Toxicity of mercury on in vitro development of parthenogenetic eggs of a freshwater cladoceran Daphnia carinata

A series of recently synthesized benzo- and pyridine-substituted macrocyclic diamides were studied to characterize their abilities as lead ion carriers in PVC membrane electrodes. The electrode based on 3,15,21-triaza-4,5;13,14-dibenzo-6,9,12-trioxabicycloheneicosa-1,17,19-triene-2,16-dione exhibits a Nernstian response for Pb²⁺ ions over a wide concentration range (1.3 × 10⁻² to 3.6 × 10⁻⁶ mol L⁻¹) with a limit of detection of 2.0 × 10⁻⁶ mol L⁻¹ (0.4 ppm). The response time of the sensor is 16 s, and the membrane can be used for more than two months without observing any deviation. The electrode revealed comparatively good selectivities with respect to many cations including alkali earth, transition and heavy metal ions. The proposed sensor could be used in pH range of 3.7–6.5. It was used as an indicator electrode in potentiometric titration of chromate ions with a lead ion solution.     

Electrochemical determination of cadmium(II) at platinum electrode modified with kaolin by square wave voltammetry

In this work, determination of cadmium(II) using square wave voltammetry (SWV) was described. The method is based on accumulation of these metal ions on kaolin platinum electrode (K/Pt). The K/Pt performance was optimized with respect to the surface modification and operating conditions. The optimized conditions were obtained in pH of 5.0 and accumulation time of 25 min. Under the optimal conditions, the relationship between the peak current versus concentration was linear over the range of 9 × 10⁻⁸ to 8.3 × 10⁻⁶ mol L⁻¹. The detection limit (DL, 3σ) was 5.4 × 10⁻⁹ mol L⁻¹. The analytical methodology was successfully applied to monitor the Cd(II) content in natural water. Interferences were also evaluated.     

Mercury(II) selective membrane electrode based on 1,3-bis(2-methoxybenzene)triazene

A plasticized poly (vinyl chloride) membrane electrode based on 1,3-bis(2-methoxybenzene)triazene (MBT) for highly selective determination of mercury(II) has been developed. The electrode showed a good Nernstian response (30.2 ± 0.3 mV decade^− 1) over a wide concentration range (1.0 × 10^− 7−1.0 × 10^− 2 mol L^− 1). The limit of detection was 5.0 × 10^− 8 mol L^− 1. The electrode has a response time about 15 s and can be used for at least 1 month without observing any deviation from Nernstain response. The proposed electrode revealed an excellent selectivity toward mercury(II) ion over a wide variety of alkali, alkaline earth, transition, and heavy metal ions and could be used in the pH range 2.6–4.2. The electrode was used in the determination of Hg²⁺ in aqueous samples and as an indicator electrode in potentiometric titration of Hg(II) ions.     

Plastic deformation behavior in dual-phase Ni–31Al intermetallics at elevated temperature

Plastic deformation behavior of dual-phase Ni–31Al intermetallics at elevated temperature was examined. It was found that the alloy exhibited good plasticity under an initial strain rate of 1.25 × 10⁻⁴ s⁻¹ to 8 × 10⁻³ s⁻¹ in a temperature range of 950–1075 °C. A maximum elongation of 281.3% was obtained under an initial strain rate of 5 × 10⁻⁴ s⁻¹ at 1000 °C. The strain rate sensitivity, m value was correlated with temperature and initial strain rate, being in the range of 0.241–0.346. During plastic deformation, both the two phases Ni₃Al and NiAl in dual-phase Ni–31Al could co-deform without any void formation or debonding, the initial coarse microstructure became much finer after plastic deformation. Dislocation played an important role during the plastic deformation in dual-phase Ni–31Al alloy, the deformation mechanism in dual-phase Ni–31Al could be explained by continuous dynamic recovery and recrystallization.     

The bromination kinetics of phenolic compounds in aqueous solution

The purpose of this study was to investigate the bromination kinetics of selected phenolic compounds in aqueous solutions over the pH range of 5–11. The experiment results indicated that the reaction of hypobromous acid with the phenoxide ions controlled the overall reaction rate, whereas the reaction between hypobromite ion and the phenoxide ions and the reaction between hypobromous acid and the undissociated phenolic species were considered to be negligible respectively in the pH range of 7–9. The apparent second-order rate constants of the reaction of hypobromous acid with the phenoxide ions ranged from 7.9 × 10⁶ M⁻¹ s⁻¹ for 3-chlorophenol to 6.5 × 10⁸ M⁻¹ s⁻¹ for 3-methoxyphenol, respectively. The Hammett correlation could be successfully used to estimate the reactivity of bromine with substituted phenols and the linear regression was log(k₂) = −2.85б + 8.00. The rate constants of the reaction of bromine with phenol-like organic compounds were about three orders of magnitude higher than with chlorine and two to three orders of magnitude lower than with ozone.     

Preparation of double-doped BaCeO3 and its application in the synthesis of ammonia at atmospheric pressure

Perovskite-type oxides BaCe_0.90Sm_0.10O_3−δ (BCS) and BaCe_0.80Gd_0.10Sm_0.10O_3−δ (BCGS) were synthesized by the sol–gel method and characterized by thermal analysis (TG-DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Using the sintered samples as solid electrolytes and silver–palladium alloy as electrodes, ammonia was synthesized from nitrogen and hydrogen at atmospheric pressure in a solid-state proton-conducting cell reactor. The maximum rate of production of ammonia was 5.82×10⁻⁹ mol s⁻¹ cm⁻².     

Optimization and kinetics of electroless Ni–P–B plating of quartz optical fiber

The preparation of Ni–P–B coatings on surface of quartz optical fibers was carried out using electroless plating method. The effects of the concentrations of nickel chloride, sodium hypophosphite, potassium borohydride, ethylenediamine, cadmium sulfate and temperature on the quality of Ni–P–B coatings were investigated by orthogonal experiment and their optimal values were determined to be: 0.1 mol L⁻¹, 0.094 mol L⁻¹, 0.185 mol L⁻¹, 0.36 mol L⁻¹, 5.68 × 10⁻⁴ mol L⁻¹ and 90 °C, respectively. The effect of coarsening time of the naked fiber on the quality of Ni–P–B coatings was also researched and the optimal coarsening time was determined to be 15 min. Stereomicroscope, Scanning Electron Microscope and X-ray diffractometer were used to characterize the apparentness, morphology and structure of the prepared Ni–P–B coatings. Inductively Coupled Plasma-Atomic Emission Spectroscopy, Thermal Shock Method and Gravimetric Analysis Method were employed to analyze the composition, force of adhesion and solderability of the coatings, respectively. The results showed that a Ni–P–B coating with low surface roughness, good strength of adhesion, low resistivity and good solderability was successfully prepared. The kinetic models (Ni–P–B deposition rate equations) of the process were established as . The theoretical values calculated by the models were proved to be basically consistent with the practical measurements through experimental verification.     

Biosensor enhanced by glucose oxidase biomimetic membrane containing the platinum and silica nanoparticles

In this paper, glucose biosensor is fabricated with immobilization of glucose oxidase (GOx) in platinum and silica sol. The glucose biosensor combined with Pt and SiO₂ nanoparticles could make full use of the properties of nanoparticles. A set of experimental results indicates that the current response for the enzyme electrode containing platinum and silica nanoparticles increases from 0.32 µA cm^− 2 to 33 µA cm^− 2 in the solution of 10 mM β-D-glucose. The linear range is 3 × 10^− 5 to 3.8 × 10^− 3 M with a detection limit of 2 × 10^− 5 M at 3σ. The effects of the various volume ratios of Pt and SiO₂ sols with respect to the current response and the stability of the enzyme electrodes are studied.     

Cu diffusion kinetics in (Cu, Ni)3Sn intermetallic compound nanolayers investigated by an Energy-Dispersive-X-ray-based permeation test

The Energy-Dispersive-X-ray-based permeation and oxidation test has been further developed by an improved theoretical analysis, in which chemical potential gradients rather than concentration gradients are employed. The developed test is able to characterize diffusion kinetics in diffusion barriers at the nanometer scale. The Cu flux coefficient in (Cu, Ni)₃Sn intermetallic compound nanolayers was determined from the test to be 8.48 × 10^− 15 mol·(m·s·J/mol)^–1 exp(− 52.3 kJ·mol^− 1/RT) in a temperature range of 250 °C–400 °C.     

Electrical and optical properties of 12CaO·7Al2O3 electride doped indium tin oxide thin film deposited by RF magnetron co-sputtering

12CaO·7Al₂O₃ electride (C12A7:e⁻) doped indium tin oxide (ITO) (ITO:C12A7:e⁻) thin films were fabricated on a glass substrate by an RF magnetron co-sputtering system with increasing number of C12A7:e⁻ chips (from 1 to 7) and at various oxygen partial pressure ratios. The optical transmittance of the ITO:C12A7:e⁻ thin film was higher than 70% in the visible wavelength region. In the electrical properties of the thin film, a decrease of the carrier concentration from 2.6 × 10²⁰ cm^− 3 to 2.1 × 10¹⁸ cm^− 3 and increase of the resistivity from 1.4 × 10^− 3 Ω cm to 4.1 × 10^− 1 Ω cm were observed with increasing number of C12A7:e⁻ chips and oxygen partial pressure ratios. It was also observed that the Hall mobility was decreased from 17.27 cm²·V^− 1·s^− 1 to 5.13 cm²·V^− 1·s^− 1. The work function of the ITO thin film was reduced by doping it with C12A7:e⁻.     

Cyclic plasticity of single crystal nickel oriented for single slip

The cyclic deformation behavior of single crystal nickel was investigated by performing uniaxial fully reversed constant plastic strain amplitude fatigue experiments at plastic shear strain amplitudes ranging from 1.1 × 10⁻⁴ to 8.8 × 10⁻³. Digitally acquired stress–strain hysteresis loops were used to calculate friction and back stresses and to relate the shapes of the loops to the evolving dislocation structures and magnetomechanical effects. The results indicate that the cyclic stress–strain curve exhibits a plateau of 50 MPa between plastic strain amplitudes of 1 × 10⁻⁴ and 7 × 10⁻³. Saturation friction stress, calculated using the Cottrell method, is reasonably constant over the entire range of plastic strain amplitudes at a value of 15 MPa. The back stress is 35 MPa within the plateau and increases to 48 MPa at the highest strain amplitude. When cycled at low plastic strain amplitude, magnetomechanical effects account for a significant portion of the measured inelastic strain.     

Microstructure and superplasticity of Mg–Al–Ca electromagnetic casting alloys after hot extrusion

Microstructure and superplastic properties of the plates extruded from the Ca containing Mg alloy (1 wt.% Ca–AZ31) billets fabricated by electromagnetic casting (EMC) without and with electromagnetic stirring (EMS) were examined. The linear intercept grain sizes of the extruded materials were 3.7 μm and 2.1 μm, respectively. The material extruded from the EMC + EMS billet exhibited good superplasticity at low temperatures as well as at high strain rates, including the tensile elongations of 370% at 1 × 10⁻³ s⁻¹, −523 K and 550% at 1 × 10⁻² s⁻¹, −673 K. These values largely exceeded those of the AZ31 alloys with the similar grain sizes. The superior superplasticity of the extruded EMC + EMS billet could be attributed to fine grains and high grain stability at elevated temperatures by the presence of finely dispersed particles of thermally stable (Al,Mg)₂Ca phase. The constitutive equations were developed for describing the high-temperature deformation behavior of the fine-grained 1 wt.% Ca–AZ31 alloys with different grain sizes in wide range of temperature and strain rate.     

Effect of chemical etching on the surface morphology of laser-patterned lines with Er-doped CaF2 nanocrystals in oxyfluoride glass

The chemical etching behavior for the lines consisting of Er³⁺-doped CaF₂ nanocrystals patterned on the surface of an oxyfluoride glass by using a laser-induced crystallization technique (laser: Yb-doped YVO₄; wavelength: 1080 nm; power: 1.7 W; a scanning speed: 2 μm/s) in a nitric acid solution (1N HNO₃) is examined, and the morphology change in the lines due to the etching is characterized from confocal laser microscope observations and photoluminescence (PL) spectrum measurements of Er³⁺ ions. The higher and wider bumps compared with the bump of the original line (no etching) are observed in etched lines, and in particular, the surrounding of lines is etching away preferentially, forming the groove in both sides of line. PL spectra of Er³⁺ ions with strong intensities are observed from etched lines, suggesting that Er³⁺-doped CaF₂ nanocrystals are largely present just at the surface of etched lines. It is found that the chemical etching rate (1.2 × 10⁻² μm/min) of the crystallized bulk sample is smaller than that (5.4 × 10⁻² μm/min) of the precursor bulk glass, suggesting that CaF₂ nanocrystals formed have a high resistance against the chemical attack.     

Determination of cadmium at ultra-trace levels by CPE–molecular fluorescence combined methodology

A highly sensitive micelle-mediated extraction methodology for the preconcentration and determination of trace levels of cadmium by molecular fluorescence has been developed. Metal was complexed with o-phenanthroline (o-phen) and eosin (eo) at pH 7.6 in buffer Tris medium and quantitatively extracted into a small volume of surfactant-rich phase of PONPE 7.5 after centrifugating. The chemical variables affecting cloud point extraction (CPE) were evaluated and optimized. The RSD for six replicates of cadmium determinations at 0.84 μg L⁻¹ level was 1.17%. The linearity range using the preconcentration system was between 2.79 × 10⁻³ μg L⁻¹ and 2.81 μg L⁻¹ with a correlation coefficient of 0.99. Under the optimal conditions, it obtained a LOD of 8.38 × 10⁻⁴ μg L⁻¹ and LOQ of 2.79 × 10⁻³ μg L⁻¹. The method presented good sensitivity and selectivity and was applied to the determination of trace amounts of cadmium in commercially bottled mineral water, tap water and water well samples with satisfactory results. The proposed method is an innovative application of CPE-luminescence to metal analysis comparable in sensitivity and accuracy with atomic spectroscopies.     

Surface and grain-boundary energies as well as surface mass transport in polycrystalline CeO2

The multiphase equilibration technique for the determination of the equilibrium angles that develop at the interphase boundaries of a solid–liquid–vapor system, has been used to calculate the surface and interfacial energies in polycrystalline CeO₂ and CeO₂/Cu system in argon atmosphere at the temperature range 1473–1773 K. Linear temperature functions were obtained by extrapolation, for the surface energy γ_sv (J/m²) = 2.465–0.563 × 10⁻³ T and the grain-boundary energy γ_ss (J/m²) = 1.687–0.391 × 10⁻³ T of the ceramic, as well as for the interfacial energy γ_sl (J/m²) = 2.623–1.389 × 10⁻³(T −1356 K) of the CeO₂/Cu system. Grain-boundary grooving studied on polished surfaces of CeO₂ annealed in argon atmosphere at the same temperature range has shown that surface diffusion was the dominant mechanism for the mass transport. The surface diffusion coefficient can be expressed according to the equation D_s (m²/s) = 3.82 × 10⁻⁴ exp(−308,250/RT).     

Growth and optical characterizations of (Ba0.32Sr0.68)5Nb4O15 crystal

(Ba_0.32Sr_0.68)₅Nb₄O₁₅ crystal with sizes of Ø 17 × 35 mm was grown successfully by Czochralski technique method. The thermal anisotropy was discussed. The principal coefficients of thermal expansion along (100), (010), (001) directions were precisely measured to be 1.308 × 10^− 5, 1.288 × 10^− 5, 1.478 × 10^− 5 K^− 1, respectively. Its optical transparency range has been measured and found to span from 323 to 5500 nm. The bands present in the IR spectra were identified and assigned to the corresponding vibration modes of NbO₆ anions.     

Novel oxidative electrophilic coupling reactions of phenoxazine derivatives with MBTH and their applications to spectrophotometric determination of residual chlorine in drinking water and environmental water samples

Novel, sensitive and rapid spectrophotometric methods, using phenoxazine (PNZ), 2-chlorophe-noxazine (CPN) and 2-trifluoromethylphenoxazine (TPN) as chromogenic reagents for the determination of residual chlorine are proposed. The methods are based on the reduction of chlorine by an electrophilic coupling reagent, 3-methyl-2-benzothiazoline hydrazono hydrochloride hydrate (MBTH) in mild hydrochloric acid medium and subsequent coupling with PNZ, CPN or TPN. The blue color formed in the reaction showed maximum absorbance at 680–690 nm and obeyed Beer's law over the range 0.1–2.2 μg ml⁻¹. The molar absorptivity values with PNZ, CPN and TPN were 2.80 × 10⁴, 2.67 × 10⁴ and 1.91 × 10⁴ l mol⁻¹ cm⁻¹ and Sandell's sensitivity values were 0.028, 0.027 and 0.028 μg cm⁻² respectively. The proposed methods were successfully applied in the determination of residual chlorine in drinking water and environmental water samples. The performance of proposed methods was evaluated in terms of Student's t-test and variance ratio F-test which indicated the significance of proposed methods over the standard spectrophotometric method.     

Experimental comparison of different dead-time correction techniques in single-channel counting experiments

For single-channel counting, the dead-time correction method using transmission formulae was compared experimentally with the live-time technique. Agreement is within 4×10⁻⁴ for count rates up to 10⁴ s⁻¹ when the formulae for dead times in series are used and the dead-time value related to the analogue pulse width is adjusted for the BIPM modules. At higher count rates, a bias of 2×10⁻³ is observed. Two different live-time modules were compared and it was demonstrated that the live-time correction is also sensitive to the analogue pulse width and to the duration or rise time of the clock pulses. When these effects are taken into account, the two modules differ by only 5×10⁻⁴.     

Growth, thermal and spectroscopic characteristics of LiNd(WO4)2 crystal

Crystal growth, thermal and optical characteristics of LiNd(WO₄)₂ crystal have been investigated. The LiNd(WO₄)₂ crystal up to Ø15 × 32 mm³ has been grown by Czochralski technique. The hardness is about 5.0 Mohs’ scale. The specific heat at 50 °C is 0.42 J g⁻¹ K⁻¹. The thermal expansion coefficient for c- and a- axes is 1.107 × 10⁻⁵ and 2.104 × 10⁻⁵ K⁻¹, respectively. The absorption and fluorescence spectra and the fluorescence decay curve of LiNd(WO₄)₂ crystal were measured at room temperature. Some spectroscopic parameters such as the intensity parameters, the spontaneous transition probabilities, the fluorescence branching ratios, the radiative lifetimes and emission cross sections were estimated.