Use of the differential pulse cathodic adsorptive stripping voltammetric method for the simultaneous determination of trace amounts of cadmium and zinc

A selective and sensitive method for the determination of cadmium and zinc is presented. The method is based on the adsorptive accumulation of the complexes of Cd(II) and Zn(II) ions with 4-amiono-5-methyl-2.4-dihydro-3H-1,2,4-triazol-3-tion (MMTT) onto hanging mercury drop electrode (HMDE), followed by the reduction of the adsorbed species using a voltammetric scan using differential pulse modulation. The ligand concentration, pH, potential and time of accumulation, scan rate, and pulse height were optimized. Under the optimized conditions, a linear calibration curve was obtained for the concentration of Cd(II) and Zn(II) in the range of 5–450 and 5–850 ng/mL, respectively, with a detection limit of 1.7 ng/mL Cd(II) and 1.3 ng/mL Zn(II). The ability of the method was evaluated by analysis of cadmium and zinc in water and alloy samples The text was submitted by the authors in English.     

Synthesis of Fe—Ni—Ce trimetallic catalyst nanoparticles via impregnation and co-precipitation and their application to dye degradation

In this study, trimetallic catalysts were prepared via the co-precipitation and impregnation methods. In order to investigate the effect of impregnation on the catalytic activity and crystallite size, a trimetallic catalyst, Fe—Ni—Ce, was prepared through the co-precipitation method in one set of experiments, and cerium was impregnated with the Ni—Fe mixture in the final stage of the preparation in another set. Fourier transform infrared spectroscopy was employed to confirm the formation of trimetallic catalysts and the success of the impregnation method. The Brunauer-Emmett-Teller nitrogen adsorption isotherm exhibits a high specific surface area (approximately 39 m² g^?1) for the nanoparticles obtained by the impregnation method. The crystallography and morphology of the trimetallic catalysts thus prepared were characterised by X-ray diffraction and scanning electron microscopy. UV-VIS spectroscopy and methylene blue dye degradation tests were also performed to investigate the catalytic activity of the synthesised catalysts. The crystalline size was found to be smaller for the catalysts prepared by the impregnation method. In addition, the samples synthesised using the cerium impregnation method showed superior activity in the methylene blue dye degradation test. The effect of the catalyst dosage on dye degradation, as well as the effect of the initial dye concentration on the catalyst activity, was also studied for both methods.     

Estimation of Activation Energy from the Survival Yields: Fragmentation Study of Leucine Enkephalin and Polyethers by Tandem Mass Spectrometry

A simple collision model for multiple collisions occurring in quadrupole type mass spectrometers was derived and tested with leucine enkaphalin a common mass spectrometric standard with well-characterized properties. Implementation of the collision model and Rice-Ramsperger-Kassel-Marcus (RRKM) algorithm into a spreadsheet software allowed a good fitting of the calculated data to the experimental survival yield (SY) versus collision energy curve. In addition, fitting also ensured to estimate the efficiencies of the kinetic to internal energy conversion for Leucine enkephalin in quadrupole-time-of-flight and triple quadrupole instruments. It was observed that the experimental SY versus collision energy curves for the leucine enkephalin can be described by the Rice-Ramsperger-Kassel (RRK) formalism by reducing the total degrees of freedom (DOF) to about one-fifth. Furthermore, this collision model with the RRK formalism was used to estimate the critical energy (E _o ) of lithiated polyethers, including polyethylene glycol (PEG), polypropylene glycol (PPG), and polytetrahydrofurane (PTHF) with degrees of freedom similar to that of leucine enkephalin. Applying polyethers with similar DOF provided the elimination of the effect of DOF on the unimolecular reaction rate constant. The estimated value of E _o for PEG showed a relatively good agreement with the value calculated by high-level quantum chemical calculations reported in the literature. Interestingly, it was also found that the E _o values for the studied polyethers were similar.

Adsorption/desorption of acid violet-7 onto magnetic MnO2 prior to its quantification by UV–visible spectroscopy: optimized by fractional factorial design

Research on Chemical Intermediates - A highly efficient magnetic adsorbent is presented to preconcentrate acid violet-7 (AV-7) prior quantifying by UV–visible spectroscopy...     

Fiber optic-linear array detection spectrophotometry in combination with dispersive liquid-liquid microextraction for preconcentration and determination of copper

In this research, simple, rapid and efficient method, dispersive liquid-liquid microextraction (DLLME) combined fiber optic -linear array detection spectrophotometry (FO-LADS) was developed using a cylindrical micro-cell for preconcentration and determination of Cu(II) in samples. DLLME and FO-LADS methods have good matching conditions for being combined since FO-LADS is a suitable method for the determination of analytes in low volume of the remained phase obtained after DLLME. Molar absorptivity of complex Cu with (4-benzylp iperidineditiocarbamate potassium salt) (BPDC) was determined as 2.75 × 10⁴ L mol^-1 cm^-1 at 7nmax = 436 nm. Under the optimum conditions the calibration graph was linear in the rage of 2–70 fug L^-1 with detection limit of 0.34 fug L^-1. The proposed procedure was successfully applied to the determination of Cu(II) in real water samples and human urine sample.     

Dispersive solid phase extraction of lead(II) using a silica nanoparticle-based ionic liquid ferrofluid

We demonstrate the application of an ionic liquid-based ferrofluid to the dispersive solid phase extraction of lead(II) using PAN as the chelator. The ionic liquid contains silica nanoparticles with a magnetic core as the dispersion medium, and its use results in improved stability of the colloidal dispersion and a complete extraction of lead(II) within a few seconds. In addition, there is no need for centrifugation. Specifically, the effect of different variables on the extraction of lead(II) was studied using an experimental design. Lead(II) was quantified by AAS. Under optimized conditions, the calibration graph for lead(II) is linear in the range from 5 to 372 μg L⁻¹, the relative standard deviation is 1.34 % (for n = 7), the limit of detection is 1.66 μg L⁻¹, and the enrichment factor is 200. The maximum adsorption capacity of sorbent was calculated to be 10.7 mg g⁻¹, and adsorption follows a Langmuir isotherm.

A schematic view of D-SPE experimental set up. We demonstrate the application of an ionic liquid-based ferrofluid to the dispersive solid phase extraction of lead(II) using PAN as the chelator. The ionic liquid contains silica nanoparticles with a magnetic core as the dispersion medium

     

Novel method for in-situ surfactant-based solid-phase extraction: application to the determination of Co(II) and Ni(II) in aqueous samples

We report on a completely new kind of solid phase extraction which we term in-situ surfactant-based solid-phase extraction (ISS-SPE). It represents a simple and rapid method for extraction from aqueous samples and preconcentration of compounds containing hydrophobic (alkyl) groups. A cationic surfactant containing alkyl chain is dissolved in the aqueous sample. Following the addition of hexafluorophosphate (HFP; an ion-pairing anion), solutions turn cloudy due to the interaction between the surfactant and the HFP ion. This is due to the formation of fine solid particles composed of the HFP salt of the cationic surfactant. The alkyl groups of the surfactant in the solid particles strongly interact with hydrophobic groups of analytes and become bound. The solid particles are centrifuged, and the sedimented particles can be either dissolved in an appropriate organic solvent, or leached with a solvent to recover the absorbed analyte(s). The method presented here has distinct advantages in that the extraction times are short and recoveries are high, probably a result of the formation of very fine particles of large specific surface, and of their good dispersion in the sample solution. The performance of ISS-SPE was demonstrated by extracting chelates of Co(II) and Ni(II) from water samples. Under the optimized conditions, the preconcentration factors are 51 and 45, respectively, and the detection limits are 0.9 and 0.6???g?L^?1. The method was validated by the analysis of a certified reference material and by comparing results with those obtained by electrothermal AAS.

P-Dodecylbenzenesulfonic acid(DBSA),a Brфnsted acid-surfactant catalyst for Biginelli reaction in water and under solvent free conditions

We report herein the use of p-dodecylbenzenesulfonic acid(DBSA) as a catalyst for a one-pot Biginelli reaction to afford 3,4- dihydropyrimidinone derivatives in good to excellent yields.This reaction proceeds efficiently in water and under solvent free conditions.Comparisons of results indicate that although the yields are high and comparable for both methods,the reaction times are considerably shorter under solvent free conditions.