Reliability of the direct ICP-MS analysis of volcanic ash nanoparticles

In the present work, major and trace element concentrations in suspensions of volcanic ash nanoparticles were determined by ICP-MS after either the acid digestion of the suspensions or the direct analysis of these suspensions. The results obtained were compared. Since the acid digestion can be accompanied by an important dilution or can consist in different steps of evaporation and dilution, the determination of some trace element concentrations became limited because of the limit of detection of the analytical instrument. Therefore, analysis after acid digestion of suspensions and direct analysis after acidification of these suspensions were carried out and compared. The concentration of Al, Fe, Y, La, Ce, Pr, Gd, Ho, Cu, Tl and Pb determined by both preparation procedures were in agreement. The values of relative standard deviation are in the range from 1% to 14%. These results prove the reliability of the direct ICP-MS analysis and the possibility of its further application in hyphenated systems for the dimensional and elemental characterisation of natural mineral nanoparticles.     

Levopimaric acid derived 1,2-diamines and their application in the copper-catalyzed asymmetric Henry reaction

Levopimaric acid, a readily available starting material, was used in efficient syntheses of new enantiopure diamines and Schiff bases with good yields. The synthetic procedure is based on the fumaropimaric acid monomethyl ester conversion into the optically pure trans-1,2-diamine via a Curtius rearrangement. New diamines were studied as ligands in the copper-catalyzed asymmetric Henry reaction.     

Neutron Scattering Studies of Structure and Self-Assembly of Star-Shaped Polymers with Fullerene Centres in Solutions

Protonated star-shaped polystyrenes with single and double fullerene C₆₀ core and the hybrid stars with pairs of polar and non-polar arms (tertbuthylmetacrylate, polystyrene) have been studied in deuterated toluene (20 °C) by small-angle neutron scattering at low and moderate polymer concentrations (c₁ ∼ 1 g/dl, c₂ ∼ 3–6 g/dl) to evaluate the peculiarities of fullerene centre action on polymers self-assembly in solutions. As we found, the cores composed of two fullerenes, linked via Si(CH₃)₂-bridge, induce stars' anisotropic interactions and association into chain-like structures (correlation radius ∼400–600 nm). Meanwhile, the single-core stars of polystyrene and hybrids organize globular clusters (size ∼ 10³ nm) those geometry do not change significantly by polymer content variation.     

A new solvate of furosemide with dimethylacetamide

The loop diuretic furosemide is used widely in the treatment of congestive heart failure and edema, and is practically insoluble in water. The physicochemical and pharmacokinetic properties of drugs can be modified by preparing the drug in an appropriate solid‐state form. A new solvate of furosemide with dimethylacetamide (DMA) {systematic name: 4‐chloro‐2‐[(furan‐2‐yl)methylamino]‐5‐sulfamoylbenzoic acid N,N‐dimethylacetamide disolvate}, C₁₂H₁₁ClN₂O₅S·2C₄H₉NO, (I), is reported. The channeled structure formed on slow crystallization contains DMA solvent molecules in its channels. This structure adds to the evidence of varied conformations observed across all known structures, so supporting the idea that this flexible molecule has conformational lability. The current structure also differs from those of other previously known furosemide solvates in the number of solvent molecules per furosemide molecule, viz. 2:1 instead of 1:1. Desolvation of (I) gives the most stable form of furosemide, i.e. Form I.     

Ion channeling study of lattice distortions in chromium-doped SrTiO3 crystals

The results of ion channeling studies of lattice distortions in SrTiO₃: Cr single crystals are presented. Two types of single crystals containing the same amount of Cr impurities but differing in stoichiometry have been investigated. The single crystals grown by the Verneuil method have the compositions of standard-grown SrTiO₃: Cr (0.05 at % Cr), whereas the single crystals grown with a strontium deficiency and a chromium compensating amount have the composition Sr_0.9995TiO₃ (0.05 at % Cr). Analysis of the angular channeling spectra indicates that, in crystals of both types, the main defects are Cr impurities located in octahedral sites. In the SrTiO₃: Cr crystals, impurity atoms manifest themselves as Cr⁴⁺ with tetragonal Jahn-Teller distortions of the surrounding lattice. In the Sr_0.9995TiO₃: Cr crystals grown with a Sr deficiency, the characteristic displacements of Ti ions in the third coordination sphere of the Jahn-Teller center Cr⁴⁺ exhibit the effect of interaction of the center with a neighboring vacancy in the Sr sublattice.