Photometric titration of total iodine at trace levels in concetrated chloride solutions

The method is based on reduction of total iodine (10^?7?10^?5 M), to iodide with sulphite in acidic solution. The excess of sulphur dioxide is removed by bubbling with nitrogen, and the resulting solution is titrated spectrophotometrically with a standard solution of iodate, the absorbance being measured at 230 nm. Some Italian table salts, iodized or common, were analyzed for their iodide and total iodine content.     

Sorption of proton and heavy metal ions on a macroporous chelating resin with an iminodiacetate active group as a function of temperature

A macroporous resin containing iminodiacetic groups (Lewatit) was investigated for its sorption properties towards proton and nickel(II) and cadmium(II). Different compositions of the aqueous phase, and different temperatures were examined. The stoichiometry, the exchange coefficients and the intrinsic constants of the sorption equilibria were obtained from the experimental data by using the Gibbs-Donnan model for the ion exchange resin. The intrinsic constants were found to be independent of the composition of the solution, so that they were used for characterizing the sorption equilibria. While the first intrinsic protonation constant of the active groups in the resin was found to depend on the temperature, the second one was independent. The sorption equilibrium of nickel in the resin was different from that of cadmium, being ascribable respectively to the formation of the complexes NiL and Cd(HL)(2). inside the resin. Their intrinsic complexation constants were found to be 10(-1.84) and 10(-3.64) at 25 degrees C. Compared to those of another resin with the same active groups, but not macroporous, they are higher. The dependence of the intrinsic constant on the temperature was also different for the two metals, allowing to evaluate a DeltaH degrees of +30.9 and of +13.7 kJ mol(-1) respectively. When a comparison is possible, these values are near to those in aqueous solution for the complexation with ligands of similar structure. These results can be used to achieve metal ion separation based on temperature variations.     

Enantioselective reduction and deracemisation using the non-conventional yeast Pichia glucozyma in water/organic solvent biphasic systems: preparation of (S)-1,2-diaryl-2-hydroxyethanones (benzoins)

Water/organic solvent two-liquid-phase systems have been successfully applied in the synthesis of enantiomerically pure (S)-benzoin through two different methodologies catalysed by whole cells from the non-conventional yeast Pichia glucozyma: the stereoselective monoreduction of benzil and the deracemisation of benzoin. The presence of the organic solvent influences the redox systems implied in the reactions, avoiding the formation of the corresponding diols, increasing the enantioselectivity and allowing the easy isolation of the products in high yields and excellent enantiomeric excesses. The use of both strategies has been extended to the preparation of different chiral benzoin derivatives.     

Optimum extraction process of polyphenols from Bridelia grandis stem bark using experimental design

Euphorbiaceae barks are known to contain an appreciable amount of polyphenolic compounds responsible for several biological activities. Preliminary extraction from Bridelia grandis stem bark afforded high content of polyphenols, determined by spectrophotometric methods such as Folin–Ciocalteu (for total phenols, TP) and n‐butanol‐HCl (for condensed tannins, CT). A preliminary Plackett–Burman screening design was used to identify the key factors that influence the TP and CT extraction. Between all the variables known to influence the extraction from vegetable matrixes, six were selected; maceration was chosen as traditional extraction methodology. To investigate the effect of solvents and extraction method, methanol, acetone 70% (v/v in water), centrifugation and ultrasound were chosen. A full factorial design 2³ was applied to optimize the extraction procedure. The responses were obtained analyzing the extracts for their TP and CT contents determined by the above‐mentioned spectrophotometric methods. The results confirm that, within the explored domain, the optimum solvent is methanol and the optimum method is one‐cycle centrifugation. Finally, it was also compared with the effect of maceration on the considered responses. It has never given results better than centrifugation, whereas in the case of CT it represents an advantage to employ a three‐cycle centrifugation instead of one.     

Solid phase extraction of copper(II) by fixed bed procedure on cation exchange complexing resins

The efficiency of the metal ion recovery by solid phase extraction (SPE) in complexing resins columns is predicted by a simple model based on two parameters reflecting the sorption equilibria and kinetics of the metal ion on the considered resin. The parameter related to the adsorption equilibria was evaluated by the Gibbs–Donnan model, and that related to the kinetics by assuming that the ion exchange is the adsorption rate determining step. The predicted parameters make it possible to evaluate the breakthrough volume of the considered metal ion, Cu(II), from different kinds of complexing resins, and at different conditions, such as acidity and ionic composition.     

Usage of Empore™ membrane in alcoholic media for copper(II) distribution studies

The sorption of copper(II) on a solid, iminodiacetic based, chelating material, the Empore™ membrane, in alcoholic solutions is considered. Determination of the acid-base properties, kinetic of metal sorption and complexing properties, in solutions with different percentages of ethanol, ranging from 0 to 40% is undertaken. The results are compared with those obtained using the classical iminodiacetic resin Chelex 100 in beads. No significant differences are found in the thermodynamic properties, but the kinetics of the metal sorption on the membrane is slower and a dependence of the process rate with the alcoholic content is observed. In the present investigation, the detection of copper(II) species both in alcoholic Italian distillate “grappa” and in its intermediate product (“flemma”), is carried out by the Resin Titration (RT) method using, as competitive reagent, the Empore™ membrane. To validate the procedure, synthetic solutions containing different percentages of ethanol are analysed.     

Inhibition of the oxygen evolution reaction during titanium passivation in aqueous phosphoric acid solution

Journal of Solid State Electrochemistry - The anodic oxide on titanium can be thickened by anodization, with the consequent corrosion properties of this oxide depending on many variables, including...