Tetrakis(4-N,N-dimethylaminobenzene)porphyrinato]manganese(III) acetate as a novel carrier for a selective iodide PVC membrane electrode.

[5,10,15,20-Tetrakis(4-N,N-dimethylaminobenzene)porphyrinato]Mn(III) acetate (MnTDPAc) was applied as an ionophore for an iodide-selective PVC membrane electrode. The influences of the membrane composition, pH of the test solution and foreign ions on the electrode performance were investigated. The sensor exhibited not only excellent selectivity to iodide ion compared to Cl- and lipophilic anions such as ClO4- and salicylate, but also a Nernstian response with a slope of -59.4 +/- 1.2 mV per decade for iodide ions over a wide concentration range from 1.0 x 10(-2) to 7.5 x 10(-6) M at 25 degrees C. The potentiometric response was independent of the pH of the solution in the pH range of 2 - 8. The electrode could be used for at least 2 months without any considerable divergence in the potential. Good selectivity for iodide ion, a very short response time, simple preparation and relatively long-term stability were the silent characteristics of this electrode. It was successfully used as an indicator electrode in the potentiometric titration of iodide ions, and also in the determination of iodide from seawater samples and drug formulations.     

Headspace SPME–GC Method for Acetone Analysis and its Biomedical Application

A new method for extraction and analysis of acetone in human urine based on headspace solid phase microextraction using a mixture of activated carbon and zeolite as sorbents in a PVC matrix coated on a silver wire and its application to the determination of ketone bodies is described. Unlike commercial fibers, which are coated on fused silica, the coating adheres strongly to the silver wire and is thermally stable up to 250 °C. After optimization of coating composition and microextraction conditions the fiber was used for the analysis of acetone in human urine.     

Metal-Assisted Oxidative Cyclization of Arylamidrazones I. Synthesis of 3-Acetyl-1,4-dihydro-1-phenyl-1,2,4-benzotriazine

In the presence of RuCl₃, N-phenylamidrazone underwent oxidative cyclization into 1,4-dihydro-1-phenyl-1,2,4-benzotriazine, the structure of which is established by spectral and X-ray diffraction data.     

The vapour pressures and saturated volumes of benzotrifluoride in the temperature range 460–530K.

A sample of benzotrifluoride was degassed in a high vacuum train, and the vapor pressure was measured in the temperature range 460 – 53OK. Also the saturated vapour and saturated liquid volumes were measured. Two simple equations were used to fit the vapour pressure data by the least square method. The heat of vaporization was calculated using Clapeyron equation.     

New many fold 1,2,3‐selenadiazole aromatic derivatives

The many fold aromatic ketones 2a‐d are versatile compounds for the synthesis of the many fold 1,2,3‐selenadiazole aromatic derivatives 5a‐d . The preparation starts with the reaction between the many fold bromomethylene benzene derivatives 1a‐d and 4‐hydroxyacetophenone, which are transformed through the reaction with semicarbazide hydrochloride or ethylhydrazine carboxylate into the corresponding semicarbazones derivatives 3a‐d or hydrazones 4a‐d . The reaction with selenium dioxide leads to regiospecific ring closure of semicarbazones or hydrazones to give the many fold 1,2,3‐selenadiazole aromatic derivatives in high yield.     

Zein film as a novel natural biopolymer membrane in electrochemical detections

Permselective modifier films are very important in preparing highly sensitive electrochemical sensors. In this work, for the first time, the behavior of gold and glassy carbon electrodes coated with biocompatible zein film as a permselective membrane for the electrochemical detection of various compounds has been investigated. For this purpose, several electroactive cationic (methylene blue, brilliant green, and thionine) and anionic (potassium ferricyanide, alizarin red S, and riboflavin-5’-phosphate) compounds have been used as model. Atomic force microscopy (AFM) and scanning electron microscopy (SEM) showed that zein membranes prepared from casting solution containing 1% zein in ethanol/water have porous structures with high nanometric roughness. The capacitance values of electrical double layers of electrodes modified with zein film were very high for hydrophilic ions in comparison with hydrophobic ions. Point of zero charge pH (pH_pzc) of zein membrane was 4.8. The results of cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) as well as pH_pzc study indicated that zein permselective membrane acts as ion exchanger film for selected cationic compounds with fast electrochemical kinetics responses in aqueous solution (pH=7). This behavior was confirmed by circulating solutions containing model compounds from homemade continuous cell equipped with polyamide membranes modified with zein film.

Graphical Abstract

     

Gamma-irradiation effects on the electrical conductivity of pure and Cu-doped Fe3O4 spinel

The electrical conductivity and IR-spectra of pure and Cu-doped Fe₃O₄ spinels were measured at 300–1000 K. Two breaks in the conductivity-temperature curves have been observed for all investigated pure and doped samples. One of these two breaks were found near the Curie point of the investigated spinel. The electrical conduction in -irradiated and non-irradiated pure and Cu-doped Fe₃O₄ occurred by a hopping mechanism due to a fast electron exchange between Fe²⁺ and Fe³⁺-ions present on octahedral sites. The Seebeck-voltage of the irradiated and non-irradiated pure and Cu-doped samples has been measured. The effect of -irradiation on the conductivity values //, activation energy and type of defects was discussed.     

Investigation on corrosion inhibition and adsorption mechanism of azomethine derivatives at mild steel/0.5 ​M ​H2SO4 solution interface: Gravimetric,electrochemical, SEM and EDX studies

The inhibition performance of five azomethine derivatives such as: 1-(4-Methyloxy phenylimino)-1-(phenylhydrazono)-propan-2-one (SB₁), 1-(4-Methylphenylimino)-1-(phenylhydrazono) propan-2-one (SB₂), 1-(phenylimino)-1(phenylhydrazono)-propan-2-one (SB₃), 1-(4-Bromo phenylimino)-1(phenylhydrazono)-propan-2-one (SB₄) and 1-(4-Chlorophenylimino)-1(phenylhydrazono) -propan-2-on (SB₅) as corrosion inhibitors for mild steel in sulfuric acid 0.5 ?M were investigated using different methods. All experimental results demonstrate that these compounds are eficients inhibitors. The inhibition efficiencies ($IE$) increase with inhibitors concentration. At 7.5 $\times$ 10^?5 ?M, the $IE$ was 97.27%, 96.31%, 94.23%, 93.19 and 91.64% for SB₁, SB₂, SB₃, SB₄ and SB₅, respectively. The potentiodynamic polarization results indicated that all the studied inhibitors act as mixed type. The adsorption process on mild steel surface obeyed Langmuir isotherm. The associated activation parameters and thermodynamic have been calculated and discussed. The adsorbed film formed on the metal surface was characterized by SEM and EDX.     

Ketoconazol‐Triiodide Ion Pair Complex as a Suitable Carrier in an Iodide Selective Membrane Electrode

A novel membrane sensor for selective monitoring of iodide, consisting of a triiodide‐ketoconazole ion pair complex dispersed in a PVC matrix, plasticized with a mixture of 2‐nitrophenyl octyl ether and dioctylphtalate with unique selectivity toward iodide ions, is described. The influence of membrane composition, pH of test solution and foreign ions on the electrode performance were investigated. The optimized membrane demonstrates a near‐Nernstian response for iodide ions over a wide linear range from 1.0 × 10^?2 to 1.0 × 10^?5 M, at 25 ± 1 °C. The electrode could be used over a wide pH range 3–10 and has the advantages of high selectivity, fast response time and good lifetime (over 4 months). It was successfully used as indicator electrode in potentiometric titrations and direct potentiometric assay of iodide ions.     

Observation on Symmetry Properties of Sodium Zinc(II)-2,9,16,23-phthalocyanine Tetracarboxylate in Water:NaOH Solution

The shift of the Q-band of sodium zinc(II)-2,9,16,23-phthalocyanine tetracarboxylate (ZnPc(COONa)₄) to about 800 nm is attributed to the influence of the electron-donating property of the carboxylate groups substituted in the β–position. ZnPc(COONa)₄ which was found to have a symmetry of D _2h characterized by a splitting of the Q transition. This splitting was interpreted by the formation of dianionic symmetric ZnPc(COONa)₄ resulting from the dissociation of the pyrrole protons as well as the possibility of Na⁺ dissolution of ZnPc(COONa)₄ in the aqueous solution of NaOH.