Spectrophotometric microgram determination of copper in organic compounds by wet or oxygen flask combustion

Summary Spectrophotometric Microgram Determination of Copper in Organic Compounds by Wet or Oxygen Flask Combustion A spectrophotometric method for the microgram (2–30 ppm) determination of copper in organic compounds after wet digestion or oxygen flask combustion has been developed. The copper content is determined through the formation of the molybdenum blue complex, which is formed by the addition of 1 ml of each of 1% KCN, 1% phosphomolybdic acid and 1M HCl solutions, in the order mentioned. The absorbance is measured at 725 nm. A series of 10 compounds with 10–40% copper gave highly satisfactory results. The total average error is ±0.05% and the overall standard deviation value is 0.220. The method described is rapid, simple and accurate; the reagents required are cheap and readily available.     

Streptomyces griseus KJ623766: A Natural Producer of Two Anthracycline Cytotoxic Metabolites β- and γ-Rhodomycinone

Background: This study aimed to produce, purify, structurally elucidate, and explore the biological activities of metabolites produced by Streptomyces (S.) griseus isolate {"type":"entrez-nucleotide","attrs":{"text":"KJ623766","term_id":"655350460"}}KJ623766, a recovered soil bacterium previously screened in our lab that showed promising cytotoxic activities against various cancer cell lines. Methods: Production of cytotoxic metabolites from S. griseus isolate {"type":"entrez-nucleotide","attrs":{"text":"KJ623766","term_id":"655350460"}}KJ623766 was carried out in a 14L laboratory fermenter under specified optimum conditions. Using a 3-(4,5-dimethylthazol-2-yl)-2,5-diphenyl tetrazolium-bromide assay, the cytotoxic activity of the ethyl acetate extract against Caco2 and Hela cancer cell lines was determined. Bioassay-guided fractionation of the ethyl acetate extract using different chromatographic techniques was used for cytotoxic metabolite purification. Chemical structures of the purified metabolites were identified using mass, 1D, and 2D NMR spectroscopic analysis. Results: Bioassay-guided fractionation of the ethyl acetate extract led to the purification of two cytotoxic metabolites, R1 and R2, of reproducible amounts of 5 and 1.5 mg/L, respectively. The structures of R1 and R2 metabolites were identified as β- and γ-rhodomycinone with CD₅₀ of 6.3, 9.45, 64.8 and 9.11, 9.35, 67.3 µg/mL against Caco2, Hela and Vero cell lines, respectively. Values were comparable to those of the positive control doxorubicin. Conclusions: This is the first report about the production of β- and γ-rhodomycinone, two important scaffolds for synthesis of anticancer drugs, from S. griseus.     

Co-substitution effect on the structural,electrical, and electrochemical properties of nanostructured Co<Subscript>x</Subscript>Ni<Subscript>1-x</Subscript>MnP<Subscript>2</Subscript>O<Subscript>7</Subscript> (x = 0, 0.25, 0.5, and 0.75)

Cobalt-nickel-manganese pyrophosphate nanostructures with formula Co_xNi_1-xMnP₂O₇ were prepared via the hydrothermal method at 150 °C, with further calcinations at 500 °C. A structural analysis of Co_xNi_1-xMnP₂O₇ samples was carried out using X-ray diffraction (XRD). The effect of Co substitution on the structural, electrical, and electrochemical properties of Co_xNi_1-xMnP₂O₇ is reported. The electrochemical results show that the specific capacity increases from 59 to 205 mAh/g with increasing Co content. This study demonstrates the Co substitution effect on the mixed electrical conductivity. The temperature dependence of the dc electrical conductivity, for both pure and Co²⁺-doped samples, obeys the Arrhenius law. The frequency dependence of ac conductivity for the materials exhibited a Jonscher’s universal power law. The plots of pre-exponent (n) versus temperature suggested that the conduction mechanism can be described using correlated barrier hopping model. The improved electrical conductivity and electrochemical proprieties of Co_xNi_1-xMnP₂O₇ nanomaterials could be ascribed to the synergistic effect of nickel and cobalt ions. The best results have been obtained for the composition x(Co) = 0.75, where the electrical conductivity is maximum, and the Co_0.75Ni_0.25MnP₂O₇ demonstrates the highest specific capacity, implying their promising potential applications in the energy storage.     

A laser extraction/combustion technique for in situ delta(13)C analysis of organic and inorganic materials

A CO(2) laser extraction system is described for in situ delta(13)C analysis of organic and inorganic materials. Carbonaceous compounds volatilized by the laser are quantitatively converted to CO(2) gas by a combustion furnace mounted after the sample chamber. Gases produced by the laser and combustion processes are swept by helium carrier gas and separated by a packed gas chromatography column prior to their introduction to an isotope ratio monitoring mass spectrometer. A sample of lentil bean was analyzed at a spatial resolution of 200 μm and yielded delta(13)C values with precision of +/- 0.3 per thousand. The accuracy of delta(13)C measurements was better than +/- 0.5 per thousand from NBS 22 (mineral oil), USGS 24 (graphite), and IAEA CO-1 (calcium carbonate). Copyright 1999 John Wiley & Sons, Ltd.     

Benzothiophene Adsorptive Desulfurization onto trihexYl(tetradecyl)phosphonium Dicyanamide Ionic-Liquid-Modified Renewable Carbon: Kinetic,Equilibrium and UV Spectroscopy Investigations

The negative environmental and industrial impacts of the presence of sulfur compounds such as benzothiophene in fuels have led to a greater interest in desulfurization research. In this work, carbon from palm waste sources was modified with trihexYl(tetradecyl)phosphonium dicyanamide-ionic liquid and characterized by SEM, EDS, XRD and FTIR to assess surface properties. Then, the prepared carbon and carbon modified with ionic liquid were evaluated for the adsorption of benzothiophene by investigating the effects of time. The equilibrium occurred after 120 min, recording adsorption capacities of 192 and 238 mg/g for carbon and carbon modified with ionic liquid, respectively. The effect of the adsorbent dose on the adsorption of benzothiophene was evaluated, indicating that the maximum adsorption capacities were obtained using a dose of 1 g/L for both carbon and carbon modified with ionic liquid. The kinetic investigation for the adsorption of benzothiophene onto carbon and carbon modified with ionic liquid indicated that the second-order kinetic model is well fitted with the adsorption data rather than the first-order kinetic model. The equilibrium investigations for the adsorption of benzothiophene onto carbon and carbon modified with ionic liquid with Langmuir and Freundlich isotherm models reveals that the Freundlich model is the most suitable for describing the adsorption process, suggesting a multilayer adsorption mechanism. The desulfurization process showed a high impact on environmental safety due to the possibility of regenerating and reusing the prepared adsorbents with promising results up to five cycles.     

Photooxidation of poly(N-vinylpyrrolidone) (PVP) in the solid state and in aqueous solution

The photooxidation of poly(N-vinylpyrrolidone) (PVP) in the solid state and in an aqueous solution has been studied under irradiation at long wavelengths (at λ ≥ 300 nm) and in the presence of oxygen, as these conditions of irradiation are those of natural outdoor aging. Infrared spectroscopy was used to follow the photochemical evolution of the polymer either for solid films of PVP or for PVP irradiated in an aqueous solution. Chemical treatments (NH₃, SF₄) were carried out on the photooxidized samples, and aqueous solutions of PVP were characterized by viscometry and size exclusion chromatography (SEC). Based on photooxidation results obtained in both the solid state and in an aqueous solution, a general mechanism that accounts for the main routes of oxidation is proposed. It was shown that the rates of oxidation and the stoichiometries of the reactions were strongly influenced by the physical state of the polymer (solid state or aqueous solution).     

Microdetermination of α-amino acids by colorimetry and atomic absorption spectrophotometry

The present work describes two simple, rapid, sensitive, and reliable methods for the determination of α-amino acids after conversion to their corresponding Cu(II) chelates. In the first method, the copper complex is treated with cyanide and phosphomolybdic acid in HCl medium followed by colorimetric measurement of the molybdenum blue produced. In the second method, the absorbance of the copper chelate is directly recorded on aspiration in the atomic absorption spectrophotometer. A variety comprising 9–10 α-amino acids were successfully determined by each of the two methods with average errors not exceeding ±0.30 and ±0.18%, respectively.     

Peculiar reduction of graphene oxide into graphene after diffusion in exponentially growing polyelectrolyte multilayers

In the present work, in situ reduction of graphene oxide (GO) into graphene was preformed, after diffusion in exponentially growing polyelectrolyte multilayers, using sodium citrate as the reducing agent. First, the graphene oxide was obtained by treating a commercial grade of Expanded Graphite (EG). Based on XRD and Raman spectroscopy results, a complete exfoliation of graphene nanopellets down to one layer was achieved during the oxidation process. Secondly, the diffusion of GO was carried out in an exponentially growing polyelectrolyte multilayer film made from poly(diallyldimethylammonium chloride) as the polycation and from poly(acrylic acid) as the polyanion. Electrical conductivity of the GO based films was measured during the reduction process as a function of time. The conductivity reached values of the order of 10(-4) S cm(-1), whereas the pristine polyelectrolyte multilayer was highly insulating (～10(-8) S cm(-1)). The conductivity also reached a maximal value after about 24 h of reduction and decreased for longer reduction duration. Some tentative explanations for this peculiar finding will be given.     

THE HADAMARD INEQUALITY FOR CONVEX FUNCTION VIA FRACTIONAL INTEGRALS

In this paper, we establish several inequalities for some differantiable mappings that are connected with the Riemann-Liouville fractional integrals. The analysis used in the proofs is fairly elementar...     

On the role of the definition of potential models in Gibbs ensemble phase equilibria simulations of the H2S-pentane mixture

The effect of treating explicitly the coulombic and polarization interactions is investigated through the calculation of the coexistence curve of the pentane-H₂S binary mixture. In this work, potential models have been developed for hydrogen sulphide and pentane, which include electrostatic sites—estimated from ab initio calculations—and polarizable sites—estimated from experimental data—in addition to Lennard-Jones sites. Compared to existing models, these new models have the same number of fitting parameters to experimental thermodynamic data. They are shown to correctly describe the coexistence curve of the pure compounds. When applied to the case of mixtures, together with Lorentz-Berthelot combining rules, they allow one to obtain a more accurate prediction of the coexisting compositions of the mixture. Furthermore, it is shown that the interaction energy in this kind of mixture cannot be properly described by using effective potential models usually considered for pure compounds.