Selective separations by reactive ion exchange: Part 4. Preconcentration of cadmium and zinc by in situ precipitation as hexacyanoferrate(II) salts on gel and macroporous ion-exchange resins

The in situ precipitation of traces of cadmium(II) and zinc(II) ions as hexacyanoferrates from aqueous matrices was studied on conventional polystyrene gel and macroporous cation- and anion-exchange resins. Coprecipitation with each other or with copper(II) ions present in binary cation resins or in solution, and the influence of added nonprecipitating ions of the same charge type such as magnesium(II) were investigated. Microporous (gel) cation exchangers gave reasonable recoveries and macroporous cation exchangers gave very good recoveries; but macroporous anion exchangers performed best, suggesting macroporous hexacyanoferrate(II) resin as an ideal phase for collection/preconcentration of traces of Cu²⁺, Cd²⁺, Zn²⁺, and possibly Co²⁺, Ni²⁺, and Pb²⁺ from waters. As expected, very low yields were obtained with conventional anion exchange resin in the hexacyanoferrate form. Uniform distribution of Cu²⁺, Zn²⁺, and Cd²⁺ over macroporous anion-exchange resin phases were established by means of electron probe scans and taken as evidence for the formation of a uniform, well-developed precipitate layer covering the entire resin particle surface.     

Relevant synthesis parameters for the sequential catalytic growth of carbon nanotubes

Sequential catalytic growth provides an efficient tool for the synthesis of carbon nanotubes periodically inserted with catalyst nanoparticles. Several synthesis parameters were found crucial in order to induce this particular growth mechanism. The presence of phosphorus is required to form metal phosphide particles active for the formation of carbon nanotubes with a matchstick morphology. The metal composition (Ni/Fe ratio) and the carbon supply have no influence on the nanofilament type but strongly affect the nanotube yield. The synthesis temperature induces important changes on both the nanofilament type and yield, which are correlated with important transformations of the catalyst layer in terms of composition, particle size, and physical state.     

Integral equation formulation for buoyancy-driven convection problems

An integral equation formulation for buoyancy-driven convection problems is developed and illustrated. Buoyancy-driven convection in a bounded cylindrical geometry with a free surface is studied for a range of aspect ratios and Nusselt numbers. The critical Rayleigh number, the nature of the cellular motion, and the heat transfer enhancement are computed using linear theory. Green's functions are used to convert the linear problem into linear Fredholm integral equations. Theorems are proved which establish the properties of the eigenvalues and eigenfunctions of the linear integral operator which appears in these equations.     

Determination of C60/C70 ratios in fullerene mixtures and film characterization by scanning tunneling microscopy

Fullerene powder mixtures with different C₆₀/C₇₀ ratios have been analyzed by a variety of techniques, and results have been compared. The fullerence mixtures have been characterized as solutions in n-hexane by high-pressure liquid chromatography (HPLC) and UV-VIS spectroscopy. Thin films of fullerenes on Au(111) have been prepared from the mixtures by sublimation. The sublimation process has been studied by simultaneous thermogravimetric and differential thermal analyses. Thin fullerene films on Au(111) have been investigated by scanning tunneling microscopy (STM). The STM images show primarily two types of ballshaped molecules arranged in a lattice with hexagonal symmetry (fcc(111) face, nearest neighbour distance: 1 nm). The two species differ in diameter. STM images of films made of mixtures of different C₆₀/C₇₀ ratios show that C₇₀ molecules display a larger apparent diameter (0.8 nm) and corrugation than C₆₀ molecules (0.7 nm). The C₆₀/C₇₀ ratios obtained by counting the corresponding molecular species in the STM images of the thin films are compared to the C₆₀/C₇₀ ratios determined by HPLC on hexane solutions of the mixtures. The observed differences might be explained by different rates of sublimation for the two species. The STM images reveal film defects (vacancies and boundaries) and dynamic processes (displacement of C₇₀ molecules and vacancies). In films prepared to have a C₆₀ coverage of less than one monolayer, stable structural units of the C₆₀(111) surface consisting of three or seven C₆₀ molecules are revealed by STM. Occasionally, substructure within individual fullerene molecules is observed.     

Opening of single-walled carbon nanotubes: evidence given by krypton and xenon adsorption

Adsorption isotherms of krypton between 77 and 93 K and xenon between 110 and 120 K on mechanically-opened single-walled carbon nanotubes (SWNTs) have been measured. The comparison of the results with those obtained under the same conditions on closed nanotubes is discussed. Evidence of adsorption inside the tubes is given through the appearance of an additional adsorbed amount at very low relative pressure on the isotherms. Different orderings are predicted for xenon and krypton, based on their respective adsorbed amounts inside the nanotubes, and on geometrical considerations. Finally, the fraction of opened nanotubes accessible to xenon and krypton was estimated, as well as the impurity content originating from the cutting process.     

A propos de la structure de pyrimidines obtenues par condensation de l'acide cyanacétique et de monoalkylurées

Classically, the condensation of cyanoacetic acid and monoalkylurea gives 1-alkyl-6-amino-1,2,3,4-tetrahydropyrimidine-2,4-dione. However, this was verified only in two instances involving a long and delicate synthesis. The structure of the N′-cyanoacetyl-N-isobutylurea, an intermediate in the preparation of this type of pyrimidine, was confirmed by nmr. This method is capable of extension.     

Polyacetylene doped with iron trichloride : Improved conductivity and stability

Trans polyacetylene (CH)_x has been doped with FeCl₃ solutions in Nitromethane. In the “in-situ” EPR experiment we have observed the evolution of the EPR spectra with time during the doping process. That enabled us to gain information about the rate of dopant diffusion in solid material. Both EPR and conductivity measurements show that the doped material is reasonably stable even in the presence of air. Raman spectroscopic studies show the usual features observed in doped trans polyacetylene.