Chemical and electrochemical treatment effects on the morphology,structure, and electrochemical performance of carbon fiber with different graphitization indexes

The association of capacitive charging of the double-layer and a faradic redox reaction is desirable on carbon fiber (CF) when oxygen functional groups or other heteroatoms are present on its surface enhancing its capacitive properties. In this work, a systematic study of carbon fiber produced at three different heat treatment temperatures (HTT) of 1000, 1500, and 2000 °C was performed upon two approaches: middle (chemical) and severe (electrochemical) oxidative treatments. Morphological, structural, and surface chemical changes were investigated by field emission gun-scanning electron microscopy, X-ray diffraction, Raman spectroscopy, and X-ray photoelectron spectroscopy. Electrochemical responses were analyzed by galvanostatic charge/discharge, electrochemical impedance spectroscopy, and cyclic voltammetry. Raman results showed that the electrochemical oxidation promoted structural variation on CF samples independently of their HTT. Concerning the specific capacitance, the results indicated that chemical treatment was more effective for CF1000 than those for CF1500 and CF2000. This behavior may be attributed to higher amount of oxygen on its surface as well as its lower structural ordering. Otherwise, for CF1000, the electrochemical treatment increased its resistivity. However, for CF1500 and CF2000, which present higher graphitization levels and less heteroatom contents, greater capacitance values were observed after their electrochemical oxidative treatment.     

Preparation and properties of aromatic polymides from 2,2′-bibenzoic acid and aromatic diamines

Aromatic polyamides having inherent viscosities up to 1.8 dL/g were synthesized either by the direct polycondensation of 2,2′-bibenzoic acid with various aromatic diamines or by the low temperature solution polycondensation of 2,2′-bibenzoyl chloride with aromatic diamines. All the aromatic polyamides were amorphous and soluble in a variety of organic solvents including N,N-dimethylacetamide (DMAc), N-methyl-2-pyrrolidone, dimethyl sulfoxide, m-cresol, and pyridine. Transparent and flexible films of these polymers could be cast from the DMAc solutions. These aromatic polymides had glass transition temperatures in the range of 226-306deg;C and began to lose weight around 350°C in air.     

Synthesis of aromatic polyethers by Scholl reaction. II. On the polymerizability of 4,4′-bis(phenoxy)diphenyl sulfones and of 4,4′-bis(phenythiol)diphenyl sulfone

4,4′-Bis(phenoxy)diphenyl sulfone ( 1 ), 4,4′-bis(phenylthio)diphenyl sulfone ( 2 ), and 1 substituted with various electron-donating groups in the phenoxy units were synthesized and polymerized under oxidative reaction conditions. The presence of methyl, tert-butyl, and methoxy groups as substituents on the phenoxy groups of 1 increases both the yield and the solubility of the resulting polymers. The structure-reactivity relationship of the monomers and of the growing species were discussed based on a radical-cation mechanism of polymerization. Monomers of high nucleophilicity and resonance stabilized radical-cation growing species are crucial to achieve polymers of high molecular weight. The structure of the polymers and in several cases of their chain ends were determined by ¹H-NMR spectroscopy. The mechanism of termination and the side reactions occuring during this polymerization process were discussed based on the structure of the resulting polymers.     

Morphological change of the micelle of poly(styrene)-b-poly(2-vinylpyridine)-b-poly(ethylene oxide) induced by binding of sodium dodecyl sulfate

Morphological change of a micelle of poly(styrene)-b-poly(2-vinylpyridine)-b-poly(ethylene oxide) (PS-PVP-PEO) polymer was induced by binding sodium dodecyl sulfate (SDS) to the PVP block in acidic aqueous solutions. The change in the size of SDS/PS-PVP-PEO complexes was detected by dynamic light scattering measurements and atomic force microscopy, and the binding of SDS was confirmed by zeta-potential measurements. When the micelle was free from SDS in acidic aqueous solutions, the hydrodynamic diameter of the micelle was 216 nm, reflecting the extended conformation of the PVP block due to the repulsion between protonated pyridine units. As the cationic PVP block was electrically neutralized with anionic SDS, the diameter was gradually reduced concomitant with the decrease in zeta-potential and finally reached 175 nm when the PVP block was completely neutralized. The decrease in the diameter shows the morphological change of the PVP block from extended to shrunken forms. Further addition of SDS did not cause the changes of the diameter nor zeta-potential. This indicates that SDS was not bound to the PS-PVP-PEO polymer after the PVP block was fully neutralized and that the hydrophobic binding of SDS to the polymer was negligible due to the low concentration of SDS.     

Preparation and properties of novel soluble aromatic polyimides from 4,4′-diaminotriphenylamine and aromatic tetracarboxylic dianhydrides

New aromatic polyimides containing triphenylamine unit were prepared by two different methods, i.e., a conventional two-step method starting from 4,4′-diaminotriphenylamine and aromatic tetracarboxylic dianhydrides and the one-step thioanhydride method starting from the aromatic diamine and aromatic tetracarboxylic dithioanhydrides. Both procedures yielded high-molecular-weight polyimides with inherent viscosities of 0.47–1.17 dL/g. Some of these polymers were soluble in organic solvents such as N,N-dimethylacetamide, N-methyl-2-pyrrolidone, m-cresol, and pyridine. All the polyimides afforded transparent, flexible, and tough films, and the color varied from pale yellow to dark red, depending markedly on the tetracarboxylic acid components. The glass transition temperatures (T_gs) of these polyimides were in the range of 287–331°C and the 10% weight loss temperatures were above 520°C in air. The polyimides prepared by the one-step method exhibited better solubility in organic solvents and had somewhat lower T_gs than the polymers prepared by a conventional two-step method.     

Determination of nonsteroidal anti-inflammatory drugs in human specimens by capillary zone electrophoresis and micellar electrokinetic chromatography

Therapeutic drug monitoring of anti-inflammatory drugs is necessary for the identification of the agents that cause toxic events and for the decision on the treatment for intoxication. Recently, capillary electrophoresis (CE) has been developed for the simple and rapid analyses of a variety of chemical agents. Micellar electrokinetic chromatography (MEKC) can separate acidic, neutral and basic anti-inflammatory drugs in serum. Furthermore, serum samples are directly applied to the CE system without any pretreatments, and some anti-inflammatory drugs can be separated from serum albumin in the MEKC analysis. On the other hand, capillary zone electrophoresis (CZE) enables us to determine a few microg/mL levels of acidic anti-inflammatory drugs with simple running buffer and stacking technique. A rapid and simultaneous determination of several analgesic anti-inflammatory agents, including ibuprofen, acetaminophen, indomethacin, and salicylic acid in human serum has been developed by using CZE. Therefore, the CZE and MEKC analysis may become a potentially useful alternative to high-performance liquid chromatography (HPLC) and fluorescence polarization immunoassay (FPIA) for therapeutic drug monitoring, particularly in serum of patients suffering from intoxication by overdosage of nonsteroidal anti-inflammatory agents.     

The Effect of Ge,Ni, and Fe Doping on the Ga Activity in the CoGa B2 Phase

Summary. Gallium activity in the B2 (CsCl-type) phase of ternary Co–Ga–X (X = Ge, Ni, and Fe) alloys was measured by the EMF method with a stabilized zirconia solid electrolyte. The temperature range was 1050–1250 K and the concentrations of the added elements were 2–6 at-% Ge and Ni, and 1–3 at-% Fe. The reference electrodes were Fe,Fe_xO or Ga,Ga₂O₃. The effect on the activity of gallium in the B2 phase with the addition of other elements was found to be the largest with Ge and the smallest in the case of Ni.     

Syntheses of 10-oxo, 10 alpha-hydroxy, and 10 beta-hydroxy derivatives of a potent kappa-opioid receptor agonist, TRK-820

Syntheses of 10-oxo, 10alpha-hydroxy, and 10beta-hydroxy derivatives of a potent kappa-opioid receptor selective agonist, TRK-820, are described. These derivatives were supposed to be potential degradation products in formulation of TRK-820 as a result of autoxidation. 10-Oxo-TRK-820 11 was derived from 10-oxo-4,5-epoxymorphinan 14 in 10 steps in 32% overall yield. Reduction of the 10-oxo group in 4,5-epoxymorphinan with NaBH(4) gave 10beta-hydroxy-4,5-epoxymorphinan, exclusively. A stepwise inversion method of the 10beta-hydroxy group to produce 10alpha-hydroxy-4,5-epoxymorphinan was established. By HPLC analyses, 10alpha-hydroxy-TRK-820 12 was confirmed to be one of the degradation products in developing formulation of TRK-820.     

Dissolving metal reduction with crown ether — reductive decyanation

Toluene radical anion generated from potassium metal/dicyclohexano-18-crown-6/toluene system has been proved to be highly effective for reductive decyanation reaction of primary, secondary and tertiary cyanides.     

Substoichiometric isotope dilution mass spectrometry as a new analytical method

A novel analytical method, the substoichiometric isotope dilution mass spectrometry (SIDMS) has been proposed. This method consists of the substoichiometric separation of the element in question and the subsequent intensity measurement of a stable isotope of the element with a mass spectrometer. In SIDMS, the correction of the mass discrimination of isotope measurement is not necessary and the use of expensive enriched stable isotopes may be avoided. The validity and the usefulness of SIDMS are demonstrated by the substoichiometric extraction of iron(III) with 4-isopropyltropolone and 3,5-dichlorophenol following microwave-induced plasma mass spectrometry.