New copper(II) complexes produced by the template reaction of acetoacetic-2-pyridylamide and amino-aliphatic alcohols

The template condensation of acetoacetic-2-pyridylamide with amino aliphatic alcohols such as 2-aminoethanol (HL1) and 3-amino propanol (HL2) in the presence of copper(II) ions gave octahedral complexes, which have been characterized by elemental analyses, u.v.-vis. and i.r. spectra, conductivity, d.t.a, magnetic and e.s.r. measurements. The molar conductance in DMF indicate that the complexes are non-ionic in character. The e.s.r. spectra of solid complexes (2) and (5) at room temperature indicate axial type symmetry (dx2-y2) with covalent bond character.     

Study of the dehydration of Portland Cement by Mössbauer spectrometry

Egyptian Portland Cement in the form of one inch cube was hydrated at different times of hydration. Nine cubes of each period of hydration were heated for five minutes 200, 300, 400 up to 1000°C then were quenched in air. The compressive strength was measured for these samples and related to unheated ones. These cubes were ground and measured by Mössbauer spectrometry to correlate the effect of dehydration of cement pastes on the states of iron, with the decrease of compressive strength. It was observed that starting from 400°C the central doublet characteristic of the hydration process decreased as the dehydration temperature was increased. At 1000°C the dehydration process was complete, the central doublet disappeared and the compressive strength vanished. The hydration process was found to be reversible. The application of Mössbauer spectrometry to estimate the degree of fire in concrete building was demonstrated.     

Mössbauer study of iron reduction in hematite containing mineral originated from Aswan area in Egypt

Mössbauer spectroscopy was used to study iron reduction in mineral originated from Aswan area in Egypt. The Mössbauer spectra of samples heat treated at 1000 °C in hydrogen atmosphere show a gradually reduction process of hematite. The main phase of sample aged for 1 h is magnetite, while alpha-iron as well as some silicates and wustite type oxide can be detected in sample aged for 3 h. Further aging of sample results in dissolution of alloying elements /Si, Al/, being present in the samples. This process starts already in samples aged at 1000 °C for 4 h, but it is more expressive in minerals heat treated at 1200 °C or 1300 °C, when all paramagnetic phases disappeared.     

Thermal Study of the Cr-Mo-O System in Air

The phase diagram of the ternary system Cr-Mo-O in air was established from the results of thermal analysis of mixtures with different initial CrO3 to MoO3 ratios. It was found that MoO3 did not take any chromium oxide into solid solution. The presence of Cr2O3 destabilized MoO3 causing it to decompose to MoO2 in the temperature range 723-958 K depending on the initial Cr/Mo ratio. The decomposition of pure MoO3 MoO2 did not occur in air at any temperature. However, this decomposition took place through the formation of the compound Cr2O3·3MoO3(ss) and its decomposition to Cr2O3·3MoO2(ss). The latter compound has never been reported before and the X-ray data for this compound are given. The previously reported catalytic activity of Cr2O3·3MoO3(ss), at high temperatures, is presumably due to its reduction to Cr2O3·3MoO2(ss). This revised version was published online in July 2006 with corrections to the Cover Date.     

UV-vis, IR and 1H NMR spectroscopic studies of some mono- and bis-azo-compounds based on 2,7-dihydroxynaphthalene and aniline derivatives

The absorption spectra of mono- and bis-azo-derivatives obtained by coupling the diazonium salts of aromatic amines and 2,7-dihydroxynaphthalene have been studied in six organic solvents. The different absorption bands have been assigned and the effect of solvents on the charge transfer band is also discussed. The diagnostic IR spectral bands and 1H NMR signals are assigned and discussed in relation to molecular structure. Also, semi-empirical molecular orbital calculations using the atom superposition and electron delocalization molecular orbital (ASED-MO) theory have been performed to investigate the molecular and electronic structures of these compounds. According to these calculations, an intramolecular hydrogen bonding is essential for stabilization of such molecules.     

Novel Cyanine Dyes: Synthesis,Characterization and Photosensitization‐Structure Correlation

Novel furo, thieno and pyrrolo[2,3‐b]pyrazole cyanine dyes were synthesized. The structure‐photosensitization properties correlation of the dyes were examined in 95% ethanol solution by absorption spectroscopy. The chemical structure of the starting biheterocyclic compounds and their derived cyanine dyes were confirmed by elemental analysis, IR and ¹H NMR spectroscopy.     

Glycosidases of turnip leaf tissues

Four myrosinase (β-thioglucosidase EC. 3.2.3.1) and seven disaccharase (β-fructofuranosidase, EC. 3.2.1.26) isoenzymes were isolated from turnip leaves. The most active enzymes were isolated in pure form. Myrosinase and disaccharase mol wt was 62.0 × 10³ and 69.5 × 10³ dalton, respectively, on the basis of gel filtration on Sephadex G-200. Myrosinase pH profile showed high activity between pH 5 and 7 with the optimum at pH 5.5. The purified enzyme was heat-stable for 60 min at 30°C with only loss of 24% of activity. Its activity is strongly inhibited (100%) by Pb²⁺, Ba²⁺, Cu²⁺ and Ca²⁺ ions, and activated (70%) by EDTA at 0.04M. The pure enzyme failed to hydrolyze amylose, glycogen, lactose, maltose, and sucrose. TheK _m andV _max values of myrosinase using sinigrin as specific substrate was 0.045 mM and 2.5 U, respectively. The maximal activity of disaccharase enzyme was obtained at pH 4–5 and 35–37°C. The enzyme was heat-stable at 30°C for 30 min with only 10% loss of its activity. Its activity is strongly activated (70–240%) by Ca²⁺, Ba²⁺, Cu²⁺, and EDTA at 0.01M. The enzyme activity is specific to the disaccharide sucrose and failed to hydrolyze other disaccharides (maltose and lactose). TheK _m andV _max of disaccharase were 0.123 mM and 3.33 U, respectively.     

Polymer-Mercury Coated Screen-Printed Sensors for Electrochemical Stripping Analysis of Heavy Metals

In the perspective of in-field stripping analysis of heavy metals, the use and disposal of toxic mercury solutions (necessary to plate a mercury film on a carbon electrode surface) presents a problem. The aim of this work was the development of mercury coated screen-printed electrodes previously prepared in the lab and ready to use in-field. Thus some commercially available polymers like Nafion®, Eastman Kodak AQ29®, and Methocel® were investigated as mercury entrapping systems for electrochemical stripping analysis of heavy metals. Screen-printed disposable cells with a silver pseudo-reference electrode, a graphite counter electrode, and a graphite working electrode were used. To modify the sensor, the polymer solution was cast onto the carbon working electrode surface. Detection limits of 0.8 and 1 μg/L were obtained for lead and cadmium respectively. Since Methocel® based electrodes showed the best performance, they were used for the analysis of real samples. The results were compared with those obtained using a classical thin mercury film electrode and ICP spectroscopy.

All the experiments reported here were performed in un-deareated solutions as required for in-field analysis.