Analytical method of cereulide in processed cereal-based foods and milk powder by LC-MS/MS

An LC-MS/MS method for analysis of cereulide, an emetic toxin produced by Bacillus cereus, was developed. Cereulide was extracted from samples, fried rice, pan-fried noodles, red bean paste and baby formula, with methanol and purified using Oasis HLB cartridges. LC separation was performed on a C18 column with a mixture of formic acid solution and methanol containing ammonium formate as a mobile phase, and the mass spectrometer was operated in the positive electrospray ionization mode. Performance evaluation showed that trueness was higher than 70% and repeatability and reproducibility were within 10%. The limits of quantification were lower than 1 μg/kg.     

F‐bar aided edge‐based smoothed finite element method using tetrahedral elements for finite deformation analysisof nearly incompressible solids

A new smoothed finite element method (S‐FEM) with tetrahedral elements for finite strain analysis of nearly incompressible solids is proposed. The proposed method is basically a combination of the F‐bar method and edge‐based S‐FEM with tetrahedral elements (ES‐FEM‐T4) and is named ‘F‐barES‐FEM‐T4’. F‐barES‐FEM‐T4 inherits the accuracy and shear locking‐free property of ES‐FEM‐T4. At the same time, it also inherits the volumetric locking‐free property of the F‐bar method. The isovolumetric part of the deformation gradient ( F ^iso) is derived from the F of ES‐FEM‐T4, whereas the volumetric part ( F ^vol) is derived from the cyclic smoothing of J(=det( F )) between elements and nodes. Some demonstration analyses confirm that F‐barES‐FEM‐T4 with a sufficient number of cyclic smoothings suppresses the pressure oscillation in nearly incompressible materials successfully with no increase in DOF. Moreover, they reveal that our method is capable of relaxing the corner locking issue arising at the corner in the cylinder barreling analysis. Copyright © 2016 John Wiley & Sons, Ltd.     

Stress corrosion cracking of copper in swollen bentonite simulating nuclear waste disposal environment

Stress corrosion cracking (SCC) of pure copper in bentonite clay was examined using a slow strain rate test (SSRT). Bentonite was swollen with pure water or aqueous solutions containing NH₃ of 5 and 10 mM. Thick corrosion films and particulate deposits were formed on the copper surface after the SSRT. Typical tarnish rupture-type SCC occurred on pure copper in swollen bentonite with and without NH₃. The crack propagation rate was enhanced by NH₃. It is confirmed that a thick oxide layer was formed on copper during plastic deformation, resulting in tarnish crack-type SCC. Many particulate deposits observed on the surface were formed due to the rapid dissolution of Cu²⁺ ions to form porous CuO at local deformed sites, regardless of the SCC occurrence.     

UV laser diode with 350.9-nm-lasing wavelength grown by hetero-epitaxial-lateral overgrowth technology

We have demonstrated a UV-laser diode with a lasing wavelength of 350.9 nm, which has a GaN-AlGaN multiquantum-well (MQW) active layer and was grown on low-dislocation-density Al/sub 0.18/Ga/sub 0.82/N template. The Al/sub 0.18/Ga/sub 0.82/N template was produced by the hetero-epitaxial lateral overgrowth technology on the low-cost sapphire substrate, and has partially low-dislocation density of approximately 2/spl times/10/sup 7/ cm/sup -2/. The lasing operation under pulsed current injection was achieved with the threshold current density of 7.3 kA/cm/sup 2/ and the operating voltage of 10.4 V.     

Electrochemical formation of Yb-Ni alloy films by Li codeposition method in a molten LiCl-KCl-YbCl3 system

Electrochemical formation of Yb-Ni alloy films at a Ni cathode was investigated in a molten LiCl-KCl-YbCl₃ (0.5 mol%) at 723 K. A very thin YbNi₂ film (∼100 nm) was formed by potentiostatic electrolysis at 0.10 V (vs. Li⁺/Li) for 24 h. A much thicker YbNi₂ alloy film (∼7 μm) was formed by Li codeposition method (cathodic galvanostatic electrolysis at 50 mA cm⁻²) for 1 h. The formed YbNi₂ films were changed to Yb₂Ni₁₇ and α-Ni phases by anodic potentiostatic electrolysis depending on the applied potentials. The formation potentials of Yb₂Ni₁₇ and YbNi₂ were found to be 0.75 and 0.25 V, respectively.     

Chemical Synthesis of Rare Natural Bile Acids: 11α‐Hydroxy Derivatives of Lithocholic and Chenodeoxycholic Acids

A method for the preparation of 11α‐hydroxy derivatives of lithocholic and chenodeoxycholic acids, recently discovered to be natural bile acids, is described. The principal reactions involved were (1) elimination of the 12α‐mesyloxy group of the methyl esters of 3α‐acetate‐12α‐mesylate and 3α,7α‐diacetate‐12α‐mesylate derivatives of deoxycholic acid and cholic acid with potassium acetate/hexamethylphosphoramide; (2) simultaneous reduction/hydrolysis of the resulting △¹¹‐3α‐acetoxy and △¹¹‐3α,7α‐diacetoxy methyl esters with lithium aluminum hydride; (3) stereoselective 11α‐hydroxylation of the △¹¹‐3α,24‐diol and △¹¹‐3α,7α,24‐triol intermediates with B₂H₆/tetrahydrofuran (THF); and (4) selective oxidation at C‐24 of the resulting 3α,11α,24‐triol and 3α,7α,11α,24‐tetrol to the corresponding C‐24 carboxylic acids with NaClO₂ catalyzed by 2,2,6,6‐tetramethylpiperidine 1‐oxyl free radical (TEMPO) and NaClO. In summary, 3α,11α‐dihydroxy‐5β‐cholan‐24‐oic acid and 3α,7α,11α‐trihydroxy‐5β‐cholan‐24‐oic acid have been synthesized and their nuclear magnetic resonance (NMR) spectra characterized. These compounds are now available as reference standards to be used in biliary bile acid analysis.     

Inkjet Aerosol Generator as Monodisperse Particle Number Standard

The AIST-inkjet aerosol generator (IAG) can generate highly monodisperse solid or liquid aerosol particles in the particle diameter range from 0.3 to 20 μm at precisely known particle generation rates. The device has been developed for evaluating the counting efficiencies of optical and condensation particle counters. Particle generation efficiency of the IAG is defined as the number of aerosol particles generated by one voltage pulse sent to an inkjet head. The 95% confidence interval of the efficiency were 0.998 ± 0.006 within the 0.4 to 10 μm particle diameter range. The efficiencies remained close to unity when the droplet generation rates were within 20–500 s^?1 and 100–900 s^?1 using ultrapure-water and isopropyl alcohol (IPA) as the solvent of the inkjet solution, respectively. The operating aerosol flowrate range of the IAG is currently 0.5 and 1.0 L/min. The coefficients of variations (C.V.) of the size distributions were 2 to 3% indicating the generated particles were highly monodisperse. The generated particle sizes were defined as the volume equivalent diameter, D_ve. The uncertainty analysis on the factors affecting D_ve indicated that 95% confidence interval of the D_ve is expected to be ±5%. The uncertainty of D_ve was entirely caused by the uncertainty of the average mass of a droplet. The reproducibility of particle sizes within 0.5 to 10 μm was evaluated using an aerodynamic particle sizer. The C.V. of the measured particle sizes were less than 6% and 4% when NaCl particles and ionic liquid droplets were generated, respectively.

Copyright 2014 American Association for Aerosol Research     

Selective formation of light olefin by n-heptane cracking over HZSM-5 at high temperatures

The catalytic cracking of n-heptane has been performed over HZSM-5 catalysts with various Si/Al ratios at 723-923 K to form light olefins selectively. The HZSM-5 zeolites with various acid site densities exhibited almost the same selectivity at the same conversion. The ethylene + propylene selectivity increased, while the propylene/ethylene ratio decreased with an increase in reaction temperatures. It is found that a high temperature is required to obtain a high ethylene + propylene yield. The highest ethylene + propylene yield obtained in this study was 59.7 C-% with a propylene/ethylene ratio of ca. 0.72 at 99.6% conversion over HZSM-5 (Si/Al = 31) at 923 K. Moreover, it is concluded from the selectivities and activation energies that the monomolecular cracking is predominant at a high temperature as 923 K.     

Studies on composites from wood and polypropylenes. II

Composites of polypropylene (PP) or maleic-anhydride-modified polypropylene (MPP) with refiner ground pulp (RGP) were prepared under various kneading conditions (mixing temperature, rate of rotation, and mixing time) and evaluated for their tensile strength (σ_max), break elongation (?_max), and Young's modulus (E). Particularly, for the rate of rotation, fiber length distribution and its fibrillation were investigated in connection with mechanical properties of the composites. Also evaluated in this study was the effect of modifiers of PP on the properties. Modified PP that can be grafted or can have affinity to RGP was proved to improve the tensile strength of the molded composites as the RGP content increases, while the strength was decreased for PP–RGP composite without a modifier. MPP was also evaluated as a compatibilizer for the PP–RGP composites, and a tremendous improvement of tensile strength was achieved with MPP addition of only 2.5%, indicating that MPP can act as a compatibilizer in its system. These lines of evidence is interpreted to be caused from the improvement of the adhesion between RGP and PP through localizing MPP at the interface of these two components.     

Production and characterization of oxidized cassava starch (Manihot esculenta Crantz) biodegradable films

Plastic is one of the most common pollutants in the environment. Therefore, the number of studies on the use of biodegradable packaging is increasing. Starch is the primary material used in the production of biodegradable plastics due to its natural abundance and high biodegradability. Yet, the strong hydrophilic character of starch presents a challenge. Therefore, the modification of its structure through oxidation may yield interesting results as the viscosity reduction. The objectives of this work were to obtain cassava (Manihot esculenta Crantz) starch oxidized with 0.8 and 2.0% active chlorine, to develop biodegradable films and characterize their mechanical properties, solubility in water, permeability to water vapor, degree of swelling, and sorption isotherms. Biodegradable films were produced with starch concentrations of 2, 3, 4, and 5% w/w and 25% glycerol (g/100 g starch) added as a plasticizer. Images of the films were obtained with an atomic force microscope and allow to observe a smooth surface and the absence of starch granules in the film produced with oxidized starches. The tensile strength of the biodegradable film produced with oxidized starch (0.8% active chlorine) was 80 MPa. The value of permeability to water vapor was 1.613 × 10⁻⁹ kg/day/m/Pa, and the average solubility was 41%. The sorption isotherms showed that biodegradable films made with oxidized starches cannot be used in environments with relative humidity below 35% or above 90%.