Mössbauer spectroscopic study of FeAl1−x Co x

We report the results of a Mössbauer study of the alloy sytem FeAl_1?x Co _x forx ≥ 0.3 at temperatures down to 83 K. Magnetic splitting is observed forx ≥ 0.35 at all temperatures. However, forx=0.3, no splitting is observed at room temperature, and superparamagnetic behavior occurs at LN₂ temperature. The magnetically split spectra are fitted each with a distribution of hyperfine fields and the average hyperfine field \(\bar B_{hf} \) as a function of temperature is obtained. The variation of \(\bar B_{hf} \) withT is explained using the model of magnetic clusters with collective magnetic excitations from which the saturation hyperfine field and the magnetic anisotropy energy for these clusters are obtained. Also, the results are discussed using the model of random atomic distributions, and the agreement between the calculated and the experimentally obtained distributions of hyperfine fields is found improve asx increases.     

Micellization of styrene/butadiene/styrene block copolymers in mixed solvents

Dilute solutions of three block copolymers, styrene/butadiene/styrene in the mixed selective solvents dioxane/different alcohols is studied at different temperatures. The molecular weight, second virial coefficient and radius of gyration in all selective solvents are also determined. From these measurements it is concluded that a maximum in the dissymmetry of the system for all the selective solvents used is observed. This maximum is observed at higher temperatures for concentrated solutions. Similarly, this maximum is also shifted to lower temperature by using strong precipitants in selective solvents. The milky opalescence is observed for all the selective solvents either by lowering the temperature of the system or by increasing the ratio of the precipitant in the selective solvent.     

N-methylpyrrolidine as an effective organocatalyst for the regioselective synthesis of 3-hydroxy-3,5/6-di-aryl-1H-imidazo[1,2-a]imidazol-2(3H)-ones

N-Methylpyrrolidine catalyzed, concise and attractive synthesis of a new class of 3-hydroxy-3,5/6-di-aryl-1H-imidazo[1,2-a]imidazol-2(3H)-ones was attained with impressive yields, in the presence of EtOH as a solvent, by means of a convenient and elegant condensation reaction between different aryl glyoxal monohydrates and guanidine hydrochloride under reflux conditions. Some specific merits of the current procedure, including encompasses low operating cost, availability of the starting substrates, reasonable reaction times, high reaction yield, operational simplicity, cleaner reaction profile, no harmful by-products, and the isolated product is in pure form. Structures of all the freshly synthesized products have been deduced by their FT-IR, ¹H-NMR, ¹³C-NMR, Mass spectrometry data and microanalysis.

Graphical abstract

     

Impedimetric sensing of uranyl ion based on phosphate functionalized cysteamine self-assembled monolayers

A phosphate functionalized cysteamine self-assembled monolayer based on gold electrode is designed for uranyl ion (UO₂²⁺) detection. The response of the modified electrode is studied by electrochemical impedance spectroscopy (EIS) and cyclic voltammetry. The EIS data are approximated using constant phase element (CPE) model from which kinetic and analytical parameters are evaluated. Uranyl ion is recognized based on blocking effect against charge transfer between p-benzoquinone as a probe and the modified electrode. This effect is detected from linear variation of charge transfer resistance (R_ct) as a function of UO₂²⁺ concentration. From the analysis of the EIS data and approximated parameters, a method is developed for UO₂²⁺ determination based on impedimetric measurements.     

Cathodic stripping voltammetric determination at a hanging mercury drop electrode of the environmental heavy metal precipitant trimercapto-s-triazine (TMT)

Trimercapto-s-triazine (TMT) is available commercially for precipitating heavy metals in effluents prior to discharge and for recovering silver and copper. The TMT content of an effluent for discharge is normally monitored down to about 2 ppm by means of its UV absorption at 285 nm. Indirect cathodic-stripping voltammetric methods of determining TMT at sub-ppb levels in standard solutions are reported here. These methods might prove suitable for the determination of TMT in effluent at levels lower than is currently possible. TMT can be accumulated and determined indirectly at pH 9.0 as its mercury salt down to sub-ppb levels. Accumulation is made at 0 V and the mercury TMT reduction peak is at -0.47 V. Alternatively, by adding nickel(II), TMT can be determined optimally at pH 7.8, using the catalytic nickel peak at -0.73 V and accumulating between -0.10 and -0.60 V: at this pH the HgTMT peak at -0.47 V is small. At slightly higher pH (pH 8.6) the nickel TMT complex can be accumulated directly at -0.40 V, but at this pH, however, a slightly increased sensitivity can be achieved by accumulating TMT as its mercury salt, at -0.1 V in the presence of nickel(II), the nickel TMT complex being formed during the potential sweep on the release of the TMT when the mercury salt is reduced. Unlike many other thiols TMT is not accumulated as its copper(I) salt on addition of copper(II) to the solution.     

Correlation of the physicochemical properties of symmetric 1,3-dialkoylamidopropane-based cationic lipids containing single primary and tertiary amine polar head groups with in vitro transfection activity

The physicochemical properties of a novel series of symmetric 1,3-dialkylamidopropane-based cationic amphiphiles [M. Sheikh, J. Feig, B. Gee, S. Li, M. Savva, In vitro lipofection with novel series of symmetric 1,3-dialkoylamidopropane-based cationic surfactants containing single primary and tertiary amine polar head groups, Chem. Phys. Lipids 124 (2003) 49-61] were studied by several techniques, in an effort to correlate cationic lipid structure with transfection efficacy. It was found that only the unsubstituted amine and tertiary amine dioleoyl derivatives 1,3lmp5 and 1,3lmt5, respectively, mediated in vitro transfection activity in the absence of helper lipids. This activity pattern was consistent with ethidium bromide fluorescence quenching studies, which indicated that only these two derivatives bound to and efficiently condense plasmid DNA at physiological pH. Dynamic light scattering indicated that lipoplexes made by these two cationic lipids were relatively small particles below 1 microm, in sharp contrast to lipoplexes bigger than 3 microm composed of saturated cationic derivatives. Transmission electron microscopy studies clearly indicated that cationic lipid dispersions made by saturated derivatives form multilamellar tubules at physiological pH. Calorimetric studies showed that cationic amphiphiles with saturated acyl chains longer than 12 carbons exhibit solid-to-liquid crystalline phase transitions above 37 degrees C. In agreement with the microscopy and calorimetry studies, Langmuir film balance experiments indicated that saturated derivatives with hydrophobic chains longer that 12 carbons are not well hydrated and exist at a chain-ordered state at ambient temperature. Calculation of compressibility moduli from monolayer compression isotherms at 23 degrees C suggested that monolayers made by cationic lipids bearing saturated acyl chains are less compressible relative to those of the dioleoyl derivatives 1,3lmp5 and 1,3lmt5. In conclusion, high hydration, increased fluidity and high elasticity of cationic lipid assemblies in isolation, all correlate with high in vitro transfection activity.     

Application of thermal desorption to the development of a gas chromatographic/mass spectrometric method for the determination of toluene,chlorinated aromatic hydrocarbons,and 2,3,7,8-tetrachlorodibenzo-p-dioxin in combustion emissions

A fast and accurate analytical method, which uses commercially available adsorbents (Tenax TA, Carbotrap B and C, and Carbosieve S-III), was developed for the sampling and determination of aromatic hydrocarbons, chloroaromatic compounds, and 2,3,7,8-tetrachlorodibenzo-p-dioxin. The breakthrough volume data show that Carbotrap C has a good capacity for compounds of high molecular weight, whereas Carbosieve S-III and Tenax TA are efficient for volatile compounds. The organic components are thermally desorbed and transferred to a gas chromatograph/mass spectrometer. Importantly, thermal desorption avoids conventional solvent extraction procedures and also allows reuse of adsorbent tubes. Preliminary results for recovery of analytes from tubes packed with single adsorbent prove that a single-adsorbent bed is not capable of sampling a wide range of compounds. The best method to obtain the desired collection and desorption properties is to use adsorbent tubes containing several different materials. The results of optimization studies are summarized.     

Spectrophotometric Determination of Prochlorperazine Maleate in Pure and Pharmaceutical Preparations

 Prochlorperazine maleate reacts with 1-naphthylamine and sodium nitrite, after heating for 110 s at 80 °C to give an orange red colour having maximum absorbance at 460 nm. The reaction is selective for prochlorperazine maleate with 0.01 mg/mL as visual limit of quantitation and provides a basis for a new spectrophotometric determination. The colour reaction obeys Beer’s law from 0.01 mg/10 mL to 0.33 mg/10 mL of prochlorperazine maleate and the relative standard deviation is 0.68%. The quantitative assessment of tolerable amounts of other drugs is also studied. Received September 22, 2000. Revision June 19, 2001     

Electrochemical Behavior and Determination of Hyoscine‐N‐Butylbromide from Pharmaceutical Preparations

The electrooxidation of hyoscine N‐butylbromide (HBB) was investigated by rotating disk electrode voltammetry, cyclic voltammetry and controlled potential coulometry in 0.1 M HNO₃ and in 0.1 M tetrabutylammonium perchlorate (TBAP) solutions of acetonitrile at a platinum (Pt) electrode. Based on the results obtained, it is suggested that a bromide ion of HBB was oxidized in one reversible step in aqueous solutions and in two reversible steps in acetonitrile. A differential pulse voltammetric (DPV) method at a Pt electrode was developed for the determination of HBB in the concentration range of 1.0 × 10^?6‐1.0 × 10^?3 M. The procedure was applied to the determination of HBB in its formulations as well as its recovery from blood serum and urine samples.