Mixture Of Acetylacetone Research Articles

Thermodynamic Excess Properties of Binary Mixtures of Acetyl acetone and Ethyl Acetate

The density (ρ), viscosity (η), surface tension (σ), and refractive index (R) of binary mixtures of acetylacetone (acac) with ethyl acetate (Etac) were determined at atmospheric pressure over the entire composition range of mixtures. The values of mixtures and pure liquids have been used to calculate the excess volume (VE), deviation in viscosity (Δη), and deviation in surface tension. The computed results were fitted to the Redlich–Kister polynomial equation. The excess molar volume (VE) for the binary system investigated exhibits a positive deviation at 298.15 K, and the positive deviation at 303.15 K becomes too negative as the mole fraction Xacac increases. The deviation in viscosity (Δη) and deviation in surface tension (Δσ) show negative values from the ideality at 303.15 The negative magnitude suggests the presence of strong intermolecular interactions between unlike molecules in the binary mixtures.

A rapid HPLC–DAD method for quantification of amikacin in pharmaceuticals and biological samples using pre-column derivatization with Hantzsch reagent

Amikacin (AMK) is an important member of aminoglycoside class, and its determination has therapeutic importance due to its matchless potency against gram –ve pathogens. Due to narrow therapeutic window, its monitoring in clinical samples is inevitable. Direct determination of AMK using HPLC with UV–visible detection is not possible because of its limited absorbance. Herein, Hantzsch reagent (mixture of acetylacetone, formaldehyde and acetate buffer) was used as pre-column derivatization for AMK. UV–visible detection was performed at 340 nm. Separation and identification of derivatized drug (amikacin) were carried out using C-18 column Kromasil 100 (15 cm × 0.46 mm, 5 μm) with isocratic mobile phase elution of pH 5 (acetate buffer 0.01 M):acetonitrile (30:70 v/v) with flow rate of 1 ml/min. The procedure was able to resolve AMK from endogenous compounds and from cephalosporin drug (most prescribed combination) with run time of 10 min. Under optimized conditions; calibration curve was linear in the range 0.10–25.0 µg/mL with LOD and LOQ values of 0.024 and 0.071 µg/mL. Method was also validated for reproducibility, ruggedness and accuracy. The procedure was found sensitive, robust and precise for the comprehensive analysis (qualitative and quantitative) that was applied for determination of AMK in pharmaceuticals, urine and blood samples.

Novel synthesis of ZnO thin films by facile solution process

A facile solution process to synthesis ZnO thin films was successfully conducted in this work. Zinc acetate dihydrates were used as the main precursor, dissolved in the mixture of acetylacetone and ethanol whichact as solvent and precursor simultaneously. This mixture deposited by spin coating and dried under ambient atmosphere at room temperature. The reaction mechanism, structure, morphology, chemical composition and optoelectrical properties of the resulted ZnO thin film were studied. The as deposited films were annealed at 500 °C for 2 h under O2 gas flow added with H2O vapor and CO2 gas. The ZnO thin films showed a dense, homogenous morphology and high transparency. The film is an n-type semiconductor with 3.18 eV bandgap, has 1.25 × 10−19 cm3 carrier concentration, 12 cm2/Vs electron mobility and 2.42 × 10−3 Ω·cm resistivity making it suitable for application as window layer in a photovoltaic cell.

Effects of acetylacetone on the thermal and photochemical conversion of benzoquinone in aqueous solution

Quinones are components of electron transport chains in photosynthesis and respiration. Acetylacetone (AA), structurally similar to benzoquinone (BQ) for the presence of two identical carbonyl groups, has been reported as a quinone-like electron shuttle. Both BQ and AA are important chemicals in the aquatic environment. However, little information is known about their interactions if co-existed. We found here that AA significantly enhanced the conversion of BQ. By analyzing the evolution of chemical concentration, solution pH, dissolved oxygen, and the final products, the interactions between AA and BQ were elucidated. The reactions between BQ and AA generated oxygen but ultimately led to the reduction of solution pH and dissolved oxygen. The reactions proceeded faster under indoor lighting condition than in the dark. The formation of semiquinone radicals is believed as the primary step. The secondary AA-derived radicals might be strongly oxidative or reductive, depending on the concentration of dissolved oxygen. Insoluble humus was generated in the mixture of BQ and AA. These results suggest that the presence of AA might interfere with photosynthesis and respiration through the interactions with quinones.

Nano3YSZ electrophoretic deposition from acetylacetone + ethanol solvent on the surface of AZ91 magnesium alloy

In the present work, the conditions for electrophoretic deposition of yttria-stabilised zirconia (YSZ) nanopowder have been investigated. For this purpose, the mixture of acetyl acetone and ethanol with different mixing ratios was used as solvent with iodine as a dispersant. To achieve a smooth, homogeneous and crack-free coatings, the following parameters were chosen to be optimised: the mixing ratio of acetyl acetone and ethanol, voltage and duration of deposition. The obtained coatings were observed by scanning electron microscope and optical microscope. The weight of deposits was also measured in different deposition conditions to observe the effects of above-mentioned parameters on the weight and consequently the quality of green coatings. All in all, the suspensions which composed of 50 vol% acetylacetone + 50 vol% ethanol led to more uniformity and fewer cracks/pores in deposits. The other parameters were optimised as follows: deposition voltage of 40 V and deposition time of 3 min. The results of polarisation test showed an improved corrosion resistance of the magnesium alloy with the application of YSZ coating, so that the Icorr value decreased from 1.16 to 0.088 mA.

Preparation of thin bilayer coatings based on lanthanum, nickel, and cerium mixed oxides by electrophoretic deposition

This paper examines the feasibility of using electrophoretic deposition for producing thin films of cathode materials based on lanthanum nickel oxides (with the lanthanum nickelate La2NiO4 + δ (LNO) as the predominant phase). We have determined the particle size and zeta potential of nonaqueous suspensions of LNO micro- and nanopowders prepared by solid-state reactions, pyrolysis of liquid precursors, and laser evaporation of a target. Using ultrasonic processing, we have obtained stable LNO nanopowder suspensions in acetylacetone and an isopropanol + acetylacetone mixture, which have zeta potentials of +25 and + 38 mV, respectively. Electrophoretic deposition on a dense model cathode has produced thin bilayer coatings from electrode and electrolyte materials (LNO and Се0.8(Sm0.75Sr0.2Ba0.05)0.2O2–δ), which are of interest for solid oxide fuel cell technology.

The acetylacetone-water complex in a low-temperature solid argon matrix

A mixture of acetylacetone and water was condensed in low-temperature Ar matrices at 5K, and infrared spectra were observed. It was found that the H2O molecules formed hydrogen bonds with the acetylacetone. The structure of the H2O-C5H8O2 complex was estimated with the aid of a density functional calculation. A similar sample was prepared using deuterium-substituted water to confirm the structure of the complex. Upon annealing the matrix-isolated sample, aggregation of H2O molecules was observed and the amount of the complex remained unchanged.

Fabrication of Chromium (III) Oxide (Cr2O3) Coating by Electrophoretic Deposition

Chromium (III) oxide has been widely used as a coating material for corrosion resistance. In this study, electrophoretic deposition (EPD) of nano chromium (III) oxide (Cr2O3) particle (60 nm) was investigated to develop coatings with potential applications of anticorrosive material. The stable suspension of Nano‐Cr2O3 particles were obtained in the mixture of acetylacetone and ethanol containing 0.00025 M nitric acid. The coating growth rate was studied with using different deposition times in the range of 1–30 min at voltages of 50–150 V with various concentrations of suspension. The electrophoretic Cr2O3 coating was sintered at 1000°C and 1200°C for 2 h. The micro‐morphology of coating was qualitatively characterized by focused ion beam scanning electron microscopy (FIB/SEM). The SEM micrographs obviously showed that the electrophoretic Cr2O3 coating has formed a uniform and dense ultrathin layer after sintering at 1200°C. We demonstrated that nano‐Cr2O3 coating could be easily obtained by EPD for the surface modification of metallic materials for potential interest in hard wear‐resistant and/or low‐friction coatings.

Fabrication of cobalt oxide (Co3O4) coating by electrophoretic deposition

In this study, electrophoretic deposition (EPD) of nano-cobalt oxide (Co3O4) particle (30nm) was investigated to develop coatings with potential applications in many fields. Nano-Co3O4 particles were suspended in mixture of acetylacetone and ethanol and stable suspensions were obtained. The deposits were characterized qualitatively by X-ray diffraction, SEM observations and EDS analysis. The coating growth rate was varied by different deposition times in the range of 1–30min at voltages of 100–150V. Results of this study demonstrate that EPD is a feasible method of fabricating nano-Co3O4 coating which is of potential interest in gas sensors, heterogeneous catalysts, supercapacitors and many other applications.

Magnetic softening of Co doped α′′-Fe<sub>16</sub>N<sub>2</sub> containing residual Fe–Co alloy prepared in low temperature nitridation

Preparation and magnetic properties were investigated on the Co doped α′′-Fe16N2 obtained in low temperature nitridation of bcc Fe1−xCox alloys to change its magnetic coercivity. The alloys were prepared by the reduction of (Fe1−xCox)3O4 obtained by hydrolysis of iron and cobalt acetylacetonate mixture in benzyl alcohol. Fine powder of the pure spinel-type (Fe1−xCox)3O4 was obtained in x = 0–0.05. The oxides were reduced to bcc Fe1−xCox alloy at 400°C in H2 gas and then nitrided at 150°C for 5 or 8 h under NH3 gas flow. XRD and X-ray absorption spectroscopy suggested the nominal “α′′-(Fe1−xCox)16N2”, similar to “α′′-Fe16N2” was obtained as a mixture with the residual bcc Fe1−xCox alloy at x = 0.03 as in the case of the nitrided product without cobalt. The present nitrided product exhibited a larger magnetization of 217 Am2 kg−1 and a smaller magnetic coercivity of 30 mT at x = 0.03 than those for the present products without the Co doping.

Enhancement of thermal stability of silver(I) acetylacetonate by platinum(II) acetylacetonate

Thermal gravimetric analysis of equimolar silver(I) acetylacetonate–platinum(II) acetylacetonate mixture shows a significant increase in thermal stability of silver(I) acetylacetonate in the presence of the Pt counterpart. The heated mixture was examined by differential scanning calorimetry and complementary analyses of gaseous products, residues and sublimed fractions by Fourier transform infrared, Raman and X-ray-photoelectron spectroscopy, X-ray diffraction and scanning and high-resolution transmission electron microscopy. It is assumed that silver(I) acetylacetonate is thermally stabilized due to a week bonding with Pt chelate. An interaction between both chelates gets support from the structure of the residual powder which is composed of Ag, Pt, C and O elements and Pt oxides and contains silver nanoparticles whose decreased unit cell parameter can be due to substitution of silver by platinum.

Excess molar volumes and refractive indices of binary liquid mixtures of acetyl acetone with n-Nonane, n-Decane and n-Dodecane at (298.15, 303.15, and 308.15) K

Density and refractive index at (298.15, 303.15 and 308.15) K for the binary liquid mixtures of acetylacetone with n-Nonane, n-Decane and n-Dodecane have been measured over the entire mole fraction range of binary liquid mixtures. Using these data, excess molar volume and deviation in molar refraction were calculated. The computed quantities were fitted to Redlich–Kister polynomial equation to derive the coefficients and estimate the standard deviation values. These quantities have been discussed in terms of intermolecular interactions.

PHYSICAL CHARACTERIZATION OF Ni(II) DOPED TiO<sub>2</sub> NANOCRYSTAL BY SOL-GEL PROCESS

Ni(II) doped titanium dioxide has been prepared by using sol-gel process. Ni(II) ion was incorporated into titanium dioxide by reacting Ni(II) chloride with titanium tetraisopropoxide (TTiP)-acetyl acetone mixture in isopropanol solvent. The effects of transition metal ion doping on the physical properties have been investigated. UV/Vis spectrophotometer, TGA-DTA, X-ray diffraction (XRD) and DR-UV/Vis were used to investigate the spectra absorption of nanosol, nanoparticle thermal transition, structure of crystal and band edge absorption, respectively. The results at addition of 5% Ni/Ti revealed that absorbance of nanosol increased from 0.811 (λmax: 342 nm) to 2.283 (λmax: 350 nm). The crystallization temperature transition from anatase to rutile decreased from 500 °C to 475 °C. The particle size increased from 18.51 nm to 20.35 nm, while the band gap energy (Eg) decreased from 2.73 eV to 2.51 eV.

ChemInform Abstract: Structural Characterization and Photoluminescent Properties of (La1‐xSmx)2Ti2O7 Solid Solutions Synthesized by a Sol—Gel Route.

AbstractThe title compounds (0 ≤ x ≤ 1.0) are synthesized by the sol—gel method from solutions of Ti(OiPr)4 in a mixture of acetylacetone and 2‐methoxyethanol and La(NO3)3 and Sm(NO3)3 in 2‐methoxyethanol (40 °C, 3 h) followed by calcination of the obtained gels at 700 °C for 6 h.

Liquid−Liquid Equilibrium, Solid−Liquid Equilibrium, Densities, and Refractivity of a Water, Chloroform, and Acetylacetone Mixture

Molybdenum is chemically combined with other elements and usually extracted from acid leaching a residual solution of molybdenite. Understanding the behavior of the solvents is important for the optimization of the separation procedures. Therefore, binary and ternary liquid−liquid equilibria (LLE) were measured for a mixture of chloroform, acetylacetone, and water at (293.15 to 333.15) K and atmospheric pressure (101.3 ± 0.7 kPa). The solid−liquid equilibrium (SLE) between chloroform and acetylacetone was also determined by visual techniques. This system has a single eutectic point. The experimental LLE and SLE data were well-correlated by the nonrandom two-liquid (NRTL) and universal quasichemical activity coefficient (UNIQUAC) models. In addition, the excess molar volume (VE) and refractivity (nD) for the binary chloroform + acetylacetone mixture were measured at 298.15 K over the entire composition range. The experimental data were satisfactorily fit using the Redlich−Kister polynomial.

Trace level determination of beryllium in natural and flavored mineral waters after pre-concentration using activated carbon

The concentrations of beryllium (Be) in natural and flavored mineral water samples were determined by flame atomic absorption spectrophotometer (FAAS) after pre-concentration based on the complexation of Be+2 with a mixture of acetylacetone (pentane-2,4-dione) plus morin (3,5,7,2′,4′-pentaoxyflavone) and adsorption on activated carbon. The adsorbed complex was eluted with 1.5 ml of 2.0 M HNO3 and evaporated to dryness. After adding 1.5 ml of 2 M HNO3 and centrifuging, Be in acid solution was determined by FAAS. To remove a number of metals present in water, EDTA was used as a chelating agent. Beryllium in mineral water samples was pre-concentrated by 500-fold, taking 750 ml as initial sample and 1.5 ml as the final volume. The relative standard deviations were sufficiently low for practical purposes and recoveries were up to 85%. Spiking experiments were performed in real samples to establish accuracy and recoveries. The limits of detection and quantification were 0.01 and 0.03 ng ml−1, respectively. Twenty samples were analyzed for their beryllium content using optimum parameters. The highest concentration of beryllium was found to be 0.94 ± 0.15 ng ml−1 in a natural mineral water, while beryllium was not detected in five samples.

Ultrasonic Studies on Binary Mixtures of Acetyl Acetone at 301K

The ultrasonic velocity (U), density (ρ) and viscosity (η) measurements have been carried out for the binary mixtures of acetyl acetone with benzene, carbon tetra chloride and isoamyl alcohol at 301 K. From the measured values of ultrasonic velocity, density and viscosity, parameters such as internal pressure (πi), free volume (Vƒ) and acoustical parameters such as adiabatic compressibility (β), inter molecular free length (Lƒ), acoustic impedance (Z), relaxation time (τ) have been calculated. The results have been analyzed and interpreted in terms of molecular interactions.

Efficient post-processing of aqueous generator eluates facilitates 68Ga-labelling under anhydrous conditions

The present study reports a convenient method for 68Ga-labelling under anhydrous conditions using solid-phase derived gallium-68-acetylacetonate ([ 68Ga]Ga(acac)3) in a microwave-enhanced radiosynthesis. Commercial 68Ge/68Ga-radionuclide generators utilizing TiO2 to adsorb 68Ge(IV) (Obninsk-generators) were used. The initial aqueous generator eluate was transferred online onto a cation exchange resin and 68Ga was absorbed quantitatively. From this resin, 68Ga was eluted with different acetone-based, non-aqueous solvent systems. More than 95% of the generator-eluted 68Ga was obtained from the cation exchange resin with 600 μL of a 98% acetone/2% acetylacetone mixture providing n.c.a. [ 68Ga]Ga(acac)3 as labelling agent. Water-insoluble macrocyclic polypyrrole derivatives were chosen as model compounds for a proof-of-principle labelling of lipophilic compounds with 68Ga. Labelling of two different porphyrin derivatives, meso -tetraphenyl-porphyrin (Tpp) and (3-(1-hydroxyheptyl)deuteroporphyrin dimethylester (HHDPD) was performed in chloroform in a focused microwave synthesis system in yields of up to 90% within 5 min using phenol as co-ligand. Moreover, new co-ligands were investigated to be more effective and significantly less toxic than phenol. Among the phenol alternatives, gentisic acid (2,5-dihydroxy benzoic acid, DHB, 5 mg) emerged as the most useful, non-toxic phenol substitute. It facilitates reducing the load of co-ligand by 95%, while providing an increased labeling yield of 97%. 68Ga-labelled porphyrins may facilitate the medical application for molecular imaging via positron emission tomography.

The effect of benzimidazole and zinc acetylacetonate mixture on cathodic disbonding of epoxy coated mild steel

Electrochemical behavior of mild steel in the presence of zinc acetylacetonate (Zn(acac) 2) and benzimidazole (BIMIDA) was evaluated by electrochemical impedance spectroscopy (EIS) in 3.5% NaCl solution and compared to zinc phosphate (ZP) pigment and zinc potassium chromate (ZPC) pigment extracts. Results showed superior performance of Zn(acac) 2 and BIMIDA mixture (ZBM) compared to ZP pigment, while it introduced inferior inhibitive action compared to ZPC pigment. The epoxy coatings were formulated with ZBM as anticorrosive additive, ZP and ZPC pigments. The disbonding rate of coated steel follows the order: Blank > ZP > ZBM > ZPC. EIS results showed a complex film could be formed at the hole area for the coatings formulated with ZP, ZBM and ZPC. It is concluded that the stronger the complex film on the surface, the lesser the cathodic disbonding rate would be.

Ultrasonic study of binary mixtures of acetylacetone with polar diluents at 303.16 K vis-a-vis molecular interaction

The ultrasonic velocity (C) and density (p) of binary mixture of acetylacetone with polar diluents have been measured at temperature 303.16 K and frequency of 2 MHz. The data of C and p have been used to evaluate, isentropic compressibility (β), acoustic impedence (Z) and intermolecular free length (L f ) to study the molecular interaction. The study reveals that interaction is maximum in bromo-benzene acetylacetone mixture.