Investigation of the novel mixed-mode stationary phase for capillary electrochromatography. I. Preparation and characterization of sulfonated naphthalimido-modified silyl silica gel

A novel packing material, 3-(4-sulfo-1,8-naphthalimido)propyl-modified silyl silica gel (SNAIP), was prepared for the use as a stationary phase of capillary electrochromatography (CEC). The sulfonic acid groups on SNAIP stationary phase contributed to the generation of electroosmotic flow (EOF) at low pH and served as a strong cation-exchanger. In CEC with SNAIP, a mixed-mode separation was predicted, comprising hydrophobic and electrostatic interactions as well as electrophoretic migration process. In order to understand the retention mechanism on SNAIP, effects of buffer pH, concentration, and mobile phase composition on EOF mobility and the retention factors of barbiturates and benzodiazepines were systematically investigated. Moreover, the retention behavior of barbiturates on SNAIP was investigated and compared with those on octadecyl silica (ODS), phenyl-bonded silica, and 3-(1,8-naphthalimido)propyl-modified silyl silica gel to confirm the presence of pi-pi interaction on its retention mechanism. It was observed that a column efficiency was more than 85,000 N/m for retained compounds and the relative standard deviations for the retention times of EOF marker, thiourea, and five barbiturates were below 2.5% (n = 4). Under an applied voltage of 20 kV and a mobile phase consisted of 5 mM phosphate (pH 3.8) and 40% methanol, the baseline separation of five barbiturates was achieved within 3 min.     

Restriction of stable bundles in characteristic

Let be an algebraically closed field of characteristic . Let be a nonsingular projective variety defined over and an ample line bundle on . We shall prove that there exists an explicit number such that if is a -stable vector bundle of rank at most three, then the restriction is -stable for all and all smooth irreducible divisors . This result has implications to the geometry of the moduli space of -stable bundles on a surface or a projective space.

     

Measurement of reaction rate distributions in a plastic phantom irradiated by 40- and 65-MEV quasi-monoenergetic neutrons

Reaction rate distributions in a plastic phantom were measured with solid state nuclear track detectors and a fission counter for 40- and 65-MeV quasi-monoenergetic neutrons generated by the 7Li(p,n) reactions with 43- and 68-MeV protons at AVF cyclotron of Japan Atomic Energy Research Institute. Measured distributions were compared with calculated ones.     

Advancement of flow-based analysis with alternative chemical reactions and new devices for environmental and biological samples.

This review includes our researches and other methodologies related to flow-based techniques, such as flow injection analysis (FIA) and sequential injection analysis (SIA). The methods will demonstrate semi-and full automated FIA and SIA, including liquid-liquid and liquid-solid extraction. FIA using alternative chemical reactions in the aqueous solution was applied to the trace analysis of metals in biological and environmental samples. For durable liquid-liquid extraction, several phase separators were designed. Moreover, multi-channel FIA with newly designed flow cells and SIA with lab-on-valve devices have been used for the simultaneous and successive determination of metals and organic compounds. On-line solid phase extraction (SPE) has also been proposed for highly sensitive analysis of organic and inorganic compounds.     

Comparison of methods for ordinal lens opacity data from atomic-bomb survivors: univariate worse-eye method and bivariate GEE method using global odds ratio

In analyses of bivariate ordered polytomous cataract data from atomic-bomb survivors, we compared two methods, the univariate worse-eye method, and the bivariate generalized estimating equations (GEE’s) method using global odds ratio by Williamson et al. (Journal of the American Statistical Association, 90, 1432–1437, 1995). When the association was large and only subject level covariates were used, model selection in the univariate and bivariate methods resulted in the same mean model and similar risk estimates. We showed that the mean parameter and the standard error (SE) in the univariate model are emphasized relative to those in the bivariate model, the biases of which are negligible when the association between both eyes is large. Large sample simulation studies indicated that the univariate Wald statistics are slightly conservative. The simulations also showed that, in bivariate cases, irrespective of the degree of association, the independence estimating equations method with robust SE, and the GEE method with model-based and robust SE are almost fully efficient in parameter estimation when only subject level covariates are included in the mean.     

Extraction of uranium from simulated ore by the supercritical carbon dioxide fluid extraction method with nitric acid-TBP complex.

The supercritical fluid extraction (SFE) method using CO(2) as a medium with an extractant of HNO(3)-tri-n-butyl phosphate (TBP) complex was applied to extract uranium from several uranyl phosphate compounds and simulated uranium ores. An extraction method consisting of a static extraction process and a dynamic one was established, and the effects of the experimental conditions, such as pressure, temperature, and extraction time, on the extraction of uranium were ascertained. It was found that uranium could be efficiently extracted from both the uranyl phosphates and simulated ores by the SFE method using CO(2). It was thus demonstrated that the SFE method using CO(2) is useful as a pretreatment method for the analysis of uranium in ores.     

Synthesis and lithium ion insertion/extraction properties of hollandite-type MnO2 prepared by acid digestion of Mn2O3

Single-phase specimens of α-MnO₂ (hollandite-type) and β-MnO₂ (rutile-type) were synthesized by the acid digestion of Mn₂O₃ under reflux conditions. The type of polymorph of MnO₂ products was strongly dependent on the reaction temperature, type of acid used, and its concentration. The pH titration curve of α-MnO₂ displayed a monobasic acid behavior toward Li⁺, but β-MnO₂ showed a poor ion-exchange property. In contrast, both α-MnO₂ and β-MnO₂ acted as a rechargeable active material in a liquid organic electrolyte lithium cell. The initial discharge capacities of both electrodes exceeded 200 mAh/g (cut-off voltage: 2 V). After discharge–charge repetition, the α-MnO₂ structure was still retained without structure collapse, although the β-MnO₂ structure was destroyed. These findings show that Li⁺ ions can be inserted only into the hollandite-type tunnels in α-MnO₂ and cannot diffuse the rutile-type linkages in α-MnO₂ as well as those in β-MnO₂ without structure collapse.     

Enhanced magnetization and ferrimagnetic behavior of normal spinel ZnFe2O4 thin film irradiated with femtosecond laser

We report on spatially selective change of magnetism from paramagnetic to ferrimagnetic-like behaviors in normal spinel ZnFe₂O₄ thin film under irradiation with 780 nm femtosecond laser pulses. The distribution of Zn²⁺ and Fe³⁺ ions in the irradiated region on the film surface becomes disordered because of local heating to high temperatures, and the metastable phase of ZnFe₂O₄ is frozen in by the rapid quenching after irradiation, resulting in the formation of the ferrimagnetic phase. The ferrimagnetic phase reverts to the paramagnetic state by annealing at 800°C. The present technique is useful for two-dimensional patterning of magnetic thin films.     

Brightness Perception of Light Source Colors in Dense Fog

The characteristics of our color vision are affected by various visual environments. In this experiment, we examined how colored lights look in dense fog. We used 12 kinds of colored light as a test stimulus. At first, in the absence of fog, subjects matched brightness of all the test stimuli with a reference white light adjusted to 0.1 cd/m² or 0.5 cd/m² in luminance, respectively. They then evaluated the apparent brightness of the test stimuli in dense fog with magnitude estimation of 10 grades. In the presence of fog, test stimuli containing a yellow component were given the highest point value of brightness, while test stimuli containing a blue component were given the lowest point value of brightness in fog. We are confident that in a visual environment involving fog, these results will be extremely helpful and practical.     

High performance liquid chromatographic determination of mazindol in human plasma.

A simple and convenient high performance liquid chromatographic method with UV detection is described for the determination of mazindol [5-(p-chlorophenyl)-2,5-dihydro-3H-imidazo[2,1-a]isoindol-5-ol] and its major metabolite, 2-(2-aminoethyl)-3-(p-chlorophenyl)-3-hydroxyphthalimidine (Met), in human plasma. The analytes were extracted with ethyl acetate from plasma samples and separated on a C18 column using acetonitrile-0.067 mol dm(-3) phosphate buffer (pH 3.5) (24 + 76 v/v) as a mobile phase. The eluates were monitored at 220 nm. Following complete validation and stability studies, the proposed method proved to be sensitive and precise. The limits of detection were 0.07 and 0.08 ng ml(-1) of plasma for mazindol and Met, respectively. The accuracy and recovery were in the ranges 94-102% and 91-102%, respectively, for both compounds. The intra- and inter-assay precisions were less than 7.6 and 9.2%, respectively, for both compounds. The stability of mazindol under different storage conditions, i.e., at room temperature (rt) and 4 degrees C and with freeze-thaw cycles, was also examined. Mazindol was unstable in plasma samples left at rt and 4 degrees C. The method was applied to the determination of mazindol and Met in the plasma of a patient treated for obesity with mazindol.