Determination of mercury in bismuth by neutron activation analysis

A method has been developed for the determination of traces of mercury in bismuth by neutron activation analysis. After sample irradiation at a flux of 7 · 10¹³ n cm^-2 s^-1 for 20 min, mercury was separated from bismuth by addition of ammonium sulfide and re-dissolution of bismuth (matrix) sulfide with nitric acid, and filtration of sulfur containing mercury on a membrane filter. The activity of the 68- or 68–77-keV region, counted with a Ge(Li) or NaI(Tl) detector, was used for quantitative measurements. The method was applied to bismuth samples containing 0.1–100 p.p.m. of mercury.     

Zur Umwandlung von Mackinawit (FeS) in Greigit (Fe3S4) durch Elektronenstrahlen

The continuous variations of reflexion intensities and lattice spacings are observed for the transformation from mackinawite. FeS (tetragonal), to greigite, Fe₃S₄ (cubic). by electron beam heating. At the beginning of the transformation, the (222) reflexion of greigite appears. At the end, the (400) and (220) reflexions of greigite are stronger than those so far reported, and the (311), (422) and (331) reflexions are weaker. The observations suggest, that the (101) plane of mackinawite changes to the (222) plane of greigite. The transformation proceeds by bulk diffusion of sulfur, which initially existed in an amorphous state on the surface of mackinawite.     

Tunable metallization by assembly of metal nanoparticles in polymer thin films by photo- or electron beam lithography

The technique of patterning of surfaces with metal-rich structures on micro- or nanoscales was developed by assembling metal nanoparticles into a thin film of polymer in a controllable way. Palladium (Pd) nanoparticles were incorporated into a thin film of poly(methyl methacrylate) (PMMA) using palladium (II) bis(acetylacetonato), Pd(acac)(2), as a precursor vaporized in a nitrogen atmosphere. Depending upon its dose, the irradiation of a PMMA film by UV light or an electron beam (EB) enhances its reducing capability against Pd(acac)(2). This dependency on dose can be used to control the formation and assembly of Pd nanoparticles. Using this technique, binary patterns consisting of metal-rich and metal-poor regions in the polymer film can be created simply by irradiating the surface of the polymer through a binary photomask. Besides the creation of binary patterns, it is also possible to create grayscale patterns where the density of Pd nanoparticles can be tuned to provide shades of gray by the use of light with continuously modulated intensity. Because the electron beam also enhances the reducing power of PMMA against Pd(acac)(2), it is thus possible to obtain highly metallized films with nanoscale pattern features. The PMMA film can be selectively removed by oxygen plasma treatment or by pyrolysis. Thus, highly metallized surfaces with binary or grayscale patterns can be obtained by selective removal of the PMMA films. The metallized regions possess relatively high resistivity against CF(4) plasma compared to the bare silicon surface; therefore, the metallized surface patterns can be transferred onto the underlying silicon substrate by CF(4) plasma treatment. Because of the nanosize effect of metal nanoparticles, the thermal treatment at 900 degrees C, which is significantly lower than the melting temperature of the bulk Pd, yields continuous metallic features by binding the assembled nanoparticles.     

Synthesis of thieno[2,3‐b][1,5]benzoxazepine derivatives

A new series of 4‐(4‐methylpiperazin‐1‐yl)thieno[2,3‐b][1,5]benzoxazepines 1a‐k has been synthesized from 4‐bromo‐2‐methylthiophene 6 or ethyl 2‐amino‐4,5‐dimethyl‐3‐thiophencarboxylate 10 . Preparation of the key intermediate thieno[2,3‐b][1,5]benzoxazepine‐4(5H)‐ones 4a‐i, 4k were carried out by treatment of 2‐bromo‐N‐(2‐hydroxyphenyl)‐3‐thiophencarboxamides 5a‐i, 5k with potassium carbonate in DMSO. Compounds 1 are thienoanalogues of loxapine, a potent antipsychotic drug. Of these compounds, the neu‐roleptic activity of 2‐methyl‐4‐(4‐methylpiperazin‐l‐yl)thieno[2,3‐b][1,5]benzoxazepine 1a (R¹, R³=H, R²=CH₃) demonstrated potent antipsychotic activity.     

Direct catalytic asymmetric aldol-Tishchenko reaction

A direct catalytic asymmetric aldol reaction of propionate equivalent was achieved via the aldol-Tishchenko reaction. Coupling an irreversible Tishchenko reaction to a reversible aldol reaction overcame the retro-aldol reaction problem and thereby afforded the products in high enantio and diastereoselectivity using 10 mol % of the asymmetric catalyst. A variety of ketones and aldehydes, including propyl and butyl ketones, were coupled efficiently, yielding the corresponding aldol-Tishchenko products in up to 96% yield and 95% ee. Diastereoselectivity was generally below the detection limit of 1H NMR (>98:2). Preliminary studies performed to clarify the mechanism revealed that the aldol products were racemic with no diastereoselectivity. On the other hand, the Tishchenko products were obtained in a highly enantiocontrolled manner.     

Mechanical properties and enzymatic degradation of poly[(R)-3-hydroxybutyrate] fibers stretched after isothermal crystallization near Tg

Poly[(R)-3-hydroxybutyrate] (P(3HB)) fibers with high tensile strength were prepared by stretching the fibers after isothermal crystallization near the glass transition temperature. Two samples with different molecular weights (M_w = 0.7 × 10⁶ and 4.3 × 10⁶) were used to investigate the effect on tensile strength. Increasing the time for isothermal crystallization of P(3HB) fibers resulted in a decrease in the maximum draw ratio. But, the tensile strength of P(3HB) fibers increased remarkably when the isothermal crystallization time was prolonged to more than 24 h. The tensile strength of low-molecular-weight drawn fibers was higher than that of high-molecular-weight fibers. Therefore, it can be concluded that this procedure does not increase the tensile strength of the high-molecular-weight drawn fibers. This is because, in this drawing method, small crystal nuclei grow initially during the isothermal crystallization process. Then, the molecular chains between the small crystal nuclei that acted as the entanglement points are oriented by stretching. In the case of the high-molecular-weight fibers, because the molecular length between the entanglement points of the small crystal nuclei is too long, the molecular chains are not sufficiently oriented by the stretching process. However, in the case of the low-molecular-weight fibers, the molecular length is suitable for generating the extended chains. Based on the result of X-ray analysis of P(3HB) fibers stretched after isothermal crystallization, fibers have the oriented α-form crystal with 2₁ helix conformation and β-form with planar zigzag conformation. The enzymatic degradation of the stretched P(3HB) fibers was performed by using an extracellular PHB depolymerase purified from Ralstonia pickettii T1. The enzymatic erosion rate of β-form was faster than that of α-form in the P(3HB) fibers stretched after isothermal crystallization.     

The Adsorption of CHClF2 on NaY5.6 Zeolite

The adsorption of CHClF₂ on NaY5.6 zeolite has been studied by measuring the H and F NMR of the adsorbed CHClF₂, focusing in particular on the measurements of the chemical shift and longitudinal relaxation time, as well as the adsorption isotherm measurements. It is possible to determine the coordination structure of the CHClF₂ adsorbed on NaY5.6 zeolite by measuring the adsorption amount dependence of the chemical shift. In addition, the motional activity of the adsorbed molecules in the super cage of the zeolite is discussed on the basis of observed longitudinal relaxation times for various adsorption amounts.     

Twelve hours exposure to inhomogeneous high magnetic field after logarithmic growth phase is sufficient for drastic suppression of Escherichia coli death.

When Escherichia coli B was aerobically grown at 43 degrees C in a medium whose concentration was one-fourth that of the Luria-Bertani (LB) medium supplemented with 1.5 g/l of glutamic acid, drastic cell death was observed after the end of the logarithmic growth phase. However, when the same experiment was conducted under inhomogeneous 5.2-6.1 T magnetic field, cell death was extremely suppressed and the ratio of viable cell number under high magnetic field to that under geomagnetic field reached as much as 100,000. When the magnetic field exposure was restricted to 12 h after the logarithmic growth phase, a similar high degree of suppressive effect on the death was observed. The findings that the amount of sigma S protein encoded by the rpoS gene under the high magnetic field was larger than that under the geomagnetic field, and that the magnetic field effect disappeared when the rpoS gene-deficient strain was cultivated under the high magnetic field, suggest the interaction of magnetic field with a stationary phase specific gene.     

Narrow bandwidth operation of high-power broad-area diode laser using cascaded phase-conjugate injection locking

A broad-area laser is injection-locked by another broad-area laser that is also injection-locked by a single-mode diode laser. Two double-phase conjugate mirrors of photorefractive BaTaO₃ are used to couple the master laser beams to the first slave laser, and the first slave laser output to the second slave laser. One of the double-phase conjugate mirrors is built up with the beams from two broad-area lasers. Two slave lasers are oscillating in single longitudinal mode at 808.5 nm and the spectral width is the same as that of the master laser. Final single-mode output power from the second slave broad-area laser is 840 mW, which is limited by the power of the injection beam. This work verifies the possibility of the multi-stage cascaded injection locking of high-power diode lasers with phase-conjugate injection. Received: 18 November 1998 / Revised version: 29 January 1999 / Published online: 7 April 1999     

Matrix Projection Exposure Using an Analogue Liquid Crystal Display Panel in Place of a Reticle

The most serious problems for the matrix projection exposure using a liquid crystal display (LCD) panel in place of a reticle are largely solved by a new breakthrough method. LCD matrix exposure is effective for small volume productions of print circuits, screen masks, micromachine parts, and other items. Since no reticles are needed, all reticle costs are saved, and turnaround times required for changing the patterns are greatly shortened. However, in the conventional method, pattern widths and positions were strictly restricted depending on the geometric size and pitch of the liquid crystal cells. In this paper, a new concept appointing the cell brightness grades continuously using an analogue interface LCD panel is proposed. Calculating the image intensity distributions for various appointments of cell brightness balances to print same wide patterns, it is clarified that the pattern widths and positions are not much different if the pattern widths are wider than 2 cell pitches of the LCD panel. Maximum width and position variations are less than ± 10% even when the patterns are printed at arbitrary positions, of course including halfway ones. The calculated results are proved by experiments using an analogue LCD panel with a cell pitch of 15 μm. Though the cell size are 13 × 10 μm², and different in x and y directions, almost same wide line-and-space patterns are successfully printed at all positions by only one exposure. It is not necessary to shift the reticle for overlapping exposures to print smooth patterns. Oblique patterns and complicated Chinese character patterns are also printed at arbitrary positions. The new breakthrough technology will make the LCD matrix exposure promising for wide uses of printing various rough patterns easily at small costs.