Effect of film thickness and supercooling on the performance of cholesteryl cinnamate liquid crystal capillary columns

Improved separations of the isomers of olefinic aliphatic insect pheromones were obtained on cholesteryl cinnamate glass capillary columns by operating in the supercooled temperature range of the liquid crystal. Capillary columns were prepared with varying film thickness of the stationary phase; choice of the correct film thickness ensured optimum retention for a wide range of compounds within the most effective temperature range of the liquid crystal. The deactivation procedures described made the liquid crystal columns suitable for separation of the geometric isomers of polar and nonpolar compounds.     

Structure and Magnetic Properties of Nickel–Zinc Ferrite Nanoparticles Prepared by Glass Crystallization Method

Summary. The magnetic and microstructure properties of Fe₂O₃–0.4NiO–0.6ZnO–B₂O₃ glass system, which was subjected to heat treatment in order to induce a magnetic crystalline phase (Ni_0.4Zn_0.6-Fe₂O₄ crystals) within the glass matrix, were investigated. DSC measurement was performed to reveal the crystallization temperature of the prepared glass sample. The obtained samples, produced by heat treatment at 765°C for various times (1, 1.5, 2, and 3 h), were characterized by X-ray diffraction, IR spectra, transmission electron microscopy, and vibrating sample magnetometer. The results indicated the formation of spinel Ni–Zn ferrite in the glass matrix. Particles of the ferrite with sizes ranging from 28 to 120 nm depending on the sintering time were observed. The coercivity values for different heat-treatment samples were found to be in the range from 15.2 to 100 Oe. The combination of zinc content and sintering times leads to samples with saturation magnetization ranging from 12.25 to 17.82 emu/g.     

Preparation and properties of rare-earth containing oxide fluoride glasses

The preparation of the rare earth containing oxide fluoride glasses LnF₃ (Ln; Y through Lu)-BaF₂-AlF₃-GeO₂ in which the nominal content of LnF₃ reached 60 mol% in maximum and their basic properties such as density, refractive index and glass transition temperature were investigated and summarized in detail. Especially, in order to discuss the local structure around the rare earth ion in the glass, the Judd-Ofelt analysis (discussion with Ω parameters) of the HoF₃-BaF₂-AlF₃-GeO₂ glasses was carried out. The unique fluorescent behavior and the magnetic properties of LnF₃-BaF₂-AlF₃-GeO₂ glasses (Ln = Tb and/or Sm) were also studied.     

Miniaturization of separation techniques using planar chip technology

Miniaturization of separation columns implies equally reduced vol- umes of injectors, detectors, and the connecting channels. Planar chip technology provides a powerful means for the fabrication of micron-sized structures such as channels. This is demonstrated by two examples. An optical absorbance detector chip exhibits the expected behavior of a 1 mm optical path length cell despite its volume of 1 nL. A capillary electrophoresis device allows integrated injections of 100 pL samples, efficiencies of 70,000 to 160,000 theoretical plates in 10 to 20 seconds, and external laser-induced fluorescence detection at any capillary length of choice between 5 and 50 mm.     

Preparation of apolar glass capillary columns by the barium carbonate procedure

As an extension of previous reports, the barium carbonate procedure has been optimized in detail for the preparation of apolar columns. The aim was to produce optimum overall column characteristics, and to maintain them unchanged under the prolonged influence of the highest possible temperature. The main parameters under optimization were glass variety, leaching of glass surface with aqueous HCl, and amount of barium carbonate deposited, while deactivation and coating were kept constant. The basic column characteristics were adsorption properties and thermostability of deactivation, acid/base behaviour and separation efficiency. They were determined by a new, quantitative testing procedure. Intense leaching was able to eliminate almost totally the differences between glass varieties and to create a well-defined glass surface. While untreated glass, leached glass, and barium carbonate treated glass showed specific weak points in the respective column quality, the combination of leaching and barium carbonate treatment yielded the highest and most stable quality. Some technical modifications of the preparation procedure are described, including deactivation in the gas phase, and use of pentane as a solvent for static coating.     

Carboxylic acid functionalization of nylon 6 by radiation grafting and conversion to zinc salts: Effects on physical properties

 Functionalization of polymers by grafting monomeric species on to the backbone of molecular chains with the use of γ-radiation has been used extensively. In this work methacrylic acid was grafted onto a commercial grade of polycaproamide (Nylon 6) by preirradiating the polymer granules to 15 kGy at a rate of 1.0 kGy per hour and subsequently immersing these in a 10% aqueous solution of methacrylic acid in the presence of small quantities of FeSO₄ as homopolymerization inhibitor. The polymer was subsequently neutralized by mixing it with zinc acetylacetonate in a laboratory scale melt mixing device. The acid-grafting polymer modification resulted in an increase in glass transition temperature, while the addition of zinc acetylacetonate gave rise to two transitions: The lower transition corresponds to a miscible mixture of free polyamide and acid-grafted polymer, both plasticized with undecomposed zinc compound, while the upper transition corresponds to the zinc salt of the acid grafted polyamide. Through rheological measurements it was shown that both the acid-grafted polymer and the derived zinc salt have a branched structure, possibly containing also some crosslinked domains. Large improvements in solvent resistance were observed for both type of polymer modifications. Received: 13 December 1996 Accepted: 10 February 1997     

Glass transition measurements of asphalts by DSC

The glass transition temperature (T_g), measured by Modulated Differential Scanning Calorimetry (MDSC), is related to the flow characteristics of asphalt at low temperatures as is the rate of change of the creep stiffnessm. This study compared the glass transition temperature of different asphalts (neat, chemically modified, and crumb rubber modified asphalts) with the creep stiffness, the rate of change of creep stiffness, and the low specification temperature of the continuous PG grading of those asphalts.From the rheological data (BBR) and the thermal data (MDSC) for the virgin and the modified asphalts, the modified products had the same variations of values ofm, S, and T_g at lower temperatures as those of their corresponding virgin asphalts. A correlation between the T_g andm value was observed for both the modified and unmodified asphalts. Since DSC measurements for asphalt low temperature properties use less operator time, less sample, and have less measurement and operator error than rheological methods, T_g has promise to be considered as a fast and easy laboratory method to obtain the low temperature useful range of asphalts in pavements.The authors would like to acknowledge Susan P. Needham for her work in conducting rheological testing for the modified and unmodified asphalts.     

透明导电玻璃(ITO)基材自加热传感静态芯片聚合酶链反应(PCR)

利用商品化ITO玻璃导电层的温阻效应, 无需任何微加工手段, 实现了自加热和传感的芯片温度自动程序控制, 最大程度地减小了传感滞后对温度控制稳定性的影响, 温度控制的稳定性达到了0.2 ℃, 升温速度最快可达20 ℃/s以上, 在冷却风扇辅助下降温速度最快达到了8 ℃/s. 芯片温控单元的引线从传统的两对(一对用于传感, 一对用于加热)减少为一对. 通过在该芯片上直接构建多个开放微池反应器的方法成功地实现了λDNA 157 bp片段的并行扩增. 将该芯片置于倒置荧光显微镜样品台上, 以蓝色(575 nm)发光二极管为光源, 以光电倍增管为检测手段检测了dsDNA和SYBR Green Ⅰ嵌合物的荧光强度随温度的实时变化曲线.     

Surface modification of soft-glass capillaries for gas chromatography by treatment with water vapour

“Leaching” or “etching” by strong mineral acids seems to be a necessary pretreatment step for the most commonly used deactivation procedures of glass capillaries by reaction with either polyethylene glycol or silylation reagents. The acidic sites which are formed on the surface during this acid treatment cannot be completely removed by the subsequent deactivation process. This drawback can be overcome by performing the leaching with water vapour, resulting in an accumulation of cations at the surface and a decrease in the number of silanol groups. Capillaries of this type show excellent properties for the chromatography of strongly basic compounds. After the wash-out of the alkaline surface layer, the acidity of the support is suited for the chromatography of strongly basic as well as strongly acidic compounds. Due to a lack of reactive acidic sites, special deactivation procedures have to be applied to capillaries produced in this way.     

A calorimetric study of the glass transition kinetics in polyisoprene

The connection between the dielectric and calorimetric relaxation behaviours of synthetic polyisoprene Cariflex IR 305 is studied. A similar comparison of dielectric and dilatometric results was described in [1]. The heat capacity was measured during heating of samples prepared with different thermal history. Experimental results were compared with the heat capacity curves calculated for a model based on the multiparameter theory of Kovacs et al. [4]. The model considers the relaxation system as being composed of a set of subsystems characterized by different relaxation times. The distribution of relaxation times and their temperature dependence were taken from the diclectric measurement. The relaxation time of a subsystem from posed to depend, not only on the actual, temperature of the sample, but also on the deviation of this subsystem from equilibrium, or alternatively, on the deviation of the system as a whole. The comparison between the measured and modeled curves shows that both influences must be taken into account in order to explain the experimental results.Dedicated to Prof. Dr. W. Pechhold on the occasion of his 60th birthday.