Multiple determinations in the micro Dumas nitrogen method

Summary A multiple analysis method for the Dumas nitrogen determination has been described. The furnace is provided with eight combustion tubes arranged in a circle around the axis of the furnace. An improved nozzle-type nitrometer, without ground joints, has been designed. The multiple determinations are simultaneously carried out as in usual method, permitting thirty two analyses in a 7-hour working day. The standard deviation-error of estimate from 88 analyses in routine work is ±0.12% N.

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Zusammenfassung Ein Verfahren zur gleichzeitigen Durchführung mehrerer Stickstoffbestimmungen nachDumas wurde beschrieben. Der Verbrennungsofen kann acht Verbrennungsrohre in gleichmäßiger Entfernung von seiner Längsachse aufnehmen. Ein verbessertes Düsenazotometer ohne Schliffverbindungen wurde konstruiert. Die Analysen werden gleichzeitig in der üblichen Art durchgeführt, so daß im 7stündigen Arbeitstag 32 Bestimmungen möglich sind. Die mittlere Abweichung von 88 Analysen im Routinebetrieb betrug ± 0,12% N.

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Résumé On a décrit une méthode d'analyse multiple pour le dosage de l'azote selonDumas. Le four est muni de huit tubes á combustion disposés suivant un cercle autour de l'axe du four. On a construit un nitromètre perfectionné de type à étranglement, sans joints rodés. On effectue simultanément les dosages multiples comme dans la méthode habituelle, ce qui permet de réaliser trente deux analyses en une journée de travail de 7 heures. L'écart type calculé à partir de 88 analyses dans un travail en série est de ±0,12% N.

     

Synthesis and estimation of gelation ability of C3-symmetry tris-urea compounds

C₃-Symmetry tris-urea low molecular weight gelator (LMWG) (1), which shows chemical stimuli responsible for a sol-gel phase transition, was divided into five regions. Based on the division, 22 derivatives were synthesized. The gelation ability of these derivatives was tested in nine organic solvents with a wide range of values for relative static permittivity (?_r=47.2-1.89). Some derivatives showed a better performance as LMWGs than the original tris-urea LMWG (1). For example, the critical gelation concentration (CGC) in acetone was improved from 1.5 wt % to 0.5 wt % by changing the core substituent (18). Highly versatile LMWG for a variety of solvents was obtained by changing the linker moiety (23). Structural information to design tris-urea LMWGs is important to create rationally a functional supramolecular gel.     

Microchip reversed-phase liquid chromatography with packed column and electrochemical flow cell using polystyrene/poly(dimethylsiloxane)

A microchip pressure-driven liquid chromatography (LC) with a packed column and an electrochemical flow cell has been developed by using polystyrene (PS) and poly(dimethylsiloxane) (PDMS). The cylindrical separation column with packed octadecyl silica particles was fabricated in the PS substrate. The three electrode system (working, reference, and counter electrode) for amperometric detection was fabricated onto the PS substrate, using the Au deposition, photolithography, and chemical etching. The detector flow cell was formed by sealing the electrode system with a PDMS chip containing a channel. In this flow cell, the effect of working electrode width (in the direction of flow) on chromatographic parameters, such as peak width and peak resolution were studied in electrode width ranging 50-5,000 microm. The effect of electrode width on sensitivity (current intensity, current density, and S/N ratio) was also examined. The sensitivity was discussed by simulating the concentration profile generated around the working electrode. The effects of the column packing size and the column size on the separation efficiency were examined. In this study, a good separation of three catechins was successfully achieved and the detection limits for (+)-catechin, epicatechin, and epigallocatechin gallate were 350, 450, and 160 nM, respectively.     

Interaction of wheat germ agglutinin with an N-acetylglucosamine-carrying telomer brush accumulated on a colloidal gold monolayer

A disulfide-carrying telomer with many pendent N-acetylglucosamine (GlcNAc) residues (Cys-PMHGlcNAc) was obtained by photo-polymerization of 1-(6'-methacryloylaminohexyl)-2-N-acetoamido-2-deoxy d-glucopyranoside) (MHGlcNAc) using a benzyl N,N-diethyldithiocarbamoyl (BDC) derivative that shows abilities of initiation, transfer, and termination (iniferter). The disulfide-carrying telomer was accumulated on a monolayer of colloidal Au on a glass substrate, and the interaction of wheat germ agglutinin (WGA) with GlcNAc residue at the polymer brush-solution interface was examined by using the localized surface plasmon resonance (LSPR) technique. For comparison, an amphiphile carrying many pendent GlcNAc residues was also prepared with MHGlcNAc and a lipophilic radical initiator and was incorporated in a phospholipid liposome to examine interaction of the GlcNAc residue with WGA on the liposome surface using turbidity measurements. Both the colloidal gold optical device and the liposome showed a concentration-dependent specific binding of WGA, and the GlcNAc-carrying liposome had a detection limit of 100 nM for WGA, whereas that of the colloidal gold device was 10nM. The sugar-carrying telomer-coated device examined here is not only useful as a simple biosensor chip but is also expected to expand our knowledge of bio-related phenomena at the liquid-telomer brush interfaces on a colloidal Au.     

Light irradiation is a factor in the bactericidal activity of silver-loaded zeolite

Silver loaded zeolite (Ag-Z) was previously found to have effective bactericidal activity against Escherichia coli. To understand the mechanisms of bactericidal activity of Ag-Z, role of light irradiation was focused and investigated in this study. In this study, we focused on light irradiation. Antibacterial assay and spectroscopic study revealed that light irradiation enabled Ag-Z to reduce dioxygen to form a reactive oxygen species, which led to bactericidal activity. These results indicate that the onset of bactericidal activity can be controlled by light irradiation.     

Reaction optimization using solid-phase catalysis-CD HTS: Nb-imidazoline-Cu(I)-catalyzed asymmetric benzoylation of 1,2-diols

Catalytic asymmetric benzoylation of 1,2-diols has been developed using a solid-phase asymmetric catalyst. The reaction conditions were optimized by the screening of different metal salts, solvents, bases, and temperatures. High-throughput screening was performed using circular dichroism detection, and the results revealed that Nb-imidazoline-copper(I) in combination with diisopropylethylamine was able to catalyze with high enantioselectivity, giving the monobenzoylated products in high yields and excellent enantiomeric excesses of up to 95% ee. [reaction: see text]     

Optical nanosensor design with uniform pore geometry and large particle morphology

Appropriate design of nanosensors for optically selective, sensitive sensing systems is needed for naked-eye detection of pollutants for environmental cleanup of toxic heavy-metal ions. Mesostructured materials with two- or three-dimensional (2D or 3D) geometries and large particle morphologies show promise as probe carriers, and can therefore be used to reproducibly fabricate uniformly packed nanosensors. This is the first report on the effects of significant key properties of the mesostructured carriers, such as morphology, geometry, and pore shape, on the functionality of optical nanosensor designs. Such mesostructured sensors with superior physical characteristics can be used as components in sensing systems with excellent stability and sensitivity, and with rapid detection response. The nanosensor design can enhance the selectivity even at low concentrations of the pollutant target ions (nanomolar level). Among the nanosensors developed here, the large pore-surface grains of highly ordered 3D monoliths (HOM) exhibited a high adsorption capability of the Pyrogallol Red probe and high accessibility to analyte ion transport, leading to possible naked-eye detection of Sb(III) ions at concentrations as low as 10(-9) mol dm(-3) and at a wide detection range of 0.5 ppb to 3 ppm. A key finding in our study was that our mesostructured nanosensor designs retained highly efficient sensitivity without a significant increase in kinetic hindrance, despite the slight decrease of the specific activity of the electron acceptor/donor strength of the probe functional group after several regeneration/reuse cycles. The results, in general, indicate that large-scale reversibility of optical nanosensors is feasible in such metal-ion sensing systems.     

Orientational isomerism controlled by the difference in electronic environments of a self-assembling heterodimeric capsule

Tetrakis(4-hydroxyphenyl)-cavitand 1 and tetra(4-pyridyl)-cavitand 2 self-assemble into a heterodimeric capsule 1.2 via four ArOH...pyridyl hydrogen bonds in CDCl3. The 1.2 expresses the orientational isomerism of an encapsulated unsymmetrical guest with high orientational selectivity because the electronic environment of the 1 unit is different from that of the 2 unit. For p-ethoxyiodobenzene and 2-iodo-6-methoxynaphthalene encapsulated in 1.2, the iodo group is specifically oriented to the cavity of the 2 unit. The orientational isomeric selectivity for methyl p-acetoxybenzoate and methyl p-ethoxybenzoate within 1.2 is 1:0.11 and 1:<0.05, respectively, wherein the methyl ester group is preferentially oriented to the cavity of the 2 unit. The delicate balance among electrostatic potential repulsion, CH-pi interaction, or CH-halogen (halogen-pi) interaction, in 1.2-guest assembly influences the orientational isomeric selectivity of unsymmetrical guests within 1.2.     

Development of a new software for the X-ray structural analysis of polymer crystals by utilizing the X-ray imaging plate system

A software and some useful tools have been developed for identifying individual x-ray reflectional peaks recorded with an x-ray imaging plate system. These techniques were applied to analyze the crystal structure of uniaxially oriented polymer samples. Characteristic features of the present method may be summarized as follows. (1) The indexing of the observed reflections and the determination of the unit cell parameters can be made easily on the display of the computer. (2) The integrated intensity of the individual component of the overlapped reflections can be evaluated quantitatively through the curve separation technique. The R_merge's for the equivalent reflections were 5–6%, indicating the exact evaluation of the integrated intensities. (3) The thus obtained reflectional data were successfully utilized for the extraction of the initial structural models by the direct method. The actual applications have been made for orthorhombic polyethylene, trigonal polyoxymethylene, and isotactic polybutene-1, giving the refined crystal structures including even the positions of hydrogen atoms in some cases. The reliability factors were 12, 5, and 15%, respectively, for these three polymer cyrstals. © 1997 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 35: 1677–1700, 1997     

Novel materials for electronic device fabrication using ink-jet printing technology

Novel materials and a metallization technique for the printed electronics were studied. Insulator inks and conductive inks were investigated. For the conductive ink, the nano-sized copper particles were used as metallic sources. These particles were prepared from a copper complex by a laser irradiation process in the liquid phase. Nano-sized copper particles were consisted of a thin copper oxide layer and a metal copper core wrapped by the layer. The conductive ink showed good ink-jettability. In order to metallize the printed trace of the conductive ink on a substrate, the atomic hydrogen treatment was carried out. Atomic hydrogen was generated on a heated tungsten wire and carried on the substrate. The temperature of the substrate was up to 60 °C during the treatment. After the treatment, the conductivity of a copper trace was 3 μΩ cm. It was considered that printed wiring boards can be easily fabricated by employing the above materials.