Synthesis of trimellitic anhydride microcapsule toner by liquid‐phase separation

A microcapsule toner containing trimellitic anhydride for use as a foam inhibitor in printing applications was synthesized by liquid‐phase separation in organic solvents. It is possible to determine materials appropriate for the microencapsulation of trimellitic anhydride from solubility parameters calculated on the basis of the molecular structures of raw material candidates. Considering solubility parameters of various polymers, the polyethylene/methacrylic acid copolymer was selected for the microcapsule wall material. In addition, two kinds of solvents, toluene [solvent (a)] and isoparaffin [solvent (b)], were employed. It was necessary for the microcapsule materials to meet the following conditions: (1) the wall material must completely dissolve in solvent (a); (2) the core material must disperse well, but not dissolve in solvent (a); and (3) the wall and core materials must not dissolve in solvent (b). By using mixtures of either lecithin and basic barium petronate or lecithin and basic calcium petronate as charge control agents, the trimellitic anhydride microcapsules could be charged either positively and negatively, respectively. The microcapsule toner fabricated in this method was successfully applied in commercial printing machines, where it inhibited foaming effectively enough to satisfy product requirements in the printing industry. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 90: 3822–3826, 2003     

High-performance polymer-based monolithic capillary column

In this report, we introduce a new entry of high-performance polymer-based monolithic capillary column for mainly small molecules. This capillary column was prepared using a newly introduced epoxy monomer with diamines. Simply heat-induced polycondensation in an appropriate porogenic solvent afforded a really homogeneous co-continuous monolithic structure having submicrometer-size skeletons with micrometer-size through-pores. We were also able to prepare chiral monolithic columns using a chiral epoxy monomer as well as a chiral diamine. A 21.5-cm-long, 100-mum-i.d. column afforded up to 40 000 theoretical plate numbers (N) for alkylbenzenes in 60% aqueous acetonitrile as a reversed-phase-mode stationary phase. Due to a quite low column pressure drop, a 150-cm-long column was prepared. This long column afforded up to 200 000 plates for alkylbenzenes with only a 4-MPa column pressure drop. In contrast, in 100% acetonitrile, this column has "HILIC" property to show up to 60 000 plates for methanol with a 17.5-cm-long column. In this mode, we were able to separate nucleic acids. In addition, we have prepared a chiral column with both of the chiral epoxy monomers and an amine. This column was able to chirally discriminate a racemic alcohol in a reversed-phase mode.     

Sensitive analyses of neutral N-glycans using anion-doped liquid matrix G3CA by negative-ion matrix-assisted laser desorption/ionization mass spectrometry

Negative-ion fragmentation of N-glycans has been proven to be more informative than that of positive-ion. In particular, it defines structural features such as the specific composition of the two antennae and the location of fucose. However, negative-ion formation of neutral N-glycans by matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) remains a challenging task, and the detection limit of N-glycans in negative-ion mode is merely at the subpicomole level. Thus, practical applications are limited. In this study, combinations of five liquid matrices and nine anions were used to ionize N-glycans as anionic adducts, and their performances for sensitive analyses were evaluated. The best results were obtained with anion-doped liquid matrix G(3)CA, which consists of p-coumaric acid and 1,1,3,3-tetramethylguanidine; the detection limits of anion adducted N-glycans were 1 fmol/well for NO(3)(-), and 100 amol/well for BF(4)(-). Negative-ion MS(2) spectra of 1 fmol N-glycans were successfully acquired with a sufficient signal-to-noise ratio and were quite useful for MS-based structural determination. The anion-doped G(3)CA matrix opens the way for sensitive and rapid analysis of neutral N-glycans in negative-ion MALDI at a low femtomole level.     

Fabrication of Ni compound nanocrystal/nanocarbon composites by cooling of chloride-based fluxes

Unique Ni compound nanocrystals were successfully grown on carbon nanotubes (CNTs) by cooling a mixed chloride flux. Cup-stacked CNTs (CSCNTs) were used as the nanocarbon materials because of their structural features. The grown nanocrystals had a nanosheet structure, which was densely assembled and had a ribbon-like morphology. Therefore, the nanocrystal/CSCNT composites were expected to have a highly active surface area for the catalyst composites. The selected area electron diffraction pattern and the related radial intensity profiles indicated that the grown nanocrystals were Ni(OH)2. When the pristine CSCNTs were used as a starting material, the formation efficiency of the nanocrystal/CSCNT composites decreased because the pristine CSCNTs were not dispersed in the KCl-LiCl flux. Therefore, functionalization of the CSCNTs was carried out with VUV light irradiation. The dispersibility of the VUV light-treated CSCNTs increased in the KCl-LiCl flux in comparison with the pristine CSCNTs because oxygen-containing functional groups, such as -COOH and -CO, were introduced onto the surfaces of the CSCNTs.     

Oxidation of green rust suspensions containing different chromium ion species

The oxidation of hydrosulphate green rust (GR2(SO₄²⁻)) suspension containing different chromium ion species was investigated by X-ray diffraction, X-ray absorption spectroscopy and transmission electron microscopy. The pH, oxidation-reduction potential and amount of dissolved oxygen in aqueous solutions were measured during the reactions. The results show that the addition of Cr(III)₂(SO₄)₃ solution suppresses the transformation of GR2(SO₄²⁻) into iron oxyhydroxides and oxides in aqueous solution, while the addition of Na₂Cr(VI)O₄ solution promotes the transformation of GR2(SO₄²⁻) in which Cr(VI) is reduced to Cr(III); α-FeOOH particles were refined by the addition of the chromium ions.     

Preliminary Heat Capacity and Vapor Pressure Measurements of 2D 4He on ZYX Graphite

We report preliminary heat capacity and vapor pressure measurements of the first and second layers of ⁴He adsorbed on ZYX graphite. ZYX is known to have much better crystallinity than Grafoil, the most commonly-used exfoliated graphite substrate, such as a ten-times larger platelet size. This allows us to distinguish different phases in 2D ⁴He much more clearly and may provide qualitatively different insights into this system. We found a significantly asymmetric density-dependence of the heat-capacity peak associated with the $\sqrt{3}\times\sqrt{3}$ phase formation comparing with that obtained with Grafoil. The 2nd-layer promotion density is determined as 11.8±0.3 nm^?2 from the heat-capacity measurement of low density samples in the 2nd layer and vapor pressure measurement.     

HCl emission during co-pyrolysis of demolition wood with a small amount of PVC film and the effect of wood constituents on HCl emission reduction

In this study, HCl emission during the co-pyrolysis of demolition wood and a small amount of polyvinyl chloride (PVC) film (the Cl content of which ranged from 0.5% to 6% by weight) in an N₂ atmosphere at elevated temperatures of up to 600 °C was measured using a laboratory-scale cylindrical batch reactor. In the pyrolysis experiments, HCl emission was reduced by the presence of wood. The effect of the primary constituents of wood (cellulose, hemicellulose, and lignin) on HCl emission was investigated by not only measuring HCl emission and Cl distribution to various phases during the co-pyrolysis of each constituent with PVC film but also by conducting thermogravimetric analysis of the constituents. This investigation first revealed that hemicellulose significantly reduced HCl emission by fixing most of the Cl molecules in a sample into pyrolyzed residue.     

Differences of drivers' reaction times according to age and mental workload

This study was designed to examine differences in reaction times of drivers of various age groups and to assess the influence of mental workload on reaction times. Experiments were performed on a simulated street and under other conditions to identify drivers with long reaction times and drivers whose reaction times are affected strongly by mental workloads while driving on a public road. Reaction times after hearing a buzzer were measured under five conditions: (1) sitting in a stationary vehicle, (2) executing mental calculations in a stationary vehicle, (3) driving on a simulated street, (4) executing mental calculations while driving on a simulated street, and (5) driving on a public road. Subjects were 10 drivers each of three age groups. Each experiment was performed by these subjects under the five conditions. Results showed that mental calculations increased the average reaction time for each age group. Mental calculations increased differences among age groups and individuals, and increased differences in respective drivers' individual performance. Mental calculations influenced elderly drivers' reaction times remarkably. Results also demonstrated that an experiment on a simulated street identified drivers who showed long reaction times on a public road.     

Positive-temperature-coefficient effect of electrical resistivity below melting point of poly(vinylidene fluoride) (PVDF) in Ni particle-dispersed PVDF composites

This paper discusses the positive-temperature-coefficient effects of resistivity in Ni particle-dispersed poly(vinylidene fluoride) (PVDF) composites based on experiment results from SEM, DSC, and pressure-volume-temperature (PVT) measurements. The melting points of composites with Ni content of 20, 30, 40, and 50vol.% were equal to that of pure PVDF. The PTC effects in composites with Ni content of 40 and 50vol.% occurred at temperatures near the melting point of the PVDF matrix, whereas those in composites with Ni content of 20 and 30vol.% occurred at temperatures below the melting point of the PVDF matrix. We found that the PTC effect occurs even without melting of the matrix polymer. Moreover, we determined that a slight increase in specific volume at temperatures below the melting point of the matrix polymer acts fully as a driving force for forming a gap between fillers. This suggestion was backed up by theoretical analyses using percolation theory and a thermal-fluctuation-induced tunneling model.