Reprint of: Application of micro-thin-layer chromatography as a simple fractionation tool for fast screening of raw extracts derived from complex biological,pharmaceutical and environmental samples

The main goal of present paper is to demonstrate the separation and detection capability of micro-TLC technique involving simple one step liquid extraction protocols of complex materials without multi-steps sample pre-purification. In the present studies target components (cyanobacteria pigments, lipids and fullerenes) were isolated from heavy loading complex matrices including spirulina dried cells, birds’ feathers and fatty oils as well as soot samples derived from biomass fuel and fossils-fired home heating systems. In each case isocratic separation protocol involving less that 1 mL of one component or binary mixture mobile phases can be completed within time of 5–8 min. Sensitive detection of components of interest was performed via fluorescence or staining techniques using iodine or phosphomolybdic acid. Described methodology can be applied for fast fractionation or screening of whole range of target substances as well as chemo-taxonomic studies and fingerprinting of complex mixtures, which are present in raw biological or environmental samples.     

Aromaticity of corazulenic fullerenes

A novel class of non-classical fullerenes, having pentagon–heptagon pairs, as in azulene, is modeled. The various coverings, sometimes alternating azulenic and benzenic units, are designed by some new sequences of map operations or generalized operations. The hypothetical azulenic fullerenes are characterized by PM3 semiempirical data and POAV1 strain energy SE. Their aromaticity is discussed in the light of several criteria. The HOMA index of aromaticity enabled evaluation of global and local aromaticity of the designed fullerenes.     

Thermally Stable,Efficient Polymer Solar Cells with Nanoscale Control of the Interpenetrating Network Morphology

By applying the specific fabrication conditions summarized in the Experimental section and post‐production annealing at 150 °C, polymer solar cells with power‐conversion efficiency approaching 5 % are demonstrated. These devices exhibit remarkable thermal stability. We attribute the improved performance to changes in the bulk heterojunction material induced by thermal annealing. The improved nanoscale morphology, the increased crystallinity of the semiconducting polymer, and the improved contact to the electron‐collecting electrode facilitate charge generation, charge transport to, and charge collection at the electrodes, thereby enhancing the device efficiency by lowering the series resistance of the polymer solar cells.     

Electron diffraction and microscopy of single-wall carbon nanotube bundles produced by different methods

The atomic structure of single-wall carbon nanotube bundles produced by three different techniques (laser ablation, electric arc discharge and catalytic chemical vapor deposition (CCVD)) has been characterized by electron diffraction and microscopy. Information on the helicity and the lattice packing has been obtained. Concerning the helicity, small bundles produced by CCVD exhibit only one or two tube helicities within a single bundle. The diffraction patterns of laser-ablation produced bundles also present well-defined but more diversified chiralities within a single bundle. By contrast the data acquired on bundles formed by arc discharge show a more diffuse pattern, characteristic of a random chirality dispersion within a single bundle. Concerning the lattice packing, informations are obtained via a detailed study of the equatorial line of the diffraction pattern for bundles produced by the three techniques. This electron diffraction study is completed by high-resolution electron microscopy. Received 8 August 2001 and Received in final form 14 March 2002     

Polymerization and depolymerization of fullerenes induced by hole injection from scanning tunneling microscope tips

Reversible polymerization and depolymerization reactions of fullerene (C₆₀) molecules are induced by tunnel injection of holes from tips of scanning tunneling microscopes similarly to the reactions induced by tunneling electrons. The bi-directional and bi-polar features of the hole-induced and electron-induced reactions can be interpreted by a unified model considering ionic reactions over symmetry-imposed barriers in the [2+2] cyclo-addition and the reverse reactions.     

Raman spectra of samarium-fullerene intercalation compounds

Samarium-fullerene intercalation compounds of nominal composition Sm_xC₆₀ (x=1,2,…,6) have been synthesized by a solid-state reaction method. We obtain a Sm_2.75C₆₀ superconducting phase with orthogonal structure and a Sm₆C₆₀ phase with body-centered cubic structure. The broadening and weakening of Raman peaks of the Sm_xC₆₀ compounds are due to the distortion of C₆₀ and electron-phonon interaction. The Raman measurements reveal that the distortion of C₆₀ decrease in Sm_xC₆₀ (x=3,4,5) exposed to air, although the fulleride solids have transformed into an amorphous state. The Raman results also show that the distortion of C₆₀ is still very large in the Sm₆C₆₀ exposed to air, or the C₆₀ molecules have been destroyed and become some amorphous carbide.     

DSC study of annealing and phase transformations of C60 and C70 polymerized under pressures in the range 9.5-13 GPa

C₆₀ and C₇₀ fullerenes polymerized under pressures between 9.5 and 13 GPa and temperatures between 670 and 1850 K were investigated by differential scanning calorimetry (DSC) in the range 240-640 K. Endothermal heat effects were observed with a peak maximum just below 540 K, a temperature characteristic for breakdown of (2+2) intermolecular links in dimers, 1D and 2D polymers. Exothermal effects, starting from 380 K, were observed for the first time in polymeric fullerenes. These effects are attributed to relaxation processes and to breakdown of other types of intermolecular bonds such as common four-sided rings and (3+3) interlinks.     

Fullerene Black Modified Screen Printed Electrodes for the Quantification of Acetaminophen and Guanine

Fullerene Black (FB) and Extracted Fullerene Black (EFB) were used in modified screen‐printed electrodes producing electrochemical transducers (FB‐SPEs and EFB‐SPEs). A complete electrochemical study was performed and the best results are obtained working with FB‐SPEs, especially in terms of: 1. improved electron‐transfer kinetic mechanisms and 2. sensitivity and selectivity toward Acetaminophen (Ac) and Guanine (G). These latter represent two important electro‐active targets to quantify in medicine field application, because: Ac is a preferred alternative (as analgesic‐antipyretic agent) to aspirin, particularly for patients who cannot tolerate aspirin; the oxidation signal of G is useful for the fabrication of emerging analytical tools, such as DNA chipsand user‐friendly diagnostic devices. Ac and G are quantify by using FB‐SPEs electrochemical devices, with an extended linearity (1–300 μM for Ac; 0.1–300 μM for G), an excellent sensitivity (2.82 μA μM⁻¹ cm⁻² in the case of Ac; and 0.183 μA μM⁻¹ cm⁻² in the case of G), a low detection limit (0.01 μM for Ac; 0.005 μM for G), a very good reproducibility (both: intra‐; inter‐electrodes reproducibility RSD % ranging from 0.3–0.5 for Ac; and 0.50–0.85 for G) and a very fast response time (6 s for Ac; 5 s in the case of G). In addition, high selectivity is obtained at FB‐SPEs, meaning that the FB‐SPEs electrochemical transducers are suitable to simultaneously quantify Ac and G in real samples, having several different (highly concentrated) interference.     

Application of micro-thin-layer chromatography as a simple fractionation tool for fast screening of raw extracts derived from complex biological, pharmaceutical and environmental samples

The main goal of present paper is to demonstrate the separation and detection capability of micro-TLC technique involving simple one step liquid extraction protocols of complex materials without multi-steps sample pre-purification. In the present studies target components (cyanobacteria pigments, lipids and fullerenes) were isolated from heavy loading complex matrices including spirulina dried cells, birds’ feathers and fatty oils as well as soot samples derived from biomass fuel and fossils-fired home heating systems. In each case isocratic separation protocol involving less that 1 mL of one component or binary mixture mobile phases can be completed within time of 5–8 min. Sensitive detection of components of interest was performed via fluorescence or staining techniques using iodine or phosphomolybdic acid. Described methodology can be applied for fast fractionation or screening of whole range of target substances as well as chemo-taxonomic studies and fingerprinting of complex mixtures, which are present in raw biological or environmental samples.