Cloud point extraction of aluminum (III) in water samples and determination by electrothermal atomic absorption spectrometry,flame atomic absorption spectrometry and UV-visible spectrophotometry

Cloud point extraction was applied as a preconcentration step for the determination of trace level of Al(III) in water samples with electrothermal atomic absorption spectrometry (ETAAS), flame atomic absorption spectrometry (FAAS) and UV-visible spectrophotometry. The aluminum was extracted as aluminum-Eriochrome Cyanine R (ECR) complex, at pH 6 by micelles of the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114). The investigations showed that the same CPE procedure can be used for different detection techniques. The results obtained from these techniques were evaluated. Under the optimal conditions, limit of detection obtained with ETAAS, FAAS and UV-visible spectrophotometry were 0.03 ng mL^?1, 0.06 µg mL^?1 and 0.01 µg mL^?1, respectively. The accuracy of the procedure was tested by analysing certified reference material. The method was successfully applied to determination of aluminum in water samples and dialysis fluid.     

Selective back-extraction and preconcentration of zinc(II) from metal-1,3,5-triketone extracts prior to its determination by flame atomic absorption spectrometry

A simple back-extraction method was developed for the separation and preconcentration of trace levels of zinc from different matrices. Ethyl-2-(4-methoxybenzoyl)-3-(4-methoxyphenyl)-3-oxopropanoylcarbamate (EMPC) was used as a new complexing agent for the extraction of zinc(II) from the aqueous sample phase to the methyl isobutyl ketone (MIBK) phase as Zn(EMPC)₂ complexes. The Zn(II) can be selectively stripped with 1?mL of 0.5?mol?L^?1 HCl from Mⁿ⁺(EMPC)_n complexes [Ag(I), Al(III), Cd(II), Cr(III), Cu(II), Fe(II), Fe(III), Mn(II), Ni(II), Pb(II) and Pd(II)] which dissolved in MIBK phase. Some experimental parameters, which are important for the whole extraction process, including pH, sample volume, shaking time, amount of the EMPC reagent, amount of MIBK, ionic strength, and type of back-extractant were investigated. The recovery for Zn(II) was greater than 95%. The detection limit of the method was found to be 0.2?µg?L ^{? 1} and the relative standard deviation as 6.4%. The concentrations of Zn(II) in the certified reference materials (LGC6019 river water and NIST-1547 peach leaves) by the presented method were in good agreement with the certified values. The proposed method was succesfully applied to the determination of zinc in some natural waters, rice, hair, soil, and tea samples.     

Synthesis in water-free DMF, characterization, electrical, and gas sensing properties of bis[2-(2-aminoethylamino)ethanol]copper(II) dibromide

2-(2-Aminoethylamino)ethanol (L) reacts with cupric bromide in dimethylformamide to give a mononuclear complex of Cu(II) [L₂Cu]Br₂, with six-coordinate distorted octahedral geometry, in which two molecules of tridentate (N,N,O) ligand are involved. The structure was confirmed by spectroscopic methods, elemental and thermogravimetric analyses, and magnetic measurements. Optimization of possible configurations indicated the formation of the trans structure of the complex. Experimental results indicate that the investigated complex, bis[2-(2-aminoethylamino)ethanol] copper(II) bromide, behaves as a semiconductor in the studied temperature range of 298–388 K. Gas sensing properties of the film for the volatile organic compounds (VOCs): acetone, tetra-chloromethane, chloroform, ethanol, and methanol, were also investigated as a function of vapor concentration and temperature in dark. The film showed maximum sensitivity to tetrachloromethane and ethanol vapors at room temperature. Responses of the film to the tested gases are reversible.     

Preparation of Methyl 6‐O‐p‐Nitrobenzoyl‐β‐d‐Glucoside

Methyl 6‐O‐p‐nitrobenzoyl‐β‐d‐glucoside was synthesized by reacting methyl 4,6‐O‐p‐nitrobenzylidine‐β‐d‐glucoside with N‐bromosuccinimide (NBS). First, methyl β‐d‐glucoside was converted into methyl 4,6‐O‐p‐nitrobenzylidine‐β‐d‐glucoside with p‐nitrobenzaldehyde. Later, methyl 4,6‐O‐p‐nitrobenzylidine‐β‐d‐glucoside was opened oxidatively with NBS to give methyl 6‐O‐p‐nitrobenzoyl‐β‐d‐glucoside.     

Synthesis and characterization of tellurium-doped CdO nanoparticles thin films by sol–gel method

In this work, tellurium (Te) doped CdO nanoparticles thin films with different Te concentrations (1, 3, 5, 7 and 10 %) were prepared by sol–gel method. The effects of Te doping on the structural, morphological and optical properties of the CdO thin films were systematically studied. From X-ray diffraction spectra, it has seen that all of thin films were formed polycrystalline and cubic structure having (111), (200) and (311) orientations. The structure of CdO thin films with Te-dopant was formed the unstable CdTeO₃ monoclinic structure crystal plane ( $ {\bar{\text{1}}\text{22}} $ 1 ¯ 22 ), however, the intensity of this unstable peak of the crystalline phase decreased with the increase of Te-doping ratio. The strain in the structure is also studied by using Williamson-Hall method. From FE-SEM images, it has seen that particles have homogeneously distributed and well hold onto the substrate surface. Additionally, grain size increases from 27 to 121 nm with the increase of Te-doping ratio. Optical results indicate that 1 % Te-doped CdO thin film has the maximum transmittance of about 87 %, and the values of optical energy band gap increases from 2.50 to 2.64 eV with the increase of Te-doping ratio. These results make Te-doped CdO thin films an attractive candidate for thin film material applications.     

Lyotropic Liquid Crystal to Soft Mesocrystal Transformation in Hydrated Salt–Surfactant Mixtures

Hydrated CaCl₂, LiI, and MgCl₂ salts induce self‐assembly in nonionic surfactants (such as C₁₂H₂₅(OCH₂CH₂)₁₀OH) to form lyotropic liquid‐crystalline (LLC) mesophases that undergo a phase transition to a new type of soft mesocrystal (SMC) under ambient conditions. The SMC samples can be obtained by aging the LLC samples, which were prepared as thin films by spin‐coating, dip‐coating, or drop‐casting of a clear homogenized solution of water, salt, and surfactant over a substrate surface. The LLC mesophase exists up to a salt/surfactant mole ratio of 8, 10, and 4 (corresponding to 59, 68, and 40 wt % salt/surfactant) in the CaCl₂, LiI, and MgCl₂ mesophases, respectively. The SMC phase can transform back to a LLC mesophase at a higher relative humidity. The phase transformations have been monitored using powder X‐ray diffraction (PXRD), polarized optical microscopy (POM), and FTIR techniques. The LLC mesophases only diffract at small angles, but the SMCs diffract at both small and wide angles. The broad surfactant features in the FTIR spectra of the LLC mesophases become sharp and well resolved upon SMC formation. The unit cell of the mesophases expands upon SMC transformation, in which the expansion is largest in the MgCl₂ and smallest in the CaCl₂ systems. The POM images of the SMCs display birefringent textures with well‐defined edges, similar to crystals. However, the surface of the crystals is highly patterned, like buckling patterns, which indicates that these crystals are quite soft. This unusual phase behavior could be beneficial in designing new soft materials in the fields of phase‐changing materials and mesostructured materials, and it demonstrates the richness of the phase behavior in the salt–surfactant mesophases.     

The uranium recovery from aqueous solutions using amidoxime modified cellulose derivatives. IV. Recovery of uranium by amidoximated hydroxypropyl methylcellulose

Amidoxime modified hydroxypropyl methylcellulose (HPMC) films (HPMC-g-AO) were used for the recovery of uranium from aqueous solutions by a complexation process. The adsorption experiments were carried out by immersion of a certain amount of films in UO₂ ²⁺ solutions (resultant pH 4.1) ranging in concentration from 100 to 1,000 ppm. The effect of temperature (25–50 °C) on the adsorption capacity of HPMC-g-AO was investigated at the optimized time. The adsorption kinetics and the thermodynamics as well as the adsorption capacity of HPMC-g-AO films were investigated. The adsorption capacity was found as 765 mg UO₂ ²⁺/g dry film. The kinetic and the thermodynamic parameters (i.e. activation energy, enthalpy, entropy and Gibbs free energy) for the interaction of UO₂ ²⁺ with HPMC-g-AO were calculated based on known basic relations. The results showed that adsorption occurred through strong electrostatic interactions with an enthalpy of ?36.5 kJ/mol. The desorption of UO₂ ²⁺ were investigated using different desorption agents such as EDTA, HCl, NaHCO₃, and NaOH. After the 2 weeks treatment period, the highest desorption yield were found as 23 % with NaHCO₃.     

Synthesis and Thermolysis of the Homoleptic Iron(II) Complex [Fe{cyclo‐(P5tBu4)}2]

Na[cyclo‐(P₅tBu₄)] ( 1 ) reacts with [FeBr₂(CO)₄] (2:1) to give the first homoleptic iron(II) complex [Fe{cyclo‐(P₅tBu₄)}₂] ( 2 ) containing two tridentate cyclo‐(P₅tBu₄)^– ligands. Thermolysis of 2 up to 500 °C produces a new phosphorus‐rich iron phosphide, calculated as FeP₆ according to the mass change.     

Chemical modification of silica gel with synthesized Schiff base hydrazone derivative and application for preconcentration and separation of U(VI) ions from aqueous solutions

Schiff base hydrazone derivative (HL) sorbent was synthesized according to the literature to be used in the adsorption and preconcentration of U(VI) ions from aqueous solution and it was exposed to immobilization, and new solid support material was obtained. For this purpose, Schiff base hydrazone derivative (HL) was chemically bonded to silica gel surface immobilized 3-aminopropyl trimethoxysilane, then analyzed by Fourier transform infrared, Brunauer–Emmett–Teller, scanning electron microscopy and elemental analysis. The influence of the solution pH, amount of sorbent, contact time, temperature, foreign ion effect and initial U(VI) concentration was investigated. The maximum U(VI) uptake capacity was found to be 8.46 mg/g.     

Simultaneous determination of seven phthalic acid esters in beverages using ultrasound and vortex‐assisted dispersive liquid–liquid microextraction followed by high‐performance liquid chromatography

A sensitive, rapid, and simple high‐performance liquid chromatography with UV detection method was developed for the simultaneous determination of seven phthalic acid esters (dimethyl phthalate, dipropyl phthalate, di‐n‐butyl phthalate, benzyl butyl phthalate, dicyclohexyl phthalate, di‐(2‐ethylhexyl) phthalate, and di‐n‐octyl phthalate) in several kinds of beverage samples. Ultrasound and vortex‐assisted dispersive liquid–liquid microextraction method was used. The separation was performed using an Intersil ODS‐3 column (C₁₈, 250 × 4.6 mm, 5.0 μm) and a gradient elution with a mobile phase consisting of MeOH/ACN (50:50) and 0.2 M KH₂PO₄ buffer. Analytes were detected by a UV detector at 230 nm. The developed method was validated in terms of linearity, limit of detection, limit of quantification, repeatability, accuracy, and recovery. Calibration equations and correlation coefficients (> 0.99) were calculated by least squares method with weighting factor. The limit of detection and quantification were in the range of 0.019–0.208 and 0.072–0.483 μg/L. The repeatability and intermediate precision were determined in terms of relative standard deviation to be within 0.03–3.93 and 0.02–4.74%, respectively. The accuracy was found to be in the range of –14.55 to 15.57% in terms of relative error. Seventeen different beverage samples in plastic bottles were successfully analyzed, and ten of them were found to be contaminated by different phthalic acid esters.