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At least 289 records · Page 16Linked to original sources

PubMed1991

Determination of gadolinium in biological materials using graphite furnace atomic absorption spectrometry with a tantalum boat after solvent extraction.

A method was developed for the determination of gadolinium (Gd) in biological material using graphite furnace atomic absorption spectrometry (GFAAS). The element is first extracted into methyl isobutyl ketone and then reextracted into hydrochloric acid. Factors influencing the recovery of extraction such as pH, choice of chelating agents, and hydrochloric acid concentration have been investigated. The element is determined under STPF (stabilized temperature platform furnace) conditions with atomization from a tantalum boat. Under optimized furnace conditions, the use of the tantalum boat improved sensitivity substantially compared to the use of pyrolytically coated graphite tubes. Around 150 measurements could be performed with 1 boat. Memory effects, being a common problem in the GFAAS determination of lanthanoids, were no longer observed after insertion of the boat. The characteristic mass and detection limit (2SD; SD = standard deviation) of the Gd determination are 1000 and 2060 pg, respectively. The precision evaluated as the relative standard deviation (RSD) of six analyses was below 10% for tissue Gd concentrations ranging from 0.92 to 72.0 micrograms g-1. The recovery of added analyte ranged between 92.0% and 99.3%. The method was found to be suitable for studying the pharmacokinetics and biodistribution of Gd in rats.

Animals↗

PubMed2000

Observation of low molecular weight poly(methylsilsesquioxane)s by graphite plate laser desorption/ionization time-of-flight mass spectrometry.

Mass spectra of polystyrene and poly(methylsilsesquioxane)(PMSSQ) derived from methyltriethoxysilane(MTES) were obtained in the 100-1,000 Da range by laser desorption/ionization time-of-flight mass spectrometry using a graphite plate without a matrix. Clean mass spectra were obtained without interference from carbon clusters or other low molecular weight compounds. Initial reaction products derived from condensation of partially hydrolyzed MTES were observed. Upon 30 min of heating at 30 degrees C, the ethoxy groups were fully hydrolyzed to hydroxy groups. Many PMSSQ species consistent with predictable polymerization reaction pathways involving intermolecular condensation and intramolecular dehydration were observed. Thus, laser desorption/ionization time-of-flight mass spectrometry using a graphite plate, without added matrix materials, is shown to provide valuable information on low molecular weight polymer not available by MALDI-TOF-MS.

Journal Article↗

PubMed1990

Determination of subnanogram per cubic meter concentrations of metals in the air of a trace metal clean room by impaction graphite furnace atomic absorption and laser excited atomic fluorescence spectrometry.

Air, drawn by vacuum through a jet, was impacted against the inside surface of an atomic absorption graphite electrothermal atomizer (ETA). The amounts of the particles thus collected were determined at the ng m-3 level by graphite furnace atomic absorption or at the pg m-3 level by laser excited atomic fluorescence. The overall reproducibility of two sets of measurements, made 7 months apart, was 23%, with no significant difference between the two sets of data, based on Student's "t" test at the 95% confidence level. Short-term reproducibility varied from 13% to 34% depending upon the air concentration of the metal. The method shows promise for monitoring long-term effectiveness of the filtering systems in trace metal clean rooms. It was not possible to test for accuracy, due to the low concentrations involved, but accuracy was expected to be within a factor of 2 or 3 of the actual value, based on theoretical aspects of impaction.

Air↗

PubMed2003

A graphitized-carbon monolithic column.

The preparation of a novel carbon monolithic column for high performance liquid chromatography is described. A phenolic resin rod with embedded 10-microm silica beads was prepared by acid-catalyzed polymerization of a resorcinol/iron(III) complex and formaldehyde. This rod was carbonized and graphitized under inert atmosphere with a programmed temperature cycle from room temperature to 1250 degrees C. Subsequently, the silica beads along with iron catalysts were removed, leaving a porous carbon rod. Imaging of this monolithic rod by scanning and transmission electron microscopies revealed a highly interconnected bimodal porous structure. The porosity and pore size distribution of the mesopores were characterized by N2 absorption/desorption. Graphene sheets were found in the TEM images of the carbon rod, and the graphite index was characterized by Raman spectrum and X-ray diffraction. A monolithic column prepared with the aforementioned carbon rod was evaluated using a mixture of alkylbenzenes. It exhibited an excellent separation power and a low hydraulic resistance. The bundle-of-capillaries model was used to characterize the hydrodynamics of this monolith. Its permeability was found to agree well with the theoretical one.

Journal Article↗

PubMed2003

Electrochemical characterization of binderless, recompressed exfoliated graphite electrodes: electron-transfer kinetics and diffusion characteristics.

Exfoliated graphite (EG) is prepared by the thermal exfoliation of graphite intercalation compounds at different temperatures. Surface and bulk physicochemical properties of EG are followed by spectroscopic and analytical methods and are observed to be a function of exfoliation temperature. EG particles can be recompressed without any binder and used as surface-renewable electrodes. Surface preparation is accomplished by either polishing or roughening the electrode surface using emery sheets. Effects of exfoliation temperature and the surface preparation on the electron-transfer kinetics and on the diffusion characteristics have been followed by electrochemical methods using several benchmark redox systems. It is found that the electron-transfer kinetics and the diffusion of K(4)[Fe(CN)(6)] are affected by the nature of the EG surface while that of iron(II)(1,10-phenanthroline)(3) and cobalt(II)(1,10-phenanthroline)(3) are not affected by the surface preparation. The redox systems are classified into different groups according to their kinetic sensitivity. Diffusion of electroactive species toward the EG electrodes is found to nonlinear. Current-time plots suggest that the recompressed EG electrodes can be modeled as fractals.

Journal Article↗

PubMedDate not supplied

Stability and properties of polyhelicenes and annelated fused-ring carbon helices: models toward helical graphites.

The geometrical structures and properties of conjugated polyhelicenes and annelated fused-ring carbon helices with analogous frameworks were theoretically studied at the HF/6-31G and B3LYP/6-31G levels. These studies focused on the stability of the fused-ring structures with special emphasis on the helical geometrical arrangements. To elucidate bonding patterns, the orbitals, electron density contours, and the electrostatic potential of these helical compounds were analyzed. The structure of fused polynaphthalenes arranged in a helical spiral can be regarded as part of a locally helical graphite lattice that is expected to give rise to special electronic properties along the helically layered conjugated single sheet that can be regarded as a single extended pi system but also involving local layer-to-layer pi-pi interactions that are typical in ordinary graphite. This dual feature might lead to novel materials.

Journal Article↗

PubMed2005

Stability of [Ru(II)(tpy)(bpy)(OH(2))](2+)-modified graphite electrodes during indirect electrolyses.

The stability of a graphite felt electrode modified by covalent attachment of [Ru(II)(tpy)(bpy)(OH(2))](2+) is investigated during the indirect electrolyses of alcohols in a flow cell. The continuous increase of the local potential of the electrode during the electrolyses attests to its degradation. Cyclic voltammetry analyses of the modified electrode after electrolyses show a total decrease of 80-90% of the wave corresponding to the Ru(III/II) couple. The concentration of remaining alcohol measured at the outlet of the cell is almost constant during all the electrolyses but increase when the potential exceeds 0.95 V(SCE). At low potentials, the electrode can be regenerated by reaction with Ru(II)Cl(2)(DMSO)(tpy) and then CF(3)SO(3)H, followed by hydrolysis, showing that the bipyridine ligand remains covalently attached to the electrode. At high potentials, the graphite is oxidized and the catalyst is partly lost in the reaction medium. XPS analyses of Ru core levels reveal that the ruthenium disappeared after electrolysis, showing that the degradation of the modified electrode is due to the demetalation of the oxidized complex.

Journal Article↗

PubMed2006

Electronic structure and charge transfer in the ternary intercalated graphite beta-KS0.25C3.

The electronic structure of the ternary intercalated graphite beta-KS(0.25)C3 is studied by means of a first-principles density functional theory approach. The nature of the partially filled bands is analyzed, and the K sublayers of the intercalate are shown to have an important contribution to the Fermi surface. This K-based contribution confers a sizable three-dimensional character to the conductivity even if considerably less than that for the related binary KC8. The electronic structure of beta-KS(0.25)C3 differs noticeably from that of the related ternary compound, KH(x)C4. The charge transfer is analyzed, and a way to evaluate it, which can be used in general for intercalated graphites, is proposed. The charge transfer per C atom in this ternary material is shown to be smaller than that in the KC8 binary compound despite a more favorable stoichiometry ratio between K and C.

Journal Article↗

PubMed1996

Enhancement of the Catalytic Activity of a Macrocyclic Cobalt(II) Complex for the Electroreduction of O(2) by Adsorption on Graphite.

In solution, the [(tim)Co](2+) complex (tim = 2,3,9,10-tetramethyl-1,4,8,11-tetraazacyclotetradeca-1,3,8,10-tetraene) reacts only slowly with O(2), but upon adsorption on graphite electrodes, it becomes an active catalyst for the reduction of O(2) to H(2)O(2). The electroreduction of O(2) proceeds in a single voltammetric step at close to the diffusion-controlled rate at a relatively positive potential (0.25 V vs SCE). The remarkable enhancement in catalytic activity is attributed to a higher affinity for O(2) of the adsorbed complex as a result of its interactions with functional groups on the surface of roughened or oxidized graphite. A possible mechanism for the catalytic reduction of O(2) is proposed. It differs from the one employed by the analogous [(hmc)Co](2+) complex (hmc = C-meso-5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane) which operates at less positive potentials and exhibits two separated voltammetric steps in the reduction of O(2), via [(hmc)CoOOH](2+), to H(2)O(2).

Journal Article↗

PubMed2001

High-pressure bulk synthesis of crystalline C(6)N(9)H(3).HCl: a novel c(3)n(4) graphitic derivative.

A novel carbon nitride compound, structurally related to the proposed graphitic phase of C(3)N(4), has been synthesized in a bulk well-crystallized form. The new material, with stoichiometry C(6)N(9)H(4)Cl, was prepared through a solid-state reaction of 2,4,6-triamino-1,3,5-triazine with 2,4,6-trichloro-1,3,5-triazine at 1.0-1.5 GPa and 500-550 degrees C and also through a self-reaction of 2-amino-4,6-dichloro-1,3,5-triazine at similar conditions. X-ray and electron diffraction measurements on the yellowish compound indicate a hexagonal space group (P6(3)/m) with cell parameters of a = 8.4379(10) A and c = 6.4296(2) A. This new compound possesses a two-dimensional C(6)N(9)H(3) framework that is structurally related to the hypothetical P6m2 graphitic phase of C(3)N(4), but with an ordered arrangement of C(3)N(3) voids. The large voids in the graphene sheets are occupied by chloride ions with an equivalent number of nitrogen atoms on the framework protonated for charge balance. The composition of the sample was determined by bulk chemical analysis and confirmed by electron energy loss (EELS) spectroscopy. The chemical and structural model is consistent with bulk density measurements and with the infrared and (13)C NMR spectra. This work represents the first bulk synthesis of a well-characterized and highly crystalline material containing a continuous network of alternating carbon and nitrogen atoms.

Journal Article↗

PubMed2003

Chiral pair monolayer adsorption of iodine-substituted octadecanol molecules on graphite.

High-resolution scanning tunneling microscopy has been used to examine the adsorbate structures formed when a racemic mixture of (9R,10R)-9,10-diiodooctadecan-1-ol and (9S,10S)-9,10-diiodooctadecan-1-ol is adsorbed at the basal plane of highly ordered pyrolytic graphite. The herringbone structure characteristic of the adsorption of long-chain molecules on graphite is observed. Close examination of the micrographs indicates a unique structure in which the chiral molecules adsorb in pairs, with one enantiomer filling half of the unit cell, and the other enantiomer filling the other half. Instead of forming separate chiral domains, as is sometimes observed when a racemic mixture adsorbs on an achiral surface, chiral pairs are formed and the pairs form an ordered monolayer, exposing opposite faces of the same molecule. An achiral racemic mixture is observed to form a chiral structure on an achiral surface in the regions of the surface examined here.

Journal Article↗

PubMed2004

Scanning tunneling microscopy of prochiral anthracene derivatives on graphite: chain length effects on monolayer morphology.

The morphology of monolayers formed upon adsorption of prochiral 1,5-substituted anthracene derivatives on highly oriented pyrolytic graphite is investigated using scanning tunneling microscopy at the liquid-solid interface. The adsorption orientation of these prochiral anthracene derivatives positions one of their enantiotopic faces in contact with the graphite. The molecules adsorb in rows with contact between adjacent anthracenes. The anthracene side chains extend perpendicular to the direction of the row repeat. All molecules within a single row adsorb via the same enantiotopic face. Anthracenes with side chains containing an even number of non-hydrogenic atoms (C, S) form monolayers in which molecules in adjacent rows adsorb via opposite enantiotopic faces. Anthracenes with side chains that contain an odd number of non-hydrogenic atoms form two-dimensional chiral domains in which all rows contain molecules adsorbed via the same enantiotopic face. This chain length effect on monolayer morphology represents a generalized example of structural effects previously observed in alkanoic acid monolayers formed on HOPG. The variation of the STM current with position in the vicinity of the anthracenes indicates that the highest occupied molecular orbital is the predominant mediator of tunneling for the aromatic group.

Journal Article↗

PubMed2004

The location of adsorbed hydrogen in graphite nanostructures.

Recent experiments suggest that the high hydrogen storage capacity in graphite nanostructures might be associated with adsorption on the edges. First-principles calculations are used to study the structure and energetics of H chemisorption on graphite zigzag edges. The properties of both singly and doubly hydrogenated edges are examined. Molecular hydrogen can dissociatively adsorb on the edge directly, with small activation barriers to the formation of either singly or doubly hydrogenated structures. A new model for the location of adsorbed H is proposed.

Journal Article↗

PubMed2006

Multiwall carbon nanotubes made of monochirality graphite shells.

A multiwall carbon nanotube (MWCNT) consists of several or many concentric carbon shells, each of which could be metallic or semiconducting. Both theoretical predictions and experimental results suggest that MWCNTs have exotic electronic structures and intriguing transport properties, which are highly dependent on chirality of each shell. However, the structural defects and the random distribution of chirality of each concentric graphitic shell make the MWCNTs difficult for basic research and technological applications. Thus far, it is still a challenge to get the high crystalline MWCNTs with limited atomic conformation. Here, we report the synthesis of high crystalline MWCNTs made of monochirality graphite shells by a low-temperature chemical vapor deposition (CVD) process in plasma environment. Structural analysis, carried out by transmission electron microscopy (TEM) image and electron diffraction methods, reveal that the MWCNTs are well-crystallized and that most of them have nearly identical chiralities.

Journal Article↗

PubMed2006

Two-dimensional surface chirality control by solvent-induced helicity inversion of a helical polyacetylene on graphite.

We report the direct evidence for the macromolecular helicity inversion of a helical poly(phenylacetylene) bearing l- or d-alanine pendants with a long alkyl chain in different solvents by atomic force microscopy observations of the diastereomeric helical structures. The diastereomeric helical poly(phenylacetylene)s induced in polar and nonpolar solvents self-assembled into ordered, two-dimensional helix bundles with controlled molecular packing, helical pitch, and handedness on graphite upon exposure of each solvent. The macromolecular helicity deposited on graphite from a polar solvent further inverted to the opposite handedness by exposure to a specific nonpolar solvent, and these changes in the surface chirality based on the inversion of helicity could be visualized by atomic force microscopy with molecular resolution, and the results were quantified by X-ray diffraction of the oriented liquid crystalline, diastereomeric helical polymer films.

Journal Article↗

PubMed2003

Tungsten permanent chemical modifier for fast estimation of Se contents in soil by graphite furnace atomic absorption spectrometry.

A tungsten carbide coating on the integrated platform of a transversely heated graphite atomizer was used as a modifier for the direct determination of Se in soil extracts by graphite furnace atomic absorption spectrometry. Diethylenetriaminepentaacetic acid (0.0050 mol L(-1)) plus ammonium hydrogencarbonate (1.0 mol L(-1)) extracted predominantly available inorganic selenate from soil. The formation of a large amount of carbonaceous residue inside the atomizer was avoided with a first pyrolysis step at 600 degrees C assisted by air during 30 s. For 20 microL of soil extracts delivered to the atomizer and calibration by matrix matching, an analytical curve (10.0-100 microgram of L(-1)) with good linear correlation (r = 0.999) between integrated absorbance and analyte concentration was established. The characteristic mass was approximately 63 pg of Se, and the lifetime of the tube was approximately 750 firings. The limit of detection was 1.6 microgram L(-1), and the relative standard deviations (n = 12) were typically <4% for a soil extract containing 50 microgram of L(-1). The accuracy of the determination of Se was checked for soil samples by means of addition/recovery tests. Recovery data of Se added to four enriched soil samples varied from 80 to 90% and indicated an accurate method.

Chemical Phenomena↗

PubMed2005

Stimulating effect of graphite admixture on hydrogen sorption-desorption properties of mechanically activated titanium powder.

The effect of graphite admixture on hydrogen sorption-desorption properties of mechanically activated electron microscopy, temperature-programmed reaction, and temperature-programmed desorption techniques. The major effect of graphite addition was found to be the formation of microporous carbon matrix particles containing randomly distributed titanium particles only several nanometers in diameter. This powder architecture enhances hydrogen transport to the titanium surface without hindrances and promotes titanium-hydrogen interaction by modifying the titanium surface and subsurface layers with interstitial carbon atoms.

Journal Article↗

PubMed2005

Graphite-incorporated MoS2 nanotubes: a new coaxial binary system.

Graphite-filled MoS2 nanotubes were synthesized by pyrolizing propylene inside MoS2 nanotubes prepared by a template-assisted technique. The large coaxial nanotubes were constituted of graphite sheets inserted between the MoS2 layers, forming the outer part, and coaxial multiwall carbon nanotubes intercalated with MoS2 inside. High-resolution electron microscopy (HREM) and electron energy loss spectroscopy techniques along with molecular dynamics simulation and quantum mechanical calculations were used to characterize the samples. The one-dimensional structures exhibit diverse morphologies such as long straight and twisted nanotubes with several structural irregularities. The interplanar spacing between the MoS2 layers was found to increase from 6.3 to 7.4 A due to intercalation with carbon. Simulated HREM images revealed the presence of mechanical strains in the carbon-intercalated MoS2 layers as the reason for obtaining these twisted nanostructures. The mechanism of formation of carbon-intercalated MoS2 tubular structures and their stability and electronic properties are discussed. Our results open up the possibility of using MoS2 nanotubes as templates for the synthesis of new one-dimensional binary-phase systems.

Journal Article↗