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91.
Yoko Aomura Yoshihiko KobayashiYuzuru Miyazawa Hideharu Shimizu 《Journal of chromatography. A》2010,1217(11):1838-1844
Rapid analysis of trace permanent gas impurities in high purity ammonia gas for the microelectronics industry is described, using a gas chromatograph equipped with a phtoionization detector. Our system incorporates a reactive precolumn in combination with the analytical column to remove the ammonia matrix peak that otherwise would complicate the measurements due to baseline fluctuations and loss of analytes. The performance of 21 precolumn candidate materials was evaluated. Copper sulfate pentahydrate (CuSO4·5H2O) was shown to selectively react with ammonia at room temperature and atmospheric column pressures, without affecting the hydrogen, oxygen, nitrogen, methane or carbon monoxide peak areas. To prevent loss of trace carbon dioxide, an additional boron trioxide reactant layer was inserted above the copper sulfate pentahydrate bed in the reactive precolumn. Using the combined materials, calibration curves for carbon dioxide proved to be equivalent in both ammonia and helium matrix gases. These curves were equivalent in both matrix gases. The quantitative performance of the system was also evaluated. Peak repeatabilities, based on eight injections, were in the range of 4.1–8.2% relative standard deviation; and detection limits were 6.9 ppb for H2, 1.8 ppb for O2, 1.6 ppb for N2, 6.4 ppb for CH4, 13 ppb for CO, and 5.4 ppb for CO2. 相似文献
92.
93.
Konno Y. 《Journal of multivariate analysis》1995,52(2)
Suppose that we have (n − a) independent observations from Np(0, Σ) and that, in addition, we have a independent observations available on the last (p − c) coordinates. Assuming that both observations are independent, we consider the problem of estimating Σ under the Stein′s loss function, and show that some estimators invariant under the permutation of the last (p − c) coordinates as well as under those of the first c coordinates are better than the minimax estimators of Eaten. The estimators considered outperform the maximum likelihood estimator (MLE) under the Stein′s loss function as well. The method involved here is computation of an unbiased estimate of the risk of an invariant estimator considered in this article. In addition we discuss its application to the problem of estimating a covariance matrix in a GMANOVA model since the estimation problem of the covariance matrix with extra data can be regarded as its canonical form. 相似文献
94.
Yousuke Konno Hiroto Kudo Atsushi Kameyama Tadatomi Nishikubo 《Journal of polymer science. Part A, Polymer chemistry》2004,42(10):2543-2550
Fluorine‐containing polyethers with pendant hydroxyl groups were synthesized by the polyaddition of fluorine‐containing bis(epoxide)s with certain fluorine‐containing diols with quaternary onium salts as catalysts. When the polyaddition was performed with 2,2′,6,6′‐tetrafluoro‐4,4′‐biphenol diglycidiyl ether and 2,2′,6,6′‐tetrafluoro‐4,4′‐biphenol, the corresponding polyether with pendant hydroxyl groups was successfully obtained in good yield. The polyaddition of certain fluorine‐containing bis(epoxide)s with diols also proceeded in bulk to provide the corresponding fluorine‐containing polyethers with high molecular weights. These polyethers were highly transparent at 157 nm for 0.1 μm thickness, with their transmittance of 14–75% at 157 nm. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 42: 2543–2550, 2004 相似文献
95.
Yoshihiko Konno 《Journal of multivariate analysis》2007,98(2):295-316
In this paper the problem of estimating a covariance matrix parametrized by an irreducible symmetric cone in a decision-theoretic set-up is considered. By making use of some results developed in a theory of finite-dimensional Euclidean simple Jordan algebras, Bartlett's decomposition and an unbiased risk estimate formula for a general family of Wishart distributions on the irreducible symmetric cone are derived; these results lead to an extension of Stein's general technique for derivation of minimax estimators for a real normal covariance matrix. Specification of the results to the multivariate normal models with covariances which are parametrized by complex, quaternion, and Lorentz types gives minimax estimators for each model. 相似文献
96.
Yoshihiko Yamamoto Hideyuki Takagishi Kenji Itoh 《Journal of the American Chemical Society》2002,124(1):28-29
In the presence of 10 mol % Cp*Ru(cod)Cl, 1,6-diynes with a tertiary center at 4-position reacted with various isothiocyanates at their C=S double bond to afford bicyclic (2H)-thiopyranimines in 35-88% yields. The (2H)-thiopyran structure was unequivocally determined by X-ray analysis. The cycloaddition of carbon disulfide with a diyne similarly gave the expected bicyclic dithiopyrone in 50% yield. 相似文献
97.
Flufenamic acid (FFA) was mixed with magnesium aluminum silicate (MAS) and stored at 60 degrees C at a reduced pressure of about 2.5 mmHg. After storage, when its concentration was not more than 20%, FFA was observed by X-ray diffraction and polarizing microscopy to be amorphous. The dissolution of FFA was thus enhanced in comparison with that of a freshly prepared mixture. Furthermore, the dissolution curves showed a typical supersaturation pattern, and the supersaturation state continued longer, the higher the pH value of the dissolution medium. Flufenamic acid, in a mixture with MAS, became amorphous more rapidly at reduced pressure than at atmospheric pressure, and therefore the effect of improved dissolution appeared earlier at reduced pressure. Infrared spectral studies suggested that FFA, after storage at a reduced pressure with MAS, was dispersed monomolecularly in an ionic form. The technique of treating crystalline medicinals, that have poor solubility in water, with adsorbent at reduced pressure may be useful for improving their dissolution characteristics. 相似文献
98.
99.
Miki ItoFujiko Konno Takuya KumamotoNoriyuki Suzuki Masatoshi KawahataKentaro Yamaguchi Tsutomu Ishikawa 《Tetrahedron》2011,67(41):8041-8049
Both enantiomers of chelidonine, a B/C-cis-11-hydroxyhexahydrobenzo[c]phenanthridine alkaloid, were synthesized by manipulation of the B/C-dehydro ring juncture of benzo[c]phenanthridine skeleton using Sharpless asymmetric dihydroxylation and stereospecific catalytic hydrogenation after introduction of oxygen functions on the C ring as key reaction steps for the construction of stereogenic centers. 相似文献
100.
Tanaka H Zaima N Yamamoto N Suzuki M Mano Y Konno H Unno N Setou M 《Analytical and bioanalytical chemistry》2011,400(7):1873-1880
Arteriovenous fistulae (AVF) using vein grafts are frequently used for vascular access in hemodialysis. When superficial veins
are used as autogenous access grafts for hemodialysis, atherosclerotic-like tissue degeneration often causes stenosis and
obstruction. Although the differences between the pathology of degeneration in AVF and atherosclerosis (i.e., peripheral artery
occlusive disease (PAD)) are known, their underlying molecular mechanisms are not. We determined the characteristic abnormal
lipid metabolism of AVF. Oil red O staining clearly showed the accumulation of lipid molecules in AVF and PAD tissues. We
found that the staining pattern was different between AVF and PAD tissues. The media and adventitia of AVF and the intima
and media of PAD were intensely stained. Quantitative lipid analysis revealed that the amount of PL was significantly increased
in AVF and PAD. Next, we performed matrix-assisted laser desorption/ionization imaging mass spectroscopy and determined the
characteristic distribution of lysophosphatidylcholine (LPC) and phosphatidylcholine (PC) in AVF. The distribution patterns
of LPC (1-acyl 16:0) and PC (diacyl 16:0/20:4) were consistent with the Oil red O staining images, suggesting that metabolisms
related to LPC (1-acyl 16:0) and PC (diacyl 16:0/20:4) are altered in AVF. 相似文献