyl)biphenyl-modified electrode showed a linear response between 1.0 × 10?5 and 1.0 × 10?3 M (R 2 = 0.9994). The detection limit of this electrode was found as 5.85 × 10?7 M (S/N = 3). The effects of different cations on the determination of mercury(II) were investigated and found that modified electrode is highly selective. The developed method was applied for mercury determination in different water samples.  相似文献   

6.
Properties of CF x /Li and CF x /Na cells were examined while using galvanostatic charging/discharging, electrochemical impedance spectroscopy and scanning electron microscopy (SEM). The capacity during the first cycle was as high as ca. 1000 mAh g?1. Such an electrode is suitable for primary CF x /Li and CF x /Na batteries. SEM images of CF x cathode showed that during discharging it was transformed into amorphous carbon and LiF or NaF crystals (of diameter of ca. 5–20 μm). These systems (C?+?LiF or C?+?NaF) cannot be reversibly converted back into CF x /Li or CF x /Na, respectively. Exchange current densities are between 10?7 Acm?2 and 10?9 Acm?2 when working with LiPF6 and NaPF6 electrolytes (1.12?×?10?7 Acm?2 and 6.82?×?10?9 Acm?2, respectively). Those values are low and indicate that the charge transfer process may be the rate-determining step. Activation energies for the charge transfer process were 57 and 72 kJ mol?1 for CF x /LiPF6 and CF x /NaPF6 systems, respectively. Higher activation energy barrier for the CF/Na+?+?e??→?C?+?NaF reaction results in lower observed exchange current density in comparison to the system with lithium ions.  相似文献   

7.
LaSr3Fe3O10 ? δ powders were synthesized by hydrothermal method and characterized by XRD and SEM. The XRD patterns showed that the sample calcined at 1000 °C was single phase and the sample calcined at 900 °C had tiny amount of LaSrFeO4 phase. The single-phase LaSr3Fe3O10 ? δ powders were used to prepare test electrode. The capacitive behaviors of LaSr3Fe3O10 ? δ electrode were analyzed by cyclic voltammetry, galvanostatic charge-discharge techniques, and electrochemical impedance spectroscopy. The electrochemical results showed a capacity as high as 470 F g?1 at a scan rate of 1 mV s?1 and 380 F g?1 at a charge-discharge current density of 0.1 A g?1 in 6 M KOH solution. The electrode showed good cyclic stability since its capacitive retention is 87.1% after 1000 charge-discharge cycles. The electrochemical performances suggest that LaSr3Fe3O10 ? δ could be a potential candidate as a capacitive electrode material.  相似文献   

8.
An investigation is conducted on enhancing lithium-ion intercalation and conduction performance of transparent organo tantalum oxide (TaO y C z ) films, by addition of lithium via a fast co-synthesis onto 40 Ω/□ flexible polyethylene terephthalate/indium tin oxide substrates at the short exposed durations of 33–34 s, using an atmospheric pressure plasma jet (APPJ) at various mixed concentrations of tantalum ethoxide [Ta(OC2H5)5] and lithium tert-butoxide [(CH3)3COLi] precursors. Transparent organo-lithiated tantalum oxide (Li x TaO y C z ) films expose noteworthy Li+ ion intercalation and conduction performance for 200 cycles of reversible Li+ ion intercalation and deintercalation in a 1 M LiClO4-propylene carbonate electrolyte, by switching measurements with a potential sweep from ?1.25 to 1.25 V at a scan rate of 50 mV/s and a potential step at ?1.25 and 1.25 V, even after being bent 360° around a 2.5-cm diameter rod for 1000 cycles. The Li+ ionic diffusion coefficient and conductivity of 6.2?×?10?10 cm2/s and 6.0?×?10?11 S/cm for TaO y C z films are greatly progressed of up to 9.6?×?10?10 cm2/s and 7.8?×?10?9 S/cm for Li x TaO y C z films by co-synthesis with an APPJ.  相似文献   

9.
The kinetics of gas reaction \(HOCl\underset{{k_r }}{\overset{{k_f }}{\longleftrightarrow}}H(^2 S) + OCl(X^2 \Pi _i )\) was analyzed by the MP4 method. In the temperature range of 100–373 K the rate constants k f and k r and equilibrium constant K were changed from 1.10 × 10?220 to 1.17 × 10?52 s?1, from 2.89 × 10?16 to 1.68 × 10?5s?1 and from 3.80 × 10?205 to 6.96 × 10?48 respectively. In the above temperature range, the activation energy of the forward reaction (E f) is 105.05 kcal/mol. In the same temperature interval there are two kinetic domains for the reverse reaction with activation energies (E r1 = 5.53 kcal/mol when T is 100–273 K and E r2 = 14.50 kcal/mol when T is 273–373 K, respectively.  相似文献   

10.
A novel enzyme-free electrochemical sensor for H2O2 was fabricated by modifying an indium tin oxide (ITO) support with (3-aminopropyl) trimethoxysilane to yield an interface for the assembly of colloidal gold. Gold nanoparticles (AuNPs) were then immobilized on the substrate via self-assembly. Atomic force microscopy showed the presence of a monolayer of well-dispersed AuNPs with an average size of ~4 nm. The electrochemical behavior of the resultant AuNP/ITO-modified electrode and its response to hydrogen peroxide were studied by cyclic voltammetry. This non-enzymatic and mediator-free electrode exhibits a linear response in the range from 3.0?×?10?5 M to 1.0?×?10?3 M (M?=?mol?·?L?1) with a correlation coefficient of 0.999. The limit of detection is as low as 10 nM (for S/N?=?3). The sensor is stable, gives well reproducible results, and is deemed to represent a promising tool for electrochemical sensing.
Figure
AuNPs/ITO modified electrode prepared by self-assembly method exhibit good electrocatalytic activity towards enzyme-free detection H2O2. The linear range of typical electrode is between 3.0?×?10?5 M and 1.0?×?10?3 M with a correlation coefficient of 0.999 and the limit detection is down to 1.0?×?10?8 M.  相似文献   

11.
An enhanced oxime-based electrochemical sensor decorated with gold nanoparticles (AuNPs) and Co3O4 hexagonal nanosheets coupled with nitrogen-doped graphene has been developed for dimethoate determination dramatically. The introduction of Co3O4 hexagonal nanosheets tackles agglomeration of AuNPs and also enhances the sensitivity of electrochemical sensors greatly. The structure and properties of the synthesized composites were characterized by scanning electron microscopy, X-ray diffraction, Raman spectroscopy and Fourier transform infrared spectroscopy, confirming the successful modification of 2-(4-mercaptobutoxy)-1-naphthaldehyde oxime and Co3O4 supported AuNPs in a great experiment. In addition, differential pulse voltammetry further revealed that the developed electrochemical sensor exhibited excellent selectivity, sensitivity and stability in real samples analysis. Under optimal conditions, the modified sensor displayed a broad linear range from 1?×?10?14 M to 1?×?10?6 M with a fairly low detection limit of 8.4?×?10?14 M (S/N?=?3) and was expected to act as a superior method for dimethoate determination.  相似文献   

12.
In this work; we constructed a silver ion-selective electrode based on N-(6-aminohexyl) carboxamide functionalized single-walled carbon nanotubes (NAHAFSWCN) as an ionophore. The selectivity constant of a number of cations was measured using silver ion selective electrode. Optimal pH was between 3 and 6 and the upper and lower detection limits of the designed electrode were 1.2 × 10–2 and 8 × 10–7 M. The electrode showed a Nernstian response over a silver ion concentration range of 1 × 10–6 to 1 × 10–2 M with a slope of 59.1 ± 0.5 mV/decade. The response time of the electrode was less than 18 s and its effective lifetime was 3 months. The isothermal temperature coefficient of the electrode dE°/dT was determined as 0.00011 V/grad. Thermodynamic functions such as ΔS°, ΔH° and ΔG° were obtained by calculating the thermal coefficient of the electrode.  相似文献   

13.
A new electrochemical sensor was developed for determination of D-penicillamine using glassy carbon electrode which had been modified by gold nanoparticles–reduced graphene oxide nanocomposite (AuNPs/RGO/GCE) in aqueous solution. Cyclic voltammetry, transmission electron microscopy and electrochemical impedance spectroscopy were used for characterization of the modified electrode. The results indicated that the kinetic of oxidation reaction of D-penicillamine at the surface of the electrode was controlled by both diffusion and adsorption processes. In 0.1 mol L?1 phosphate buffer (pH 2.0), the oxidation current increased linearly with concentration of D-penicillamine with a linear range of 5.0 × 10?6 to 1.1 × 10?4 mol L?1 and regression coefficient of R 2 = 0.9972. Theoretical detection limit, defined based on 3σ of the blank signal (n = 9) divided by the slope of the linear regression equation, was 3.9 × 10?6 mol L?1 D-penicillamine using differential pulse voltammetry. The developed method was successfully applied to the determination of D-penicillamine in pharmaceutical formulation and blood serum samples.  相似文献   

14.
Deposited cobalt microparticales (Co-MPs) film onto the platinum disk electrode has been successfully used as a new amperometric sensor for the determination of ascorbic acid (AA). AA is detected by surface catalyzed oxidation involving cobalt(III) oxyhydroxides in alkaline solution. The Co-MPs/Pt electrode exhibits a high electrocatalytic activity toward the AA oxidation. The diffusion coefficient of AA (6.09 × 105 cm2/s) and the catalytic rate constant (k cat = 6.27 × 103 M–1s–1) have been determined using electrochemical approaches. The amperometric response of the modified electrode is linear against the AA concentration in the range (0.01?0.48 mM). The sensor displays the best activity with a high response signal, a good sensitivity of 74.3 μA/mM, a low detection limit of 2.5 μM (signal/noise = 3) and a fast response time (<3 s). Moreover, the reproducibility, selectivity and applicability of this biosensor are satisfactorily evaluated.  相似文献   

15.
In this work, we described an electrochemical sensor using a nanocomposite based on graphene oxide (GO), silver nanoparticles (AgNP), and disordered mesoporous silica (SiO2), which was used for the determination of bisphenol A in water samples. Initially, the hybrid material SiO2/GO was synthesized via sol-gel process, subsequently decorated with AgNP with an approximate 20 nm particle size prepared directly on the surface of the SiO2/GO using N, N-dimethylformamide (DMF) as an agent reducer. A glassy carbon electrode was modified with SiO2/GO/AgNP and used in developing a sensitive electrochemical sensor for the determination of bisphenol A in phosphate buffer 0.1 mol L?1 (pH 7.0). The detection limit was 45.2 nmol L?1 with a linear response range between 1.0 × 10?7 and 2.6 × 10?6 mol L?1 and a sensitivity of 1.27 × 10?7 A mol?1 L. Finally, the optimized electrochemical sensor was used for the quantitation of endocrine interfering in natural waters.  相似文献   

16.
The temperature dependences of birefringence Δn, anisotropy of permittivity ?a, and elastic constants K 11 and K 33 in the nematic phase of a tetrapalladium organyl-pentadecane system with a pentadecane content of 55 wt % have been investigated experimentally. It has been shown that, as temperature is elevated, ?a, K 11, and K 33 values decrease and Δn remains unchanged. Elastic constants K 11 and K 33 have been established to vary from 3.4 × 10?7 to 5.6 × 10?6 dyn and from 1.3 × 10?6 to 27.4 × 10?5 dyn, respectively. The value of ?a has been revealed to vary over the range 0.2–0.5. It has been found that, at temperatures above the N2 → Cr phase transition by 6°C, an imposed electric field induces the growth of tetrapalladium organyl crystals.  相似文献   

17.
The electrocatalytic mechanism of Cr(III) reduction in the presence of diethylenetriaminepentaacetic acid (DTPA) and nitrate ions is studied theoretically and experimentally by using stripping square-wave voltammetry (SWV). Experimental curves are in excellent agreement with theoretical profiles corresponding to a catalytic reaction of second kind. This type of mechanism is equivalent to a CE mechanism, where the chemical reaction produces the electroactive species. Accordingly, the reaction of Cr(III)–H2O–DTPA and \( {\mathrm{NO}}_3^{-} \) would produce the electroactive species Cr(III)–NO3–DTPA and this last species would release \( {\mathrm{NO}}_2^{-} \) to the solution during the electrochemical step. In this regard, the complex of Cr(III)–DTPA would work as the catalyzer that allows the reduction of \( {\mathrm{NO}}_3^{-} \) to \( {\mathrm{NO}}_2^{-} \). Furthermore, it was found that the electrochemical reaction is quite irreversible, with a constant of k s?=?9.4?×?10?5 cm s?1, while the constant for the chemical step has been estimated to be k chem?=?1.3?×?104 s?1. Considering that the equilibrium constant is K?=?0.01, it is possible to estimate the kinetic constants of the chemical reaction as k 1?=?1?×?102 s?1 and k ?1?=?1.29?×?104 s?1. These values of k 1 and k ?1 indicate that the exchange of water molecules by nitrate is fast and that the equilibrium favors the complex with water. Also, a value for the formal potential E°’?≈??1.1 V was obtained. The model used for simulating experimental curves does not consider the adsorption of reactants yet. Accordingly, weak adsorption of reagents should be expected.  相似文献   

18.

Background

Thiazolidinedione is a pentacyclic moiety having five membered unsaturated ring system composed with carbon, oxygen, nitrogen and sulfur molecules at 1 and 3 position of the thiazole ring and widely found throughout nature in various form. They favourably alter concentration of the hormones secreted by adipocytes, particularly adiponectin. They also increase total body fat and have mixed effects on circulating lipids. Thiazolidinedione nucleus is present in numerous biological moieties and has different pharmacological activities likes, e.g. antimalarial, antimicrobial, antimycobacterial, anticonvulsant, antiviral, anticancer, anti-inflammatory, antioxidant, anti-HIV (human immunodeficiency virus) and antituberculosis.

Results and discussion

The synthesized compounds were screened for their in vitro antimicrobial potential against Gram (positive and negative) bacterial and fungal strains by tube dilution technique. In this series, compound 10 exhibited significant antimicrobial activity against B. subtilis and S. aureus with MIC?=?4.2?×?10?2 µM/ml, compound 15 showed significant activity against K. pneumonia with MIC?=?2.60?×?10?2 µM/ml and compound 4 displayed potent antibacterial activity against E. coli with MIC?=?4.5?×?10?2 µM/ml. Compound 10 had most potent antifungal activity against C. albicans and A. niger with MIC?=?4.2?×?10?2 µM/ml. Compounds 12 and 15 were found as most active antidiabetic agents having IC50?=?27.63 μg/ml and 22.35 μg/ml, respectively, using DPPH assay. Antioxidant activity results indicated that compounds 3 and 9 displayed good antioxidant agent with IC50?=?29.04 μg/ml and 27.66 μg/ml respectively, using α amylase assay.

Conclusion

All the synthesized derivatives exhibited good antimicrobial, antidiabetic and antioxidant activities using specific methods then compared with mentioned standard drugs. Especially, compounds 3, 4, 9, 10, 12 and 15 displayed highest activity. Structure activity relationship demonstrated that presence of electron withdrawing group (o-NO2, p-Cl, p-Br) enhanced the antibacterial activity against E. coli as well as increased the antioxidant activity while the presence of electron releasing group (o/p-OCH3, 3,4,5-trimethoxy) enhanced the antibacterial activity against S. aureus, B. subtilis, S. typhi, K. pneumonia, C. albicans and A. niger as well as the antidiabetic activity.
  相似文献   

19.
The antihypertensive drug amlodipine has been characterized voltammetrically in a carbon paste electrode by means of anodic stripping voltammetry. An adsorptive stripping method in a carbon paste electrode for trace determination of amlodipine has been described. Cyclic voltammetric studies indicated the oxidation of amlodipine besylate at the electrode surface through a single two-electron irreversible step fundamentally controlled by adsorption. A study of the variation in the peak current with solution variables such as pH, ionic strength, concentration of amlodipine, possible interference, and instrumental variables, such as preconcentration time and accumulation potential, has resulted in the optimization of the oxidation signal for analytical purposes. By anodic adsorptive anodic stripping voltammetry, the calibration plot was linear in the range 9.9 × 10?9 ? 1.4 × 10?7 M with a detection limit of 2 × 10?10 M in a carbon paste electrode at pH 11.0. The procedure was successfully applied to the assay of amlodipine besylate in some commercial products in the market (Amlopres®, Amlodipine, and Norvasc®). The percentage recoveries were in agreement with those obtained by the reference method.  相似文献   

20.
In this work, a simple and novel electrochemical biosensor based on a glassy carbon electrode (GCE) modified with graphene oxide nanosheets (GO) was developed for detection of DNA sequences. The morphology of prepared nanoplatform was investigated by scanning electron microscopy, infrared (FTIR) and UV/Vis absorption spectra. The fabrication processes of electrochemical biosensor were characterized with cyclic voltammetry and electrochemical impedance spectroscopy (EIS) in an aqueous solution. The optimization of experimental conditions such as immobilization of the probe BRCA1 and its hybridization with the complementary DNA was performed. Due to unique properties of graphene oxide nanosheets such as large surface area and high conductivity, a wide liner range of 1.0 × 10?17–1.0 × 10?9 M and detection limit of 3.3 × 10?18 M were obtained for detection of BRCA1 5382 mutation by EIS technique. Under the optimum conditions, the proposed biosensor (ssDNA/GO/GCE) revealed suitable selectivity for discriminating the complementary sequences from non-complementary sequences, so it can be applicable for detection of breast cancer.  相似文献   

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