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High Yield Syntheses of Stable, Singly Bonded Pd26+ Compounds
2006
A general method for the syntheses of dipalladium compounds having a singly bonded Pd26+ core and the formula R,S-cis-Pd2(C6H4PPh2)2(O2CR)2Cl2 is described. When the alkyl group in the carboxylate ligands is an electron donating group, the compounds are stable and the yields high. The Pd-Pd distances for the diamagnetic compounds with R = CF3 and CMe3 are 2.5434(4) and 2.5241(9) A, respectively. Calculations at the DFT level suggest that the electronic configuration is sigma2pi4delta2delta*2pi*4. These represent rare examples of palladium(III) compounds.
Copper Isotope Fractionation during Complexation with Insolubilized Humic Acid
2010
The bioavailability, mobility, and toxicity of Cu depend on Cu speciation in solution. In natural systems like soils, sediments, lakes, and river waters, organo-Cu complexes are the dominating species. Organo-complexation of Cu may cause a fractionation of stable Cu isotopes. The knowledge of Cu isotope fractionation during sorption on humic acid may help to better understand Cu isotope fractionation in natural environments and thus facilitate the use of Cu stable isotope ratios (delta(65)Cu) as tracer of the fate of Cu in the environment. We therefore studied Cu isotope fractionation during complexation with insolubilized humic acid (IHA) as a surrogate of humic acid in soil organic matter…
Determination of major carotenoids in vegetables by capillary electrochromatography.
2006
A simple and rapid method for the isocratic separation and determination of carotenoids (carotenes and xanthophylls) in vegetables by CEC is described. The capillary column (100 microm ID, 25 cm effective length) was packed with 3 microm Hypersil ODS particles. The optimized mobile phase contained 60% ACN, 35% THF and 5% of a 5 mM Tris aqueous buffer of pH 8. beta-Carotene, lycopene and lutein were separated with efficiencies of 66 000-128 000 plates/m within a short time (less than 12 min for the last peak eluted, 13/13'-cis-beta-carotene). An excellent resolution of the three carotenoids, as well as partial resolution of their geometrical isomers, was achieved. Application to the determin…
Rapid evaluation of oxidised fatty acid concentration in virgin olive oil using Fourier-transform infrared spectroscopy and multiple linear regression
2011
Abstract Fourier-transform infrared spectroscopy (FTIR), followed by multivariate treatment of spectral data, was used to evaluate the oxidised fatty acid (OFA) concentration in virgin olive oil samples characterised by different oxidative status. The entire FTIR spectra (4000–700 cm−1) of oils were divided in 25 wavelength regions. The normalised absorbances of the peak areas within these regions were used as predictors. In order to predict the OFA concentration, multiple linear regression (MLR) models were performed. After a cube root transformation of data, an MLR model constructed using eight predictors was able to predict OFA concentration with an average error of 17%. The main wavelen…
Microphase separation in linear multiblock copolymers under poor solvent conditions
2010
Molecular dynamics simulations are used to study the phase behavior of linear multiblock copolymers with two types of monomers, A and B, where the length of the polymer blocks $N_{A}$ and $N_{B}$ ($N_{A}=N_{B}=N$), the number of the blocks $n_{A}$ and $n_{B}$ ($n_{A}=n_{B}=n$), and the solvent quality varies. The fraction $f$ of A-type monomers is kept constant and equal to 0.5. Whereas at high enough temperatures these macromolecules form coil structures, where each block A or B forms rather individual clusters, at low enough temperatures A and B monomers from different blocks can join together forming clusters of A or B monomers. The dependence of the formation of these clusters on the va…
Block and graft copolymers of 2-oxazolines
1994
The cationic ring-opening polymerization of 2-oxazolines is known to be initiated by alkyl halides, Lewis acids and esters of strong acids. The polymerization proceeds by a living mechanism. Numerous block and graft copolymers have already been described. Recently it was found that chloroformates (R-O-CO-CI) are also useful initiators. The mechanism of the initiation and propagation is discussed. This type of initiators allows the synthesis of different novel two-block and three-block copolymers, star-shape polymers, and a graft copolymer with a polyvinylacetate backbone.
Cementing agents involved in the macro- and microaggregation of a Mediterranean shrubland soil under laboratory heating
2014
The heating effect on aggregation and cementing agents of a Mediterranean soil was studied in two fractions (macro- and microaggregates) in different environments: under Quercus coccifera soil (UQ), under Rosmarinus officinalis soil (UR) and between plants or bare soil (BS). Samples were heated under laboratory conditions at different temperatures (220, 380, 500, 750 and 1000. °C) to establish their effects on the studied soil properties by comparison with unheated control samples (25. °C). Increasing temperature treatments caused significant changes in most soil variables. In both soil fractions, the presence of vegetation contributed to increase of the soil organic matter (SOM) content, w…
Biogeochemical evaluation of historical sediment contamination in the Gulf of Palermo (NW Sicily): Analysis of pseudotrace elements and stable isotop…
2012
Abstract Sedimentary biogeochemical data from the Gulf of Palermo, which borders one of the major urban and industrial areas of the central Mediterranean, provide a decennial–centennial-scale record of the effects of human activity on this coastal environment. In this study we report trace elements (TE), C org /N tot ratios, δ 13 C org , and δ 15 N tot from dated ( 210 Pb) sediments collected in two coastal stations variably influenced by urban/fluvial loadings and illegal dumping and we compare them with published data for offshore sediments, in order to investigate at a large spatial scale the influence of on-land activities on sedimentary marine system. TE were generally low except for H…
Probe diffusion in homogeneous diblock copolymers
1998
Forced Rayleigh scattering was used to investigate the diffusion of a photoreactive dye molecule in two homogeneous poly(styrene-b-isoprene) (SI) diblock copolymers with overall molecular weights of approximately 2000. Although diffusion rates were intermediate to TTI transport in homopolymer polystyrene (PS) and polyisoprene (PI), system dynamics appear to be largely dictated in each case by the PI block. The size of the polymer jumping unit, on the other hand, is evaluated from a free-volume analysis of the data, and is found to be governed predominantly by the PS component of the copolymer. The mechanism for tracer diffusion in low-molecular-weight block copolymers appears analogous to t…
Spectrophotometric determinations of binding constants between cyclodextrins and aromatic nitrogen substrates at various pH values
2001
The inclusion capacity of native β-cyclodextrin (1) and mono-(6-amino-6-deoxy)-β-cyclodextrin (2) versus aromatic compounds having a nitro or an amino group or both has been investigated at three different pH values. Molecular interactions in inclusion complexes have also been investigated by means of molecular mechanics (MM2/QD) models. Electrostatic and van der Waals interactions and the formation of a hydrogen bond between the donor amino group and the oxygen atom of the secondary hydroxyl group seem to be the more important contributions in determining complex stability. The inclusion capacity of two different cyclodextrins versus aromatic compounds has been investigated at three differ…