Selective extraction and preconcentration of ultra-trace amounts of arsenic(V) ions using carbon nanotubes as a novel sorbent

In the present study, multiwalled carbon nanotubes (MWCNTs) as solid phase extraction sorbent were developed for preconcentration of arsenic(V) species prior to graphite furnace atomic absorption spectrometry (GFAAS) determination. Arsenic(V) was selectively sorbed on the packed column with MWCNTs within a pH 9.5 in the presence of 2-(5-bromo-2-pyridylazo)-5-diethyl amino phenol (5-Br-PADAP). The adsorbed species was then desorbed with 1 mL of 2.0 M HNO₃. Experimental parameters including pH, sample volume and flow rate, type, volume and concentration of eluent that influence the recovery of the arsenic(V) species were optimised. Under the optimised conditions, the calibration curve was linear in the range of 0.2–10.0 µg L^?1 with detection limit of 0.016 µg L^?1. The relative standard deviations (RSD) for seven replicate determinations at 1.0 µg L^?1 level of arsenic was 6.69%. The proposed method was successfully applied to the determination of arsenic in water samples and certified reference material (NIST RSM 1643e).     

Flame atomic absorption determination of trace amounts of cadmium after preconcentration using a thiol-containing task-specific ionic liquid

Dispersive liquid-liquid microextraction (DLLME) based on a task-specific ionic liquid (TSIL) was developed for the extraction and preconcentration of trace amounts of cadmium from aqueous samples, followed by flame atomic absorption spectrometry (FAAS) determination. In the proposed approach, cadmium ions are extracted from aqueous samples using small volumes of trioctylmethylammonium thiosalicylate (TOMATS) dissolved in acetone. TOMATS is a thiol-containing TSIL that can form metal thiolate complexes due to the chelating effect of the ortho-positioned carboxylate group relative to the thiol functionality. The main parameters affecting the performance of DLLME based on TSIL, such as pH, amount of TOMATS, extraction time, injection volume, salt addition, and centrifugation time, were optimized. Under optimum conditions, an LOD of 1.16 ng/mL and a good RSD of 1.8% at 60.0 ng/mL were obtained (n=7). The proposed method was applied to tap water, wastewater, well water, and milk samples. The results showed that DLLME based on TSIL combined with FAAS is a rapid, simple, sensitive, selective, low cost, volatile organic solvent-free, and efficient analytical method for the separation and determination of trace amounts of cadmium ions.     

Picosecond pulse radiolysis of direct and indirect radiolytic effects in highly concentrated halide aqueous solutions

Recently we measured the amount of the single product, Br(3)(-), of steady-state radiolysis of highly concentrated Br(-) aqueous solutions, and we showed the effect of the direct ionization of Br(-) on the yield of Br(3)(-). Here, we report the first picosecond pulse-probe radiolysis measurements of ionization of highly concentrated Br(-) and Cl(-) aqueous solutions to describe the oxidation mechanism of the halide anions. The transient absorption spectra are reported from 350 to 750 nm on the picosecond range for halide solutions at different concentrations. In the highly concentrated halide solutions, we observed that, due to the presence of Na(+), the absorption band of the solvated electron is shifted to shorter wavelengths, but its decay, taking place during the spur reactions, is not affected within the first 4 ns. The kinetic measurements in the UV reveal the direct ionization of halide ions. The analysis of pulse-probe measurements show that after the electron pulse, the main reactions in solutions containing 1 M of Cl(-) and 2 M of Br(-) are the formation of ClOH(-?) and BrOH(-?), respectively. In contrast, in highly concentrated halide solutions, containing 5 M of Cl(-) and 6 M of Br(-), mainly Cl(2)(-?) and Br(2)(-?) are formed within the electron pulse without formation of ClOH(-?) and BrOH(-?). The results suggest that, not only Br(-) and Cl(-) are directly ionized into Br(?) and Cl(?) by the electron pulse, the halide atoms can also be rapidly generated through the reactions initiated by excitation and ionization of water, such as the prompt oxidation by the hole, H(2)O(+?), generated in the coordination sphere of the anion.     

The discrete heat source approach to dust cloud combustion

In the present paper, combustion of dust clouds from the discrete point heat source method has been addressed. Time-place temperature profile generated by single particle burning has been obtained to study the dust combustion. The summation of the temperature profiles of burned and burning particles predict the temperature in the preheating zone so that the ignition time of layer in flame front can be determined. Consequently the flame propagating speed was obtained based on the dust concentration corresponding to particles spacing and particle diameter. This method has been validated with aluminum dust cloud combustion. Decrease in the dust concentration leads to the lean limit of dust combustion. Increase in particles diameter or reduction in the dust concentration causes higher lean limit and also reduction in the flame propagating speed. Adding the ignition energy as igniter to this system, provides the path to study the effects of ignition energy in the dust combustion.     

Encapsulation of palladium chloride using 2‐formylbenzoic acid supported by Fe3O4 nanoparticles modified with SiO2 and propylamine,its characterization and its application for Suzuki coupling reaction

A magnetically separable heterogeneous nanocatalyst, Fe₃O₄@SiO₂(CH₂)₃N―CH―Ar@Pd(0), was simply prepared and characterized using various techniques. The catalytic activity of this nanocatalyst was evaluated via the Suzuki–Miyaura cross‐coupling reaction of aryl halides with phenylboronic acid under various experimental conditions such as kind of base, solvent and temperature. This nanocatalyst is completely magnetically recoverable because of the superparamagnetic behaviour of Fe and can be reused with sustained selectivity and activity.     

A Simple, Rapid and Reagentless Turbidimetric Method for Determination of Light Stabilizer Tinuvin 622 in Polyethylene

This study presents an inexpensive and reagentless turbidimetric technique for the determination of Tinuvin 622 in polyethylene matrix. Tinuvin is dissolved in acetone, and water is added to it. The solubility of the analyte is reduced in the water/acetone mixture and it precipitates in the form of small particles. Different parameters affecting the analysis were studied, and it was found that in a 50:50 mixture of water and acetone high turbidity was obtained. Turbidity increases to 30min and remains constant for at least 1h. Stirring speed and ionic strength are no effective factors in this method. The linear dynamic range is relatively large (10–250mgL^–1) with a limit of detection of 3mgL^–1. The repeatability of the method is good, and the relative standard deviation for six repeated experiments performed on solutions containing 100mgL^–1 is 1.5%. To analyze real samples (polyethylene polymer), the matter is dissolved in hot xylenes, and methanol is added while the solution is being stirred. The precipitated polymer is filtered and the solution evaporated into the rotary. The remaining solids are dissolved in acetone and analyzed as standards. The obtained results were compared with those obtained by gas chromatography (after saponification) and no significant differences were observed.     

A novel composite derived from a metal organic framework immobilized within electrospun nanofibrous polymers: An efficient methane adsorbent

In this study, tantalum(V) metal organic framework (Ta-MOF) nanostructure was incorporated within polyvinyl alcohol (PVA) nanofibers to prepare an electrospun porous composite as a novel CH₄ adsorbent. The crystallinity, thermodynamic behavior, and textural properties of the products were investigated using instrumental analyses techniques. The results confirmed that the developed PVA/Ta-MOF electrospun nanofibrous composite exhibits higher thermal stability, considerable porosity, and larger surface area compared to the parent Ta-MOF. A 2^k factorial design was used for systematic study of the adsorption process. The results of response surface methodology (RSM) optimization indicated that the highest methane adsorption can be achieved at 24.40 °C and 3.70 bar in 23.60 min. These nano pore sorbents showed a significant potential for CH₄ adsorption due to the presence of Ta-MOF at the surface of nanofibrous composite compared to many other conventional sorbents that have been already used. This study introduces a novel biocompatible/biodegradable nanofibrous composite material with high methane adsorption performance and potentials for other applications.     

Highly porous WO3/CNTs-graphite film as a novel and low-cost positive electrode for vanadium redox flow battery

Journal of Solid State Electrochemistry - In this study, novel and low-cost tungsten oxide/carbon nanotubes-graphite-polyvinyl chloride (WO3/CNTs-graphite-PVC) film with porous 3D network structure...     

Application of modified multiwalled carbon nanotubes as solid sorbent for separation and preconcentration of trace amounts of manganese ions

In this work, the potential of modified multiwalled carbon nanotubes for separation and preconcentration of trace amounts of manganese ion is studied. Multiwalled carbon nanotubes were oxidized with concentrated HNO₃ and then modified with loading 1-(2-pyridylazo)-2-naphtol. Mn(II) ions could be quantitatively retained by modified multiwalled carbon nanotubes in the pH range of 8–9.5. Elution of the adsorbed manganese was carried out with 5.0 mL of 0.1 mol L^?1 HNO₃. Detection limit is 0.058 ng mL^?1 and analytical curve is linear in the range of 0.1 ng mL^?1–5.0 μg mL^?1 in the initial solution with a correlation coefficient 0.9977 and the preconcentration factor is 100. Relative standard deviation for eight replicate determination of 0.5 μg mL^?1 of manganese in the final solution is 0.41%. The effects of the experimental parameters, including the sample pH, flow rates of sample and eluent solution, eluent type, breakthrough volume and interference ions, were studied for preconcentration of Mn(II) ions in detail to optimize the conditions. The method was successfully applied for separation, preconcentration and determination of manganese in different samples.