Characterizations for Vinylimidazolium Based Ionic Liquid Polymer Stationary Phases for Capillary Gas Chromatography

Six polyvinylimidazolium based ionic liquids were prepared for use as stationary phases for gas chromatography. The influences of the attached side-chains (hexyl-, octyl- and phenylpropyl-) on the vinylimidazolium cations and of different counter ions (bromide, hexafluorophosphate, bis-trifluoromethanesulfonlyimide, and bis-trifluoroethanesulfonylimide) were studied. Linear solubility parameter experiments were conducted to characterize the specific interactions of these stationary phases. Some of the polymerized ionic liquid stationary phases exhibited unique structural selectivity. m-, and p-xylenes could be distinguished. The preparation of the polymerized ionic liquid column is simple and reliable. This work provides detailed information for designing polymerized ionic liquids, and shows that these materials have great potential extending the range of options for stationary phases in gas chromatography.     

High uniform illumination of light-emitting diodes lighting with applying the multiple-curvature lens

Light-emitting-diode (LED) sources will play a very important role in the future. Nowadays, there are many traditional light sources gradually being replaced by LED sources. From the viewpoint of illumination, different environments have the same requirement uniformity of illumination. The basic reason for this is to insure human comfort. Therefore, the promotion of illumination uniformity is an especially important key issue. In this article, we propose one effective design to improve the uniformity of illumination of LEDs with Lambertian radiation profiles by inserting into the lighting system, multiple-curvature lens. The enhanced illumination uniformity of LEDs, in this system, is due to energy redistribution by controlling the direction of incident light, using geometrical optics theory. Ray tracing was applied for the simulations required. Finally, the uniformity of illumination is 76.17% in LEDs using multiple-curvature lens, which is twice the uniformity of conventional LEDs. Furthermore, the phenomenon of overload in the multiple-curvature lens is reduced by increasing the numbers of rings on the lens. The overload is less than 0.02 lm in the case of lens designed with 23 rings.     

Calculating specific absorbed fractions with standard Korean male adults

Based on data representing standard Korean male adults, a mathematical anthropomorphic phantom was developed to calculate the specific absorbed fraction for several organs. The results were then compared against values calculated with other phantoms (OTOKO of Japan, MIRD of the U.S. and GOLEM of Germany). We compared the specific absorbed fractions of six organs (the adrenals, kidneys, liver, lungs, pancreas and spleen) for two cases: when the source and target organs are the same, and when they are different. When both the source and target organs are the same the organ with the highest specific absorbed fraction regardless of energy level was found to be the adrenals in all phantoms. In comparing phantoms, the phantom developed on the basis of standard Koreans produced the highest specific absorbed fraction. Also, as a result of conducting an assessment by separating source organs from target organs, the phantom developed on the basis of standard Koreans displayed relatively high specific absorbed fractions although there were slight differences per organ.     

Maximum-entropy TFμSR study of vortex states in 1/2/3 cuprates

A maximum-entropy (ME) method has been applied to TFSR vortex data of RBa₂Cu₃O₇ (R1237; R=Er, Gd and Eu). The obtained information on the field distribution is of much better quality than that resulting from Fourier transformation and curve-fitting of the same data. ME application to R1237 TFSR data taken below T_c at LAMPF show asymmetrical, nearly triangular, field distributions, which broaden with decreasing temperature. Significant deviations from Abrikosov predictions have been observed for the estimated R1237-vortex field distributions. Below 10 K, for Er1237 and Gd1237, the non-Abrikosov features appear to be influenced by the rare-earth magnetism. The low-field tail in the field distribution and the ME-intensity anomaly near T_c suggest glassy features in the 1/2/3 cuprate vortex states.     

Nucleophilic substitution reactions of aryl dithioacetates with pyridines in acetonitrile

Kinetic studies of the pyridinolysis (XC(5)H(4)N) of aryl dithioacetates (CH(3)C(=S)SC(6)H(4)Z) are carried out in acetonitrile at 60.0 degrees C. A biphasic Br?nsted plot is obtained with a change in slope from a large value (beta(X) congruent with 0.9) to a small value (beta(X) congruent with 0.4) at pK(a) degrees = 5.2, which is attributed to a change in the rate-limiting step from breakdown to formation of a zwitterionic tetrahedral intermediate, T(+/-), in the reaction path as the basicity of the pyridine nucleophile increases. A clear-cut change in the cross-interaction constants rho(XZ) from a large positive value (rho(XZ) = +1.34) to a small negative value (rho(XZ) = -0.15) supports the mechanistic change proposed.     

Effects of pH During the Base Catalyzed Reaction of Two-Step Acid/Base Catalyzed Process on the Microstructures and Physical Properties of Poly(dimethylsiloxane) Modified Silica Xerogels

Poly(dimethylsiloxane) (PDMS) modified silica xerogels were prepared by two-step acid/base catalyzed sol-gel process. By keeping the acid amount and hydrolysis period in acidic environment fixed, and adding different amounts of base to the sol afterwards, attempts had been made to study the effect of the different amounts of base catalyst on the micro-structure and physical properties of the prepared ORMOSILs. DTA, SEM, BET, FTIR were performed to characterize the derived specimens. The microstructure and physical properties are greatly influenced by the amount of base added to the sol. With increasing base content the crystallite size and porosity increase and the pore size distribution takes a broad spectrum. Whereas, the glass transition temperature seems to decrease with increasing of base catalyst amount. This is explained in terms of the change in the relative amounts of hydrolysis and condensation reactions due to the addition of different amount of base catalyst, which predominantly influences the condensation reactions. The results are reported in this communication along with possible explanations behind the observations.     

Capillary electrophoresis of baclofen with argon-ion laser-induced fluorescence detection

A capillary electrophoretic method with laser-induced fluorescence detection for baclofen (4-amino-3-p-chlorophenylbutyric acid) has been developed. 6-Carboxyfluorescein succinimidyl ester was used for precolumn derivatization of the non-fluorescent drug. Optimal separation and detection were obtained with an electrophoretic buffer of 50 mM sodium borate (pH 9.5) and an air-cooled argon-ion laser (excitation at 488 nm, emission at 520 nm). Linearity (r > or = 0.99) over three orders of magnitude was generally obtained and the lowest derivatizable concentration limit for baclofen in aqueous solution was 10 nM (2 ng baclofen/ml). Coupled with a simple clean up procedure, the method can be applied to the analysis of baclofen in human plasma at micromolar level. Recovery of spiked baclofen in plasma was 95%. The relative standard deviation values on peak size (0.5 microM level) and migration time were 8.2 and 1.0% (n=7), respectively. The limit of detection of baclofen in plasma was 0.1 microM (21 ng/ml).     

Vibrational spectroscopic studies of sol-gel derived physical and chemical bonded ORMOSILs

Fourier transform infrared (FT-IR) and FT-Raman Spectroscopy have been utilized to characterize the structure of physical and chemical bonded ORMOSILs (organically modified silicates) and to compare with the physical properties, reported earlier. The classic and sono ORMOSILs were synthesized by sol-gel method via traditional- and sono-catalysis routes, respectively. The physical and chemical bonding is established by Poly(ethylene glycol) (PEG) and Poly(dimethoxysilane) (PDMS), respectively. Existence of band at ∼560 cm⁻¹ (FT-IR) and ∼490 cm⁻¹ (FT-Raman) for the sono and classic gels with 5-10 wt% of PEG indicates the presence of structural defect due to the four-membered siloxane rings. Application of long molecular PEG chain and PDMS increases this defect. Modification in the intensity and peak position of siloxane (Si-O-Si) bands is found correlative with the physical properties. The xerogels with 5-10 wt% of PEG possess a large number of residual surface silanol groups than the xerogels with long molecular PEG chains and PDMS and is found related with the ν(OH) band at ∼3470 cm⁻¹. These results are attributed to the way of hydrolysis-condensation reactions and discussed with the help of Percolation and DLVO models.     

Shape‐Induced,Hexagonal, Open Frameworks: Rubidium Ion Complexed Cucurbituril

A honeycomb structure is shown by the one‐dimensional coordination polymer comprising D_6h‐symmetric cucurbituril molecules and rubidium ions (see picture). The cucurbituril molecules stack atop one another and show coordination of their carbonyl groups to the rubidium ions in between. The shape and symmetry of the building blocks encourage the coordination polymer chains to be arranged in such a way as to produce an open‐framework structure with large, linear, hexagonal channels.     

Grain boundary diffusion of Cu in TiN film by X-ray photoelectron spectroscopy

In this study, the grain boundary diffusion of Cu through a TiN layer with columnar structure was investigated by X-ray photoelectron spectroscopy (XPS). It was observed that Cu atoms diffuse from the Cu layer to the surface along the grain boundaries in the TiN layer at elevated temperature. In order to estimate the grain boundary diffusion constants, we used the surface accumulation method. The diffusivity of Cu through TiN layer with columnar structure from 400 °C to 650 °C is D_b≈6×10⁻¹¹exp(−0.29/(k_BT )) cm²/s. Received: 18 May 1999 / Accepted: 8 September 1999 / Published online: 23 February 2000