Structural determination of subsidiary colors in commercial Food Green No. 3 (fast green FCF, FD & C Green No. 3).

HPLC analysis revealed that eight subsidiary colors existed in commercial Food Green No. 3 (fast green FCF, FD & C Green No. 3). Among them, four subsidiary colors C, F, G, and H were isolated by using preparative HPLC and their structures were determined by MS and NMR. They were the disodium salt of 2-[[4-[N-ethyl-N-(3- sulfophenylmethyl)amino]phenyl][4-[N-ethyl-N-(4- sulfophenylmethyl)amino]phenyl]methylio]-4-hydroxybenzenesulfonic acid (abbreviated as m,p-G-3), the sodium salt of 2-[[(4-N-ethylamino)phenyl][4-[N-ethyl-N-(3- sulfophenylmethyl)amino]-phenyl]methylio]-4-hydroxybenzenesulfonic acid [abbreviated as HSBA-(EA) (m-EBASA)], the sodium salt of 2-[[(4-N-diethylamino)phenyl][4-[N-ethyl-N-(3- sulfophenylmethyl)amino]phenyl]-methylio]-4-hydroxybenzenesulfonic acid [abbreviated as HSBA-(di-EA) (m-EBASA)], and the sodium salt of 2-[[4-[N-ethyl-N-(phenylmethyl)amino]phenyl][4-[N-ethyl-N-(3- sulfophenylmethyl)-amino]phenyl]methylio]-4-hydroxybenzenesulfonic acid [abbreviated as HSBA-(EBA)(m-EBASA)], respectively. HSBA-(di-EA) (m-EBASA) was a subsidiary color newly found in commercial Food Green No. 3.     

Influence of swelling of noncrystalline regions in silk fibers on modification with methacrylamide

The degrees of swelling of noncrystalline regions of domestic and tussah silk fibers were investigated by measuring the small-angle X-ray scattering intensity of the fibers in wet conditions and analyzing the scattering intensity based on a two-phase model, i.e., crystalline regions and water-swollen noncrystalline regions. The influence of the degree of swelling of noncrystalline regions on the graft treatment of these fibers with methacrylamide was investigated. The changes in the structure caused by the graft treatment were also analyzed using the wide-angle X-ray diffraction measurements. As compared with the tussah silk fibers, the domestic silk fibers showed a larger degree of swelling of the noncrystalline regions, and gained a larger amount of resin by the graft treatment. The crystallites with smaller sizes in the tussah silk fibers were destroyed preferentially by the graft treatment. For the domestic silk fibers, the crystallites were destroyed more seriously and rather homogeneously independent of the crystallite sizes. © 1996 John Wiley & Sons, Inc.     

Resinification Behavior of Regenerated Feather Keratin Powder

A preliminary study was performed on the resinification behavior of regenerated feather keratin powder by changing the sintering conditions, and the thermal and mechanical properties for the obtained resin were investigated. It was confirmed that the molding at 140°C was enough to complete the resinification. The resin obtained was amorphous and its glass transition temperature could be raised to 93°C. In addition, the hardness of the resin could be increased from 20–25 HV to 90 HV by leaving the as-sintered compact resin in ambient air at room temperature for 133 days. Crosslinking agents that work even at room temperature seem to be synthesized during the molding.     

Decomposition of Carbon Dioxide to Carbon with Active Wustite at 300°C

Active wustite (FeδO, with a δ value of 0.98) was prepared by keeping normal wustite (δ value of 0.94) in a N₂ atmosphere at 300°C for 10 min. This reaction is given by (4δ₂–3)Fe_δ1O→(4δ₁–3)Fe_δ2O + (δ₂–δ₁)Fe₃O₄ where δ₁= 0.94 and δ₂= 0.98. The equation indicates that the normal wustite undergoes eutectoid decomposition into active wustite and stoichiometric magnetite (Fe₃O₄). Carbon dioxide (1.013 × 10⁵ Pa) was almost completely (100%) decomposed into carbon (zero valence) by the active wustite at the low temperature of 300°C, which was associated with the transformation of the active wustite into the stoichiometric magnetite. The internal pressure of the reaction cell eventually became a vacuum.     

Compression Deformation Mechanism of Silicon Carbide: I, Fine-Grained Boron- and Carbon-Doped β-Silicon Carbide Fabricated by Hot Isostatic Pressing

The deformation behavior of boron- and carbon-doped β-silicon carbide (B,C-SiC) with an average grain size of 260 ± 18 nm containing 1 wt% boron was investigated by compression testing at elevated temperatures. Extensive grain growth during deformation was observed. The stress–strain curves were compensated for grain growth by assuming power-law type of dependence on grain size and strain rate. The stress exponent n was ∼1.3 and the grain size exponent p was ∼2.7 at temperatures ranging from 1593° to 1758°C. The apparent activation energy of deformation Q _d was ∼760 kJ/mol, which was lower than the activation energy for lattice diffusion of silicon and carbon in SiC and higher than that for grain-boundary diffusion of carbon in SiC. These results suggest that the deformation mechanism of the fine-grained B,C-SiC is grain-boundary sliding accommodated by the grain-boundary diffusion.     

Morphological study by TEM on uniaxially oriented thin films of PET, PEN and their blends

Uniaxially oriented thin films of poly(ethylene terephthalate) (PET), poly(ethylene 2,6-naphthalene dicarboxylate) (PEN) and their blends were prepared by applying shear strain to their respective melts, and the resulting morphologies were studied by transmission electron microscopy. Selected-area electron diffraction of each film revealed well-defined uniaxial orientation of polymer chains in the shearing direction. In the uniaxially oriented thin film of PEN, stacked-lamellar structure with the average long period of 27 nm consisting of a crystalline region about 15 nm thick and an amorphous one about 12 nm thick was found here and there in the dark-field image: PEN-type. On the other hand, stacked-lamellar structure was rarely observed in the case of PET: PET-type. In PET/PEN blends, the morphologies changed from the PET-type to the PEN-type with increasing content of PEN.     

Evaluation of a Method to Measure Black Carbon Particles Suspended in Rainwater and Snow Samples

We conducted a detailed evaluation of a method for measuring the mass concentrations and size distributions of black carbon (BC) particles in rainwater and snow. The method uses an ultrasonic nebulizer (USN) and a single particle soot photometer (SP2). The USN disperses sample water into micron-size droplets at a constant rate and then dries them to release BC particles into the air. The masses of individual BC particles are measured by the SP2, using the laser-induced incandescence technique. The loss of BC particles during the extraction from liquid water to air depends on their sizes. We determined the size-dependent extraction efficiency using polystyrene latex (PSL) spheres with 12 different diameters between 107 and 1025 nm. The PSL concentrations in water were measured by the light extinction at 532 nm. The extraction efficiency of the USN showed a broad maximum of about 10% in the diameter range 200–500 nm and decreased substantially at larger sizes. The accuracy and reproducibility of the measured mass concentration of BC in sample water after long-term storage were about ±25% and ±35%, respectively. We tested the method by analyzing rainwater and surface snow samples collected in Okinawa and Sapporo, respectively. The measured number size distributions of BC in these samples showed negligible contributions of BC particles larger than 300 nm to the total number of BC particles. A dominant fraction of BC mass in these samples was observed in the diameter range 100–500 nm.

Copyright 2013 American Association for Aerosol Research     

Incorporation of Dust Particles into a Growing Film During Silicon Dioxide Deposition from a TEOS/O2 Plasma

The effects of gas flow rate on particle formation and film deposition during the preparation of silica thin film using a TEOS/O₂ plasma were investigated. Particle formation and growth are suppressed with increasing gas flow rates. The film deposition rate increases with increasing gas flow rate, reaches a maximum value, and eventually decreases again. However, the uniformity of the film tends to degrade at high gas flow rates. At a high gas flow rate, some particles trapped in the sheath near the grounded electrode pass through the sheath to reach the substrate and are then embedded in the growing film. A self-consistent sheath model combined with particle force balance based on charge fluctuation was developed to explain these experimental findings qualitatively. The model reveals that charge fluctuation is a key factor for the particle to overcome the potential barrier of the negatively charged particles to pass through the sheath, eventually reaching the substrate. The model further shows that the probability of a particle being deposited on the substrate is higher for increased gas flow rates, which correctly predicts the experimentally observed trend.     

Effect of CaO Addition on Compressive Deformation of Silicon Nitride Ceramic with Y‐Mg‐Si‐O‐N Glassy System

Creep behavior of Si₃N₄ polycrystals containing Y₂O₃‐MgO‐SiO₂ glass phase (with and without Calcium oxide [CaO] additive) was studied by compression tests between 1500 and 1700°C. We studied the effect of CaO additive on flow stress, microstructural evolutions, and thermal stability of the intergranular glass phase during deformation. While the addition of CaO did not affect grain size, the flow stress decreased with the amount of CaO. This result suggested that the addition of CaO reduced the viscosity of intergranular glass phase. The addition of CaO further improved the thermal stability of the glass phase by suppressing the evaporation at elevated temperatures.     

Novel High‐Temperature Antiferroelectric‐Based Dielectric NaNbO3–NaTaO3 Solid Solutions Processed in Low Oxygen Partial Pressures

The (1?x)NaNbO₃–(x)NaTaO₃ solid solution was investigated for x ≤ 0.4 in terms of new high‐temperature and high‐permittivity dielectric system that is suitable for base metal inner electrode capacitor applications. The addition of Ta significantly enhanced the resistivity of the dielectric, resulting in superior resistivity than the dielectrics‐formulated BaTiO₃ systems that dominate the multilayer ceramic capacitor dielectric devices. The voltage dependence of the permittivity was also superior to BaTiO₃‐based materials, providing higher capacitance at higher temperatures. A transmission electron microscopy study illustrated that the grains had so‐called core‐shell structure. According to the electron diffraction analysis, the core region had an inhomogeneous structure between antiferroelectric and ferroelectric phases, and shell region had an incommensurate ferroelectric‐like structure. The core and shell region had Nb‐ and Ta‐rich composition, respectively, and their interface was compositionally sharp, implying that shell region was formed via a liquid phase during the sintering process with an incongruent Ta dissolution reprecipitation. We anticipate that these or similar materials based on the alkali‐niobate perovskites can be further enhanced to provide capacitor solutions from 150°C to 250°C, which is an important range for a number of new AC–DC invertor and engine control units.