A simple,rapid and sensitive method based on modified multiwalled carbon nanotube for preconcentration and determination of lead ions in aqueous media in natural pHs

In this study, multiwalled carbon nanotube (MWCNT) was modified by the pyridine group using a silane agent and characterized by infrared spectroscopy (IR), thermal analysis (TG/DTA), and elemental analysis (CHN) and scanning electron microscopy (SEM). The application of this sorbent was investigated in determination of lead ions in aqueous samples, using flame atomic absorption spectrometry (FAAS). Through this study, different parameters such as pH and sample flow rate on adsorption process and eluent concentration, volume and flow rate were optimized. The limit of detection (LOD), the relative standard deviation and the recovery of the method were 2 ng mL^?1, 1.3% and 99.7%, respectively. Two standard reference materials (NIST 1571 and NIST 1572) were used to verify accuracy of this method. Finally, the sorbent was successfully applied for extraction and determination of low levels of Pb(II) ions in aqueous samples.     

Constructing a new optical sensor for monitoring ammonia in water samples using bis(acetylacetoneethylendiamine)-tributylphosphin cobalt(III) tetraphenylborate complex-coated triacetylcellulose.

A new ammonia optical sensor was designed using bis(acetylacetoneethylendiamine)tributylphosphin cobalt(III) tetraphenylborate complex, coated on transparent triacetylcellulose film as membrane. The change in the absorbance of the optode at the maximum wavelength of 408 nm was related to ammonia concentration in aqueous samples. A buffer solution with a pH of 9 (sodium borate-HCl) was used. The optode was fully regenerated in pH 2. The linear dynamic range for determination of ammonia was 3.3 x 10(-4) to 6.9 x 10(-3) mol l(-1) with a detection limit of 5.0 x 10(-5) mol l(-1) and a response time range of 4 - 6 min. This membrane was successfully applied for determination of ammonia in drinking water.     

Donor ligand, basal ligand and solvent effects on the equilibrium constants of triphenylphosphinecobalt(III) Schiff base complexes with phosphite ligands

The equilibrium constants and the thermodynamic parameters were spectrophotometrically measured for the 1:1 adduct formation of [Co(Salen)(PPh₃)]ClO₄.H₂O, and [Co(7,7′-Me₂Salen)(PPh₃)]ClO₄.H₂O as acceptors, with P(OR)₃ (R = methyl, ethyl, and i-propyl) as donors, in acetonitrile (CH₃CN) and dimethylformamide (DMF) as solvents at constant ionic strength (I = 0.1 M NaClO₄), and various temperatures (t = 10–50 °C). Our results revealed the following trends: stability of the cobalt(III) Schiff base complexes toward a given phosphite donor, [Co(7,7′-Me₂Salen)(PPh₃)]⁺ < [Co(Salen)(PPh₃)]⁺; binding of the donors (phosphites) toward a given cobalt(III) Schiff base complex, P(OEt)₃ > P(OMe)₃ > P(O-ⁱPr)₃; influence of solvent on the stability of a given cobalt(III) Schiff base complex toward a given phosphite donor, CH₃CN < DMF.     

A selective modified carbon paste electrode for determination of cyanide using tetra-3,4-pyridinoporphyrazinatocobalt(II)

A chemically modified carbon paste electrode with 3,4-tetra pyridinoporphirazinatocobalt(II) (Co(3,4 tppa) was applied to the determination of free cyanide ion. The electrode has a linear range between 1.5 × 10⁻⁵ M and 1.0 × 10⁻² M with a Nernstian slope of 60 ± 1.5 mV/decade and its detection limit is 9 × 10⁻⁶ M. The response time of electrode is 5 min. The proposed electrode was applied successfully for the determination of cyanide in commercially available spring water. Some anions, such as SCN⁻, I⁻, Cl⁻, Br⁻ and oxalate that are usually serious interfering species for most of cyanide selective electrodes, did not have any interfering effect for this proposed electrode.     

Solvent selection in ultrasonic-assisted emulsification microextraction: Comparison between high- and low-density solvents by means of novel type of extraction vessel

There are numerous published reports about dispersive liquid phase microextraction of the wide range of substances, however, till now no broadly accepted systematic and purpose oriented selection of extraction solvent has been proposed. Most works deal with the optimization of available solvents without adequate pre-consideration of properness. In this study, it is tried to compare the performances of low- and high-density solvents at the same conditions by means of novel type of extraction vessel with head and bottom conical shape. Extraction efficiencies of seven basic pharmaceutical compounds using eighteen common organic solvents were studied in this work. It was much easier to work with high-density solvents and they mostly showed better performances. This work shows that although exact predicting the performance of the solvents is multifaceted case but the pre-consideration of initial selection of solvents with attention to the physiochemical properties of the desired analytes is feasible and promising. Finally, the practicality of the method for extraction from urine and plasma samples was investigated.     

HEXAMETHYLDISILAZANE IN THE PRESENCE OF N,N′,N″,N‴-TETRAMETHYLTETRA-2,3-PYRIDINOPORPHYRAZINATO COPPER (II) IS A NEW,MILD AND HIGHLY EFFICIENT REAGENT FOR SILYLATION OF ALCOHOLS AND PHENOLS

Alcohols and phenols are protected with hexamethyldisilazane in the presence of N,N′,N′,N?-tetramethyletra-2,3-pyridinoporphyrazinato copper (II) in good-to-excellent yields at room temperature.     

Computational Study on the Structural and Electronic Properties of Multi-Nuclear Palladium and Nickel Silyl Complexes via DFT and QTAIM Approaches

In this research, we have concentrated on the survey of ability of density functional methods and also modern semi-empirical approaches to reproduce the crystal structure of a binuclear silyl nickel complex and a trinuclear palladium silyl complex. In the structural analysis of the aforesaid nickel and palladium complexes, we have also interested to investigate the possibility of Si-Si bond formation between SiH₂ and μ-SiH moieties from the structural and electronic viewpoints. Comparison of our calculated structural parameters of aforementioned complexes with the available X-ray crystallographical data reveals that both functionals (B3LYP and M062X) can well reproduce X-ray structure of the complex with a near accuracy while the PM6-D2 semi-empirical calculated values are not in a reliable agreement with the crystallographical data. In the next step, we assessed the nature of interactions between palladium and nickel metal ions with silyl ligands via Quantum Theory of Atoms in Molecule (QTAIM) computations. Furthermore, we have analyzed the possibility of Si-Si bond formation in the aforementioned complexes by means of topological electronic indices. Strictly speaking, QTAIM calculations have been performed to explore the electronic density, its laplacian and electronic energy density at some key bond critical points to interpret the structural features of aforesaid complexes from the electronic point of view.     

Isocyanide-based four-component synthesis of ferrocenyl 1,5-disubstituted tetrazoles

A convenient four-component synthesis of ferrocenyl tetrazoles by the reaction of ferrocenecarboxaldehyde, isocyanides, azidotrimethylsilane and alkyl or aryl amines in CH₂Cl₂ at room temperature is reported.