Determination of selenoamino acids by gas chromatography-mass spectrometry

The application of the recently introduced ethylchloroformate derivatization method for the separation and determination of selenomethionine and selenocystein in selenium-enriched yeast and yeast-free tablets by means of a gas chromatography-mass spectrometry (GC-MS) system has been studied. The efficiency of three methods for the extraction of selenomethionine from the tablets were compared. Total selenium content of the same tablets were measured using inductively coupled plasma (ICP)-MS and it was found that in the selenized yeast tablets about 80% of the total selenium is present as selenomethionine. The results were in agreement with the values in the labels and with the literature. The accuracy of the total selenium analysis was controlled by the analysis of a reference material.     

Levels of natural and artifical radioactivity in sediments in the Eastern Black Sea of Turkey

Sediment samples collected from the Eastern Black Sea in 1993 from 15 sampling stations of different depths have been analyzed. Natural and artifical radionuclide activity levels in offshore sediment samples from the Eastern Black Sea in Turkey are reported about seven years after the Chernobyl accident. The purpose of this paper is to follow up the earlier study and present results for the distributions of radionuclides in sediments of the Black Sea.     

Porous structure of synthetic opals

Some adsorption, structural, and annihilation characteristics of synthetic opals are measured. An analysis of these characteristics makes it possible to conclude that the total porosity in opals comprises macropores, which are in essence the voids between structure-forming spheres, and nanopores connected to the substructure of the spheres. The systems of macropores and nanopores are separated by narrow channels that collapse upon the thermal treatment of opals. The sizes of primary a-SiO₂ particles and nanopores, which correspond to the voids between these particles, are estimated.     

Effect of operating parameters on selective separation of heavy metals from binary mixtures via polymer enhanced ultrafiltration

Performance of continuous polymer enhanced ultrafiltration (PEUF) method was investigated for removal of mercury and cadmium from binary mixtures. This method includes the addition of polyethyleneimine (PEI) as a water soluble polymer to bind the metals, which was followed by ultrafiltration operation performed on both laboratory and pilot scale systems. The influence of various operating parameters such as temperature, metal/polymer ratio, presence of calcium ions and pH on retention of metals and permeate flux was investigated. To investigate the possibility of selective separation of mercury and cadmium, experiments were conducted for binary solutions at different pH and loading ratios. It was seen that the retention of mercury decreased and permeate flux increased when the temperature increased. The increased pH and decreased metal/polymer ratio, loading (L), resulted in higher retention of both metals. Shapes of retention vs. pH or L curves were very similar for both metals. Retentions stay almost constant at a value very close to unity until a critical L or pH value was reached, then, R decreases almost linearly with L or pH. However, retention of cadmium was affected more than that of mercury as the pH decreased and L increased. This leads to the selective separation of mercury and cadmium. At low pH values (about 5) and at high L values (about 0.3), mercury was removed by ultrafiltration operation while almost all cadmium passed through the membrane. At pH 5.5 and cadmium/polymer ratio about 0.35 and mercury/polymer ratio about 0.39, the highest separation factor was obtained as 49.     

Layer arrangement in the structure of octakis-(trimethylsiloxy)octasilsesquioxane and dodecakis-(trimethylsiloxy)cyclohexasiloxane

Layers of [(CH₃)₃SiO]₈(SiO_1.5)₈ and [(CH₃)₃SiO]₁₂(SiO)₆ organosilicon compounds obtained by chemical vapor deposition were investigated by X-ray diffraction (DRON-RM4, R = 192 mm, CuK radiation) and Raman spectroscopy (Triplemate, SPEX). The layers were found to be ideally oriented polycrystalline films. The octakis-(trimethylsiloxy)octasilsesquioxane polycrystals are oriented in one crystallographic direction — [001], while the dodecakis-(trimethylsiloxy)cyclohexa-siloxane polycrystals are oriented in the and directions. Crystal structure analysis in these directions yielded the type of the planar lattice followed by the molecules and their orientation relative to the support.Original Russian Text Copyright © 2004 by S. A. Gromilov, T. V. Basova, D. Yu. Emelyanov, A. V. Kuzmin, and S. A. ProkhorovaTranslated from Zhurnal Strukturnoi Khimii, Vol. 45, No. 3, pp. 497–501, May–June 2004.     

Ascorbic acid as a potential masking agent in the tanning process. Olated chromium complexes involving ligating ascorbate and bridging sulfate groups

Two polynuclear complexes, a dimer and a tetramer, involving sulfate and hydroxo bridges and ligating ascorbate were isolated from aqueous solutions. Structural formulae are proposed on the basis of microanalytical and thermal analysis results, i.r., ¹³C-n.m.r., mass spectral data and magnetic measurements.     

Spectrophotometric determination of samarium(III) with chrome azurol S in the presence of cetylpyridinium chloride

A sensitive, simple method for the determination of trace amounts of samarium by spectrophotometry is described based on the formation of the samarium-chrome azurol S (CAS) complex in micellar medium. The molar absorptivities of the complexes at pH 7.5 at 505 nm were 3.6x10(4) and 1.4x10(5) l mol(-1) cm(-1) for water media and cetylpyridinium chloride (CPC), respectively. Beer's law is obeyed from 0.05-2 mg l(-1) of samarium at 505 nm as Sm-CAS-CPC complex. Optimal conditions such as reagent amounts, and pH for the samarium determination were reported. The effects of foreign ions were also investigated. The proposed method was successfully applied to the determination of samarium contents in synthetic samples.     

Surface Characterization of Sepiolite by Inverse Gas Chromatography

Inverse gas chromatography (IGC) was applied to characterize the surface of sepiolite. The adsorption thermodynamic parameters (the standard enthalpy (ΔH ⁰), entropy (ΔS ⁰) and free energy of adsorption (ΔG ⁰)), the dispersive component of the surface energy (γ _S ^d ), and the acid/base character of sepiolite surface were estimated by using the retention time of different non-polar and polar probes at infinite dilution region. The specific free energy of adsorption (ΔG ^sp ), the specific enthalpy of adsorption (ΔH ^sp ), and the specific entropy of adsorption (ΔS ^sp ) of polar probes on sepiolite were determined. ΔH ^sp were correlated with the donor and modified acceptor numbers of the probes to quantify the acidic K _A and the basic K _D parameters of the sepiolite surface. The values obtained for the parameters K _A and K _D indicated an acidic character for sepiolite surface.     

Methodological modifications on quantification of phosphatidylethanol in blood from humans abusing alcohol,using high-performance liquid chromatography and evaporative light scattering detection

Background  

Phosphatidylethanol (PEth) is an abnormal phospholipid formed slowly in cell membranes by a transphosphatidylation reaction from phosphatidylcholine in the presence of ethanol and catalyzed by the enzyme phospholipase D. PEth in blood is a promising new marker of ethanol abuse depending on the high specificity and sensitivity of this marker. None of the biological markers used in clinical routine at the present time are sensitive and specific enough for the diagnosis of alcohol abuse.