Spectrophotometric studies on the complexation equilibria of Ni and Pb with 2-carboxy-2-hydroxy-5'-sulfo-formazylbenzene. Simultaneous determination of trace amounts of Ni and Pb

Spectrophotometric studies have been made to investigate the reaction of Nickel and Lead with 2-carboxy-2'-hydroxy-5'-sulfoformazyl-benzene (zincon) in 50%(v/v) ethanol-water at 25 degrees C and an ionic strength of 0.1 M NaClO4. A complete picture of the complexation equilibria in the pH range (4.2-12.0) for nickel and (1.9-11.5) for lead are presented. Simple, rapid, selective and sensitive methods for the spectro-photometric determination of nickel and lead has been developed based on the color reaction of their complexes with zincon. The methods allow the determination of 4.69 microg mL(-1) of nickel at pH = 6.3 (lambdamax = 665 nm) and 10.3 microg ml(-1) of lead at pH = 5.6 (lambdamax = 610 nm). The apparent molar absorptivities were epsilon = 1.3 x 10(4) L mol(-1) cm(-1) for nickel and epsilon = 0.6 x 10(4) L mol(-1) cm(-1) for lead. The interference of a large number of foreign ions and complexing agents has been studied. Thiosulphate, as masking agent allows the simultaneous determination of nickel and lead in the presence of high concentrations of copper. Ascorbic acid, sodium cyanide and or sodium fluoride provide the elimination of many other interferences. The methods have been applied successfully to the simultaneous determination of nickel and lead in an aluminium and non-ferrous alloy.     

Nano-sized Co(II)-8-hydroxyquinolate complex thin film via surface layer-by-layer chemical deposition method: Optimized factors and optical properties

An extensive study was performed and reported for evaluation and optimization of the factors affecting thin film formation of nano-sized Co(II)-8-hydroxyquinolate complex by surface layer-by-layer chemical deposition method. The formation of uniform thin films of nano-crystalline metal complex is heavily dependent on several important factors. Variation in metal and ligand concentrations (1:1–1:3) was found to show insignificant contribution to the molar stoichiometric ratio of the synthesized thin film of nano-sized Co(II)-8-hydroxyquinolate. The number of dipping cycles (2–50) was characterized by strong influence on the thin film thickness. The dependence of the immersion time (2–50 s) was proved to influence the crystal growth and homogeneity of the thin film. The role of pH of metal and ligand solutions was identified by strong contribution in development and formation of deposited Co(II)-8-hydroxyquinolate complex thin film. Finally, the role of solvent on the thin film formation was also studied and evaluated. Metal analysis, SEM, EI-MS, FT-IR and TGA were applied as monitoring techniques of these factors. The optical properties of Co(II)-8-hydroxyquinolate complex were also studied and the complex thin films were characterized by the highest optical transition from π–π* or n, π* states with energy gap in the UV-range at 3.13 eV. The lowest optical transition resulted from d–d transition or metal centered transition with energy 1.5 eV while, the optical transition at 2.35 eV is the contribution of metal ligand or ligand metal transition. In the light of the optical measurement, Co(II)-8-hydroxyquinolate complex can be considered as an organic semiconductor with the potential applications in the design of organic light-emitting diodes (OLEMs).     

Influence of Process Parameters on the Reaction Kinetics of the Chromium‐Catalyzed Trimerization of Ethylene

In this paper we report the results of an extensive experimental kinetic study carried out on the novel ethylene trimerization catalyst system, comprising the chromium source [CrCl₃(thf)₃] (thf=tetrahydrofuran), a Ph₂P‐N(iPr)‐P(Ph)‐N(iPr)H (PNPNH) ligand (Ph=phenyl, iPr=isopropyl), and triethylaluminum (AlEt₃) as activator. It could be shown that the initial activity shows a first‐order dependency on the ethylene concentration. Also, a first‐order dependency was found for the catalyst concentration. The initial activity follows a typical Arrhenius behavior with an experimentally determined activation energy of 52.6 kJ mol^?1. At elevated temperatures (ca. 80 °C), a significant deactivation was observed, which can be tentatively traced back to a ligand rearrangement in the presence of AlEt₃. After a fast initial phase, a pronounced ‘kink’ in the ethylene‐uptake curve is observed, followed by a slow, almost linear, further increase of the total ethylene consumption. The catalyst composition, in particular the ligand/chromium and the cocatalyst/chromium molar ratio, has a strong impact on the catalytic performance of the trimerization of ethylene.     

Snail Hepatopancreatic Lipase: A New Member of Invertebrates Lipases' Group

Higher animal's lipases are well characterized; however, much less is known about lipases from mollusks. A lipolytic activity was located in the land snail (Eobania vermiculata) digestive glands (hepatopancreas), from which a snail digestive lipase (SnDL) was purified. Pure SnDL has a molecular mass of 60 kDa; it does not present the interfacial activation phenomenon. It was found to be more active on short-chain triacylglycerols than on long-chain triacylglycerols. The NH₂-terminal sequence of the SnDL shows 66% of identity with the 17 NH₂-terminal amino acids of a putative lipase from sea urchin (Strongylocentrotus purpuratus). No sequence identity was found with known lipases. Interestingly, neither colipase nor bile salts were detected in the snail hepatopancreas. This suggests that colipase evolved in vertebrates simultaneously with the appearance of an exocrine pancreas and a true liver which produces bile salts. Altogether, these results suggest that SnDL is a member of a new group of digestive lipases belonging to invertebrates.     

Spectral-optical-electrical-thermal properties of deposited thin films of nano-sized calcium(II)-8-hydroxy-5,7-dinitroquinolate complex

Spectral–optical–electrical–thermal properties of deposited thin films of nano-sized calcium(II)-8-hydroxy-5,7-dinitroquinolate complex, Ca[((NO₂)₂-8HQ)₂], were explored, studied and evaluated in this work. Thin films of Ca[((NO₂)₂-8HQ)₂] were assembled by using a direct, simple and efficient layer-by-layer (LBL) chemical deposition technique. The optical properties of thin films were investigated by using spectrophotometric measurements of transmittance and reflectance at normal incidence in the wavelength range 200–2500 nm. The refractive index, n, and the absorption index, k, of Ca[((NO₂)₂-8HQ)₂] films were determined from the measured transmittance and reflectance. The real and imaginary dielectric constants were also determined. The analysis of the spectral behavior of the absorption coefficient in the intrinsic absorption region reveals a direct allowed transition with band gaps of 1.1 eV and 2.4 eV for the optical and transport energy gaps, respectively. The current–voltage characteristics of Ca[((NO₂)₂-8HQ)₂] showed a trap-charge limited conduction in determining the current at the intermediate and high bias regimes. Graphical representation of the current–voltage characteristics yields three distinct linear parts indicating the existence of three conduction mechanisms. Structural characterization and identification were confirmed by using Fourier transform infrared spectroscopy (FT-IR). Scanning electron microscopy (SEM) was also used to image the surface morphology of the deposited nano-sized metal complex and such study revealed a high homogeneity in surface spherical particle distribution with average particles size in the range 20–40 nm. Thermal gravimetric analysis (TGA) was also studied for [(NO₂)₂-8HQ] and Ca[((NO₂)₂-8HQ)₂] to evaluate and confirm the thermal stability characteristics incorporated into the synthesized nano-sized Ca[((NO₂)₂-8HQ)₂] complex.     

Spectroscopic and Conductive Properties of Some Charge Transfer Complexes of Iodine

Abstract

The interaction of iodine with donor bases such as neutral red (NR) and 1, 10 -phenanthroline (Ph) have been studied spectrophotometrically in C₂H₅OH. The results indicate the formation of 2:3 charge transfer complexes of the type (base)₂3I₂. Mass, Raman and ¹H NMR spectra have been recorded for each complex. I₃ ^? and I₂ species are observed in these complexes. In addition, the d.c. conductivity is measured in the range (300–400) K°. The energy gap of the ionic conduction has been calculated. The conduction process is thought to involve iodide transfer between polyanions.     

Tautomerism in Chlorinated O-Hydroxyschiff Bases: Effect of Chlorine Atom Substitution

The UV spectra of some chlorinated o-hydroxyschiff bases were studied in different solvents. It was found that schiff bases derived from condensation of 2-hydroxybenzaldehyde or 5-chloro-2-hydroxy benzaldehyde with substituted aniline exist as enol form, whereas schiff bases derived from the condensation of 3,5-dichloro-2-hydroxybenzaldehyde with substituted aniline exist as enol form, whereas schiff bases derived from the condensation of 3,5-dichloro-2-hydroxybenzaldehyde with aniline exist as keto form especially in dimethyl sulfoxide. The ratio of enol/keto isomers were calculated for these schiff bases.