Perpendicular oriented cylinders via directional coalescence of spheres embedded in block copolymer films induced by solvent annealing

Polystyrene-b-poly(methyl acrylate) (PS-b-PMA) block copolymer with PS volume fraction of 25.2 vol% was synthesized by atom transfer radical polymerization. Non-pretreated silicon wafers were used as the substrates to prepare perpendicular oriented PS cylinders in PMA matrix via solvent annealing which could induce the transformation of spheres to vertically oriented and hexagonally packed cylinders. The spherical microdomains were formed after the evaporation of solvents from the solutions of the block copolymer in selective solvents mixed from methanol, acetone and dichloromethane. The thickness of films could be as thick as 1000 nm, which were much thicker than usual cases and the cylinders came from the directional coalescence of the spheres, thus any pre-treatments of the substrates were not required for perpendicular orientation. The structures were characterized by small angle X-ray scattering (SAXS), transmission electron microscope (TEM), atom force microscopy (AFM) and grazing incidence small angle X-ray scattering (GISAXS).     

Partially biobased polyamphiphile-bearing reactive epoxy groups in the side chains and its application to the hydrogel

Partially biobased polyamphiphile-bearing reactive epoxy groups in the side chains were obtained in 62–78 % yields by a radical copolymerization of limonene oxide (LO) and PEG methylacrylate (PEGA) with different feed ratios. Degree of LO incorporation into the copolymer was determined as 12–23 % by ¹H NMR spectroscopic analysis. The copolymer having LO unit:PEGA unit = 19:81 formed polymer associates in water, particle diameter of which was ranged mainly from 4 to 66 nm and hydrodynamic mean diameter was 12.3 nm. Its critical micelle concentration was determined as 0.53 g/L by fluorescence spectroscopic analysis. A cross-linking reaction of the epoxy groups in the side chains was conducted with 3.97 mol% (to the epoxy group) of branched poly(ethylene imine) as a cross-linker to give the corresponding hydrogel in 56 % yield. The hydrogel can absorb water as much as 13 times its own mass.     

Lightning occurrence data observed with lightning location systems of electric power companies in Japan: 2009–2013

Nine electric power companies in Japan have been collecting lightning data with lightning location systems. Five years of the lightning data (2009–2013) are summarized and analyzed in this paper. The recent annual number of lightning flashes of which the current is more than 10 kA in Japan is around 1 million. The variations of lightning occurrence characteristics by areas, seasons, and so on, are clarified. Meteorological conditions that may affect lightning occurrence are also discussed. Furthermore, we show that there is a clear correlation between the number of lightning strikes and the outage rate of transmission lines. © 2016 Institute of Electrical Engineers of Japan. Published by John Wiley & Sons, Inc.     

Automated single nucleotide polymorphism typing using bead array in capillary tube

A low-cost and simple on-site technique for genotyping single nucleotide polymorphisms (SNPs) was developed. The technique is based on allele-specific primer PCR and the recently developed bead arrays in a single tip technique. The performance of the method was verified by genotyping four SNPs that correlate with cardiovascular diseases.     

In Vitro and in Vivo Characteristics of Fluorapatite-Forming Calcium Phosphate Cements

This study reports for the first time in vitro and in vivo properties of fluorapatite (FA)-forming calcium phosphate cements (CPCs). The experimental cements contained from (0 to 3.1) mass % of F, corresponding to presence of FA at levels of approximately (0 to 87) mass %. The crystallinity of the apatitic cement product increased greatly with the FA content. When implanted subcutaneously in rats, the in vivo resorption rate decreased significantly with increasing FA content. The cement with the highest FA content was not resorbed in soft tissue, making it the first known biocompatible and bioinert CPC. These bioinert CPCs might be useful for applications where slow or no resorption of the implant is required to achieve the desired clinical outcome.     

In Vivo Characteristics of Premixed Calcium Phosphate Cements When Implanted in Subcutaneous Tissues and Periodontal Bone Defects

Previous studies showed that water-free, premixed calcium phosphate cements (Pre-CPCs) exhibited longer hardening times and lower strengths than conventional CPCs, but were stable in the package. The materials hardened only after being delivered to a wet environment and formed hydroxyapatite as the only product. Pre-CPCs also demonstrated good washout resistance and excellent biocompatibility when implanted in subcutaneous tissues in rats. The present study evaluated characteristics of Pre-CPCs when implanted in subcutaneous tissues (Study I) and used for repairing surgically created two-wall periodontal defects (Study II). Pre-CPC pastes were prepared by combining CPC powders that consisted of CPC-1: Ca(4)(PO(4))(2)O and CaHPO(4), CPC-2: α-Ca(3)(PO(4))(2) and CaCO(3) or CPC-3: DCPA and Ca(OH)(2) with a glycerol at powder-to-liquid mass ratios of 3.5, 2.5, and 2.5, respectively. In each cement mixture, the Ca to P molar ratio was 1.67. The glycerol contained Na(2)HPO(4) (30 mass %) and hydroxypropyl methylcellulose (0.55 %) to accelerate cement hardening and improve washout resistance, respectively. In Study I, the test materials were implanted subcutaneously in rats. Four weeks after the operation, the animals were sacrificed and histopathological observations were performed. The results showed that all of the implanted materials exhibited very slight or negligible inflammatory reactions in tissues contacted with the implants. In Study II, the mandibular premolar teeth of mature beagle dogs were extracted. One month later, two-wall periodontal bone defects were surgically created adjacent to the teeth of the mandibular bone. The defects were filled with the Pre-CPC pastes and the flaps replaced in the preoperative position. The dogs were sacrificed at 1, 3 and 6 months after surgery and sections of filled defects resected. Results showed that one month after surgery, the implanted Pre-CPC-1 paste was partially replaced by bone and was converted to bone at 6 months. The pockets filled with Pre-CPC-2 were completely covered by newly formed bone in 1 month. The Pre-CPC-2 was partially replaced by trabecular bone in 1 month and was completely replaced by bone in 6 months. Examination of 1 month and 3 month samples indicated that Pre-CPC-2 resorbed and was replaced by bone more rapidly than Pre-CPC 1. Both Pre-CPC pastes were highly osteoconductive. When implanted in periodontal defects, Pre-CPC-2 was replaced by bone more rapidly than Pre-CPC-1.     

Effect of magnetron sputtering conditions and subsequent annealing on the structure and magnetic properties of Fe97−x Zr3N x films

X-ray diffraction analysis was used to study the structure of Fe_97?x Zr₃N _x thin films produced under different conditions of rf magnetron sputtering (on rotary and stationary substrates) and subsequent annealing. Either a single-phase structure, namely, a supersaturated bcc α-(FeN) solid solution, or a mixed structure that consists of two crystalline phases, such as a supersaturated bcc α-Fe(N) solid solution and an fcc Fe₄N nitride, and a Fe-based amorphous phase were shown to be formed in films deposited on either stationary or rotating substrate, respectively. As the annealing temperature increases, the content of nitrogen in the bcc phase decreases; the grain size of the bcc phase in the films deposited on rotating and stationary substrates increases from 8 to 14 nm and from 10 to 30 nm, respectively; the amount of the Fe₄N phase increases. The results of the study of the magnetic properties of the films are reported. The maximum saturation induction B _s reached is 1.8–1.9 T; the minimum coercive force H _c is 1 Oe. The optimum combination of the magnetic properties (B _s = 1.8–1.9 T and H _c = 1.5–1.8 Oe) is observed for the films deposited on the rotating substrate and subsequently annealed at 400°C.     

Negative staining--carbon replica method, a new procedure to reveal ultrastructure of freeze-fractured membrane.

The present study was undertaken to report a new method which reveals the ultrastructure of freeze-fractured membrane faces. The method consists of initial replication of fractured surfaces of frozen specimens with evaporated carbon and treatment of the replicas with a negative staining solution after dissolution of specimens. This negative staining-carbon replica method reveals clear distribution, ultrastructures and precise size of intramembrane particles on the fractured membrane faces by means of density difference of negative staining solution which is deposited on the surfaces of carbon replicas.     

Enzymatic enrichment of arachidonic acid from Mortierella single-cell oil

An attempt was made to enrich arachidonic acid (AA) from Mortierella single-cell oil, which had an AA content of 25%. The first step involved the hydrolysis of the oil with Pseudomonas sp. lipase. A mixture of 2.5 g oil, 2.5 g water, and 4000 units (U) Pseudomonas lipase was incubated at 40°C for 40 h with stirring at 500 rpm. The hydrolysis was 90% complete after 40 h, and the resulting free fatty acids (FFA) were extracted with n-hexane (AA content, 25%; recovery of AA, 91%). The second step involved the selective esterification of the fatty acids with lauryl alcohol and Candida rugosa lipase. A mixture of 3.5 g fatty acids/lauryl alcohol (1:1, mol/mol), 1.5 g water, and 1000 U Candida lipase was incubated at 30°C for 16 h with stirring at 500 rpm. Under these conditions, 55% of the fatty acids were esterified, and the AA content in the FFA fraction was raised to 51% with a 92% yield. The long-chain saturated fatty acids in the FFA fraction were eliminated as urea adducts. This procedure raised the AA content to 63%. To further elevate the AA content, the fatty acids were esterified again in the same manner with Candida lipase. The repeated esterification raised the AA content to 75% with a recovery of 71% of its initial content.